Proceedings of

XIII International Seminar on

Mineral Processing Technology
MPT-2013
10-12, December 2013

VOLUME - I

Editors

Alok Tripathy
D.B. Ramesh
A. K. Sahu
S.K. Biswal
B. Das
P.S.R. Reddy
B.K. Mishra

Jointly Organized by
CSIR-Institute of Minerals and Materials Technology
Bhubaneswar
&
Indian Institute of Mineral Engineers
 MPT-2013

© 2013, CSIR-Institute of Minerals and Materials Technology, Bhubaneswar, India

(CSIR-IMMT)

No Part of this publication can be reproduced, copied or translated in any form or

by any means without the written permission from copyright owner.

Theme of MPT-2013

Minerals to Metals for Sustainable Development (Minmet)

CSIR-Institute of Minerals and Materials Technology, Bhubaneswar and MPT-2013

is not responsible for the views, statement and facts expressed by the authors in any
of its publications.

ISBN 978-81-928552-0-2

Published by CSIR-Institute of Minerals and Materials Technology, Bhubaneswar,

Odisha 751013, India
Printed at : Reproprint Pvt. Ltd., N-5/44, I.R.C. Village, Nayapalli, Bhubaneswar.
 MPT-2013

Foreword

The XIII International Seminar on Mineral Processing Technology (MPT) is being organized at CSIR-
Institute of Minerals and Materials Technology, Bhubaneswar during 10-12 December 2013. We
are indeed honoured to host this prestigious seminar on the occasion of our Golden Jubilee year.
The theme of the seminar “Minerals to Metal for Sustainable Development (Minmet)” has been
selected to address the current challenges like land, water, and energy faced by mineral based
industries. There are also challenges with respect to sustainability. The International Seminar is
the best platform for mineral processing professionals to deliberate on such challenges.

This year MPT is jointly organized by CSIR-IMMT, Bhubaneswar and IIME Bhubaneswar Chap-
ter with the sponsorship of Essar Steel, Longi Magnet Ltd., JSPL, Tata Steel, Triveni Earthmovers
Pvt. Ltd., Bhushan Power & Steel Ltd., Adhunik Group, Chandan Steel, Mineral Technologies,
Westech, Trimex Group, Gallant, allmineral Gmbh, Vedanta Group, BRPL and many Gold and
Silver sponsors. Altogether 268 abstracts have been received from the all over the world apart
from 9 plenary lectures and 30 invited talks by eminent persons. About 30 technical sessions
have been planned and out of this 4 technical sessions are set aside exclusively for the student
participants. The Technical Committee has reviewed the papers and made suitable format to
publish the full paper in the seminar proceeding.

I am grateful to the members of the International Advisory Committee, National Advisory Com-
mittee and Local Organising Committee for their guidance, help and cooperation. I am especially
grateful to our patrons, sponsors, and Exhibitors for their supports to make this event successful.
I look forward to meet you at Bhubaneswar during MPT 2013.

Prof. B. K. Mishra
Chairman, Organising Committee, MPT-2013
& Director, CSIR-IMMT

iii
MPT-2013
 MPT-2013

Preface

Rocks and minerals have contributed immensely to the growth and development of
human civilization. These also provide opportunities to understand the evolving rela-
tionship of humankind with nature. While the evolving relationship varies over time
and place, there is no denying the fact that current consumption of minerals to pro-
duce metals worldwide are taking a heavy toll on our planet—its environment and
resources. Whereas in the nineteenth century, environmental protection was largely
advanced for utilitarian purposes, the scientific basis for the need to protect the envi-
ronment and its natural resources gained significant ground in the twentieth century.
Today it is all about sustainable development. The mineral processing community has
been adequately responding to the call but we still have a long way to go.

Extraction and development of different ores are closely interlinked with other natural
resources like land, water, air and forest. Sustainable development of mineral resources
means to follow scientific methods starting from exploration, mining, and beneficiation,
extraction of metals by proper environmental management to balance the ecology
and improve the socio-economic balance of locality. Mineral development in a region
should be carried out within its available social and environmental ‘carrying capacity’
and infrastructure facility at a given point of time.

The state of art technology is presently available to recover the mineral values in the
most economic and sustainable manner. Simultaneously the associated waste genera-
tion can be minimized by making value added products. To improve the air quality
associated with mining, advanced technologies like pipe conveyor and pipeline for
slurry transportation may be made mandatory to avoid pollution. Without the avail-
ability of water, mineral processing is impracticable. Water is used as medium not only
to transport materials but also to process the ore to meet the required specification of
downstream industries. The major challenges to water management in India are stag-
gering which calls for conservation of water in mining and mineral processing. Min-
eral industry must consider by adopting new technologies to replace the fresh water
with waste water and saline water. The tailings disposal is one of the major problems of
mineral industries which must be tackled using proper disposal method after filtration
or thickening at higher solid concentration.

v
 MPT-2013

This seminar has received good number papers on important issues like beneficiation
using low grade ores, effective grinding circuit, equipment development, disposal of
tailings, utilisation of waste generated in the plant, pipe line transportation, pelletisation
of high LOI, high Blaine number iron ore concentrate, chemical reduction of ores,
leaching, solvent extraction, etc. And in all these topics the environmental issues are
addressed.

Mineral processing is at crossroads. Sustainable consumption and production, and

managing the planet’s natural resource base for the benefit of all are the overarching
challenges of sustainable development. We emphasize its value and hope that these
will be deliberated during MPT2013 to guide us towards the future we want.

Alok Tripathy
D.B. Ramesh
A. K. Sahu
S. K. Biswal
B. Das
P.S.R. Reddy
B. K. Mishra

vi
 MPT-2013

CONTENTS
Foreword iii
Preface v

Volume I

Characterization

1 Investigation on nanomineralogy of Indian coals and coal fly 03

ashes
Binoy K Saikia and Bimala P. Baruah
2 Characters of some lead zinc ores from the Benue trough, 07
Nigeria
Obassi Ettu and B. Nayak
3 Hydrocarbon generation potential of shales from Raniganj 12
basin, west Bengal, India
Atul Kumar Varma, Bodhisatwa Hazra, Vinod Atmaram Mendhe and
Itishree Chinara
4 Characterization of minerals in coal development of a novel low 19
temperature device for quick isolation of minerals
S. Kumar, T. Gouri Charan, S.C. Maji, M.K. Saini, G. Udayabhanu
and A. K. Bandopadhyay
5 Characterisation of PGE mineralisation at Boula Nuasahi 27
igneous complex, Odisha, India
M. S. Jena, D. Dash, J. K. Mohanty, N. R. Mandre and R. Venugopal
6 Geology of “Eklama iron ore complex” with special emphasis on 39
geochemistry of iron ore
Mofid Ali
7 Mineralogical characterisation of the iron ores having varying 45
degrees of LOI from Gua and Kiriburu mines, SAIL
Sanjay Hembram and Ram Pravesh Bhagat
8 Characterisation of eluvial ruby (corundum) from dumerpadar, 51
kalahandi, Odisha
S.K. Das and J.K. Mohanty
9 Heavy mineral distribution and characterisation of ilmenite of 56
astaranga and ersama coastal tracts, Odisha
S. K. Das, B. K. Nayak and S. Aich

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 MPT-2013

Communition and Classification

10 Exploring new grinding aids to improve the energy efficiency of 65

dry grinding process
Veerendra Singh, P. K. Banerjee, V. K. Saxena and R. Venugopal
11 Mass balance study on the grinding classification circuit of 75
Hindustan Zinc Limited at Rampura Agucha mines
Jayesh B. Gakare, T. S. Anil Kumar Nistala, Ajit Swain and K. D.
Sharma
12 Improving reliability of screens in closed circuit crushing coal 81
Partha Das, Naveen Kumar, and Pallav Garg
13 Optimization of grinding circuit in Uranium milling operations 87
S. Siddique, K. Srinivas and N. R. Mandre
14 Energy optimization of ball mill grinding operation 93
Shivani Sharma and V. K. Gupta
15 Understanding Bond work index and its limitations 99
V. K. Gupta
16 Effect of breakage on coal characteristics – a case study 104
Arun K Hardha, Anubhav kumar, Utkarsh Singh and V K Saxena
17 High energy milling of boehmite: changes in particulate 109
characteristics
T.C.Alex, Rakesh Kumar, S.K. Roy and S.P. Mehrotra

Gravity Separation
18 A simple laboratory alternative to large scale jigging tests 115
Philip Thompson
19 Misplacement of particles in liquid solid fluidization 119
Alok Tripathy, S.K. Biswal and B.C. Meikap
20 Segregation of minerals in floatex density separator – A study 125
by using synthetic mixture
Sharath Kumar Bhoja , Srijith Mohanan, C. Raghu Kumar, Ashok
Kumar, Shobhna Dey and Avimanyu Das
21 Performance evaluation of ultra fine gravity concentration 130
circuit
Y. Rama Murthy, Sunil K. Tripathy, V. Singh, A. Ranjan and A.
Srinivsulu
22 Developments in fine mineral spiral separation technologies 137
Glen Rampola, Alex, D Costa and O.K. Venugopal

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 MPT-2013

Flotation

23 Single green reagent for graphite flotation 145

N.Vasumathi, T.V.Vijaya Kumar, S.Ratchambigai, S.Subba Rao,
S.Prabhakar, G.Bhaskar Raju, S.Shiva Kumar and Uma Raman
24 An alternative for the conventional graphite depressant in lead 154
zinc flotation at Rampura Agucha mines of Hindustan Zinc
Limited
Jayesh B. Gakare, T. S. Anil Kumar Nistala, Ajit Swain and Dr. K. D.
Sharma
25 Hydrodynamics of flotation column using sphalerite fines 160
Kamalendu Bhunia, Gautam Kundu and Dibyendu Mukherjee
26 Sulphide mineral flotation – a new insight into oxidation 169
mechanisms
Alireza Javadi Nooshabadi and Kota Hanumantha Rao
27 Optimisation of Operating Variables in Cassiterite Flotation 183
HoSeok Jeon, SangHo Baek, S. I. Angadi and B. K. Mishra

Dewatering & Tailing Disposal

28 Studies on settling characteristics of coal preparation plant 191

tailings by flocculation
S. Kumar, N.R. Mandre and S. Bhattacharya
29 Effective control of high rate thickener process parameters with 196
respect to run of mines in Wet Processing Plant at Noamundi
Iron Mines
S.Mishra , V.Agarwal , A.Kumar and D.Mukherjee
30 Parametric optimisation for filtration of iron oxide concentrate 202
S. S. H. Naqvi, P. S. Maji, Aslam Khan and Sushil Dubey
31 Enhancement of fine coal dewatering in screen bowl centrifuge 208
A. Das, S. Jaiswal and P. K. Banerjee
32 Sedimentation studies on non coking coal fines with some 214
industrial flocculants
K. M. P. Singh, G. Udayabhanu, T. Gouricharan and J. K. Pandey
33 Paste backfill and thickened tailings disposal – A solution for 220
sustainable development in mining industry
Gautam Chatterjee,Atul Gandhe, P. Pierre and Chris Lee

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 MPT-2013

Modelling & Simulation

34 Model for seggregation of binary mixture of solids in fluidized 235
beds
S. Narasimha Reddy and P. S. T. Sai
35 Review of simulation of work index determination 240
A. Pathak, R. Kishore, U.K. Chanda, K.K. Sahu, S. Pati and N.P. H.
Padmanabhan
36 Grinding and classification circuit optimization with modelling 244
and simulation study at Hindustan Zinc Limited S.K. Mines
T. S. Anil Kumar Nistala, Ajit Swain and K. D. Sharma
37 A fixed grid model of solidification of semitransparent materials 249
S. P. Kar and P. Ratha
38 CFD modelling of column flotation: Prediction of two phase 257
flow hydrodynamics
Balraju Vadlakonda and Narasimha Mangadoddy
39 Computational and experimental study of the effect of 265
inclination on hydrocyclone performance
Kedar Kumbhar, VTSR Kumar Reddy and Narasimha Mangadoddy
40 Modelling and optimization process for beneficiation of coal 274
fines using artificial neural network
Sweta Kumari, V. K. Kalyani, T. Gouri Charan, G. S. Jha and
Amalendu Sinha

Coal Preparation
41 Chemical beneficiation of high sulphur North-East Indian coals 281
by alkaline oxidation
Runjun Chetia, Binoy K Saikia , Dileep K Dutta and Bimala P Barauh
42 Microbial up-gradation of Meghalaya coal by Rhodococcus 287
Rhodochras and Pseudomonous Aeruginosa
A.Ghosh, Sujata, Abhilash and B.D.Pandey
43 Washability curve versus Mayer’s curve 294
Ajit Singh Choudhary, Eshan Tiwari and I.Narendra Kumar
44 Media stability issues with heavy medium separators 299
Pankaj Kumar Jain and S. Bhattacharya
45 Application of native microbes for biodesulphurization of North 308
east high sulphur coal
S. Mishra, P. P. Panda, N. Pradhan, D. Satapathy, S. K. Biswal and
B.K. Mishra
46 Semi supervised classification of mapping between coal blend 313

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 MPT-2013

B.K. Mishra
46 Semi supervised classification of mapping between coal blend 313
parameters and coke strength after reaction (CSR)
Tathagata Ray, A. Suresh, Pratikswarup Dash and Pradip Banerjee
47 Studies on the cleaning potentialities of Ib valley coals by 318
washability investigations for power generation
T. Gouri Charan, P. C. Nagnoor and B. P. Ravi
48 Chemical fractionation analysis on some Indian coal sources and 322
their correlation with ash fusion temperature
S. Chakravarty, A. K. Mohanti, Anita Kumari, Arun K Mahato and
Mamta Sharma
49 Process amenability studies for de-shaling of coking coal sample 326
from Bokaro, central coalfields limited, India
P. C. Naganoor, T. Gouricharan, B. S. Prasad, S. M. Gowda, K.
Manjula and G. B. Balachandar
50 Prediction of coking properties of coals using 329
thermogravimetric analysis
J.V.S. Murty, C.V. Nageswara Rao, Nilu Kumar, A. Srinivasa Rao,
U. Hari Prasad and Ch. V. R. Murty
51 Studies on the effect of coal beneficiation on ash fusion 334
temperatures
Banashree Mahanta, Binoy K Saikia, Arju Moni Dutta, Prasenjit
Saikia and Bimala P Baruah
52 Beneficiation of low rank north east Indian coals by ultrasonic 338
action in ionic liquids: a green approach
Arju Moni Dutta, Binoy K Saikia, Lakshi Saikia and Bimala P Baruah
53 Washability characteristics of Kusmunda seam coals, Korba 344
coalfield
A.K.Chattopadhyay, M.K.Sethi and S.K.Konar
54 Scope of selective washing of thick inter-banded coal seams: 348
Few case studies
A.K.Chattopadhyay, M. K. Sethi and S.K.Konar
55 Chemical beneficiation of physically treated Hingula coal on 352
laboratory scale
S. Pramanik, B.K. Purohit, P. Meshram, S.K. Sahu and B.D. Pandey
56 A study on pressure and sp. gravity inside heavy media 360
cyclone to optimize the yield & quality of washed coal
Mofid Hussain, S.P. Singh, and Bidhan Ch. Dey

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 MPT-2013

57 A Study of coal washing spirals treating Indian coals 365

K.M.K.Sinha, Nilesh Kumar, Pradeep Sahu, G.S.Jha and T. Gouri
Charan
58 Studies on characterization and beneficiation of a low volatile 369
coking (LVC) coal
Divya jyoti, V. K. Saxena and S. Bhattacharya
59 New coal preparation plant circuitry for Indian metallurgical 374
coal
S. Saurabh, Z. Wang, A. Mahapatra and S. Pal
60 Suitability of froth flotation in comparison to spiral washer for 382
an existing coking coal washery – A case study for its
improvement in respect to yield% at desired ash level
Sanjay Chaudhuri, S.K. Kabiraj, U.S. Chattopadyay, S.C. Maji and
T.G. Charan
61 High ash non-coking coal from India: beneficiation and 385
implications
A. Vidyadhar, Renuka and M. Sharma
62 Recovery of settling pond coal fines through physicochemical 391
techniques for optimum utilization
U.S.Chattopadhyay, T. Gouri Charan and R.Venugopal
CHARACTERIZATION
 MPT-2013

2
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Investigation on Nano-Mineralogy of Indian Coals and Coal Fly

Ashes
Binoy K Saikia* and Bimala P Baruah
Coal Chemistry Division, CSIR-North East Institute of Science & Technology, Jorhat-
785006, India

Abstract
The mining and utilization of coals may cause serious impact on the environment. In present
investigation, the nano-mineralogy of some coal and coal fly ash (CFA) samples from North Eastern
region (NER) of India were extensively studied for sustainable environment. A combined approach
using XRD and FE-SEM/HR-TEM techniques has revealed the presence of major minerals such as
Quartz, Calcite, Bassanite, Kaolinite, Dolomite, Tschermigite and Ankerite. The pyrite in these
coals is found to occur in different forms, e.g. framboids and cubic crystals. The nano-minerals
with Fe-Al nano-(hydr) oxides, e.g. hematite, goethite, magnetite; and nano-sulphates, e.g. jarosite,
are found in the coal and fly ash samples. The hematite, magnetite and goethite have high
concentrations of hazardous elements viz. As, Cd, Cr, Hg, Pb, and V. The coal-derived nano-
particles from coals, which could be environmentally hazardous, are discussed in this paper.

Keywords: Indian coal; nano-mineralogy; high sulphur coals; coal fly ash.

1. Introduction detrimental to health when present in sufficient

India has about 10% of the world’s coal reserves,
which is enough for the next 200 years. North
Eastern region of India has a substantial deposit
of high sulphur coals (Figure 1) (Saikia et al.,
2009). Mining and industrial operations during
usage of these coals c ontribute severely
towards environmental degradation (Baruah
et al., 2006). They have been generally used in
thermal plants of paper mills, tea factories, and
cement plants, among other industries. The
occurrence of environmental hazards during
mining and utilization of coals is a serious
concern. Coal and coal fly ashes (CFAs) contain
trace concentrations of hazardous volatile
elements (HVEs) that are known to be
* Correspending Author: bksaikia@gmail.com
quantities. The presence of mineral matters in
Indian pulverized coal may diversely affect the
behaviour of the emitted particles during
combustion and could also influence the level
of un-burnt carbon in ash experienced in power
plants (Saikia and Ninomiya 2011). Coal-
derived nanoparticles have been known to have
adverse effects on human health and the
environment (Zhao et al 2006; Hower et al 2008;
Silva and DaBoit 2011). They mainly originate
from the heterogeneous nature of the mineral
matter present in CFAs and are formed by
complex physical and chemical processes,
involving vaporization, condensation, melting,
fragmentation, and coalescence (Takuwa et al.,
2006). Nano-particles inc luding ultrafine
particles are thought to induce more severe
health impacts than larger particles.

3

Coal fly ash (CFA) is one of the residues
generated in combustion, and comprises the
fine particles that are transported with the flue
gases. Depending upon the sourc e and
composition of the coal being burned, the
components of CFAs vary considerably, but all
CFAs include substantial amounts of SiO2 (both
amorphous and crystalline) and Al2O3, with
lesser amounts of CaO. Therefore, a more
detailed study on the mineralogy of this CFA is
required towards the enhancement of their
utilization in other aspects and to assess the
potential exposure risks to human and
ec ologic al systems, espec ially from the
c ontribution from the re-suspension of
ultrafine/nano-particles to air particulate
matter around the power plant.
The present Field Emission Scanning Electron
Microscope (FE-SEM) and high-resolution
transmission electron microscope (HR-TEM)
with energy-dispersive X-ray spectroscopy
(EDS) study is the first to identify nanominerals,
ultrafine particles, and hazardous elements in
any Indian coals and coal fly ashes. Thus, a
better understanding of the chemistry of these
coals to improve their environmental concerns
in the coal fired sector is a crucial step towards
correct energy planning and management. The
knowledge on mineral matter and associated
nano-minerals in these c oals will surely
provide a systematic route to design the clean
coal technology principle. Thus, some of the
advanced instrumental techniques are used for
mineralogical investigation of two industrially
important coal samples to understand the
potential importance of hazards associated
with their increased utilization.
2. Materials and Methods
The representative coal and c oal fly ash
samples were supplied by Shyam Century
Ferrous Limited, Meghalaya and Nagaon Paper
Mill, Assam. The c oal samples were
characterized for their physical and chemical
4
MPT-2013
properties using standard procedures (ASTM,
1991 and 1996) (Table 1). The mineralogy of
coal and fly ash was analysed by X-ray powder
diffraction using a X-ray diffractometer
(Rigaku) with Cu K-alpha radiation, and the
minerals present identified by reference to the
ICDD Powder Diffraction File.
In order to provide further information on the
minerals and ultrafine particles present in the
coals high-resolution transmission electron
microscopy (HR-TEM) and scanning electron
microscope with energy dispersive X-ray (SEM/
EDS) were performed on samples from the
different sites.
2. Results and Discussions
2.1 Petro-chemical characteristics of the coals
The chemical analyses of the two coals are
shown in Table 1 respectively, which expresses
the coal to be of sub-bituminous in rank with
high sulphur. The fly ash samples have high
ash and carbon contents.
2.2. Mineralogy of the coal and coal fly ash
A combined study consisting of XRD and FTIR
analysis were carried out on the coal and fly
ash samples and are depicted in Figs. 1 and 2. It
indicates the presence of minerals viz. quartz,
kaolinite, calcite etc. as the major phases in the
coal samples. The fly ash samples include the
major phases of quartz and hematite. Hematite
in the fly ash samples are formed during the
c oal c ombustion through the mineral
transformation. The dominance of silicate and
detrital clay minerals including kaolinite were
seen in these sub-bituminous NE Indian coals.
Calcite was also found in these coals. The
abundant quartz identified by the XRD analysis
suggests its form as á-quartz.
2.3. Nano-mineralogy of the coals and fly ash
The pyrite in these coals is found to occur in
different forms, inc luding nanomineral

particles pyrite, framboids and cubic crystals.
Pyrrhotite, marcasite, and chalcopyrite were
detected as accessory ultrafine minerals in both
coals samples. A small amount of sphalerite
was also observed. In addition, hazardous
elements were detec ted in the Fe-
nanosulphides. The hematite, magnetite and
goethite observed by HR-TEM/EDS have high
concentrations of As, Cd, Cr, Hg, Pb, and V. The
knowledge on the nano-minerals in coals has
been overlooked in prior studies dealing with
their behaviour in environment and
communities. Thus, the presence of nano-
particles including nano-pyrite and Fe-hydr/
oxide should be taken into consideration during
coal utilization particularly for the workers in
the thermal plants. The nano-minerals with Fe-
Al nano- (hydr) oxides (e.g. hematite, goethite,
magnetite; and nano-sulphates (e.g. jarosite) in
ultrafine/nanoparticles might act as major
absorption sites for hazardous elements. The
nano-hematite characteristics identified by the
HR-TEM/SAED/FFT/EDS analysis revealed
individual nanoparticle sizes for the different
ash samples ranging between 1.9, 8.6, 20.1, 25.6,
and 40 nm (Oliveira et al., 2014). The lattice
fringes were apparent on the HR-TEM nano-
hematite images.
4. Conclusions
High sulphur Indian Coal ash were primarily
composed of quartz, kaolinite, gypsum and
pyrite, followed by feldspars and jarosite,
which are the main precursor for the formation
of nano-particle as well as mobility of toxic
elements. Further research is warranted to gain
a better understanding of high sulphur coal ash
c hemistry and their environmental
implications. The release of mercury from coal
fly ashes is to be diminished before their
disposal to the open environment.
5
MPT-2013
Acknowledgements
Authors are thankful to Director, CSIR-NESIT,
Jorhat for his interest to this works. Authors
are also grateful to Dr Luis F Silva and his
groups, Centro Universitário La Salle, Brazil for
his assistance in electron beam data.
References
Baruah, B.P., Saikia, B.K., Kotoky, P., Gangadhar
Rao, P. 2006. Aqueous leaching on high
sulfur sub-bituminous coals, in Assam,
India. Energy and Fuels, 20, pp.1550-1555
Hower J.C., Graham U., Dozier A., Tseng M.,
Khatri R. 2008. Association of the Sites of
Heavy Metals with Nanoscale Carbon in
a Kentucky Electrostatic Precipitator Fly
Ash. Environ. Sci. Technol. 42, pp.8471-
8477.
Oliveira, M.L.S., Marostega, F., Taffarel, S.R.,
Saikia, B. K., Waanders, F.B., DaBoit, K.,
Baruah, B.P., Silva, L.F.O., 2014. Nano-
mineralogical investigation of coal and fly
ashes from coal-based captive power
plant (India): An introduc tion of
occupational health hazards, Science of
The Total Environment, 468-469, pp.1128–
1137.
Saikia B.K., Ninomiya Y. 2011. An investigation
on the heterogeneous nature of mineral
matters in Assam (India) coal by CCSEM
technique. Fuel Processing Technology, 92,
pp.1068-1077.
Saikia, B. K., 2009. Sc anning Elec tron
Microscopy of Assam Coals, India, Journal
Geological Society of India, 74, 749-752
Silva .LF.O, Boit K.M. 2011. Nanominerals and
nanoparticles in feed coal and bottom ash:
implications for human health effects.
Environmental Monitoring and
Assessment, 174, pp.187-197.
Takuwa, T., Mkilaha I.S.N., Naruse I. 2006. Fine
particle formation from co-combustion of
sewage sludge and bituminous coal. Fuel,
85, pp.671–686.
Zhao Y., Wang S., Aunan K., Martin S. H,
Hao J. 2006. Air pollution and lung cancer
risks in China: a meta-analysis Sci. Total
Environ, 366, pp.500–513.
 MPT-2013

Figure 1: Map showing the coal sample 1000 2000 3000 4000
locations in dark spots (not to scale) 45

SCF
40 K

Q K K
35

30
50

45 K

BP
40 K
Q K

35

30
FA-2 40
Q K
30
K
Table 1: Physico-chemical properties of the 20
coals (as received basis, wt%)
10
40
Coal Samples (wt Ash Moisture VM FC C H N Stotal O
%)
35
MK 14.64 2.56 42.47 40.33 65.01 4.61 1.07 2.54 12.13 Q K
30
FA-1

T2 3.31 1.29 42.29 53.11 77.89 5.69 0.83 2.95 4.37 K

FA-1 79.30 1.98 8.80 9.87 15.70 0.29 0.98 0.64 82.39 25
FA-2 61.10 2.82 9.80 26.20 33.40 0.62 1.10 1.19 63.69
20
15
1000 2000 3000 4000
Q -1
Coal-2 cm
Coal-1 Figure 3: FTIR spectra of Indian coal and fly
K FA-2
P
P
H FA-1 ash samples
PH I
Q
K P
P I
Intensity

P H P C H K
Q
P I
P H P C

Q
P PH

0 20 40 60 80 100
2

Figure 2: XRD of Indian coal and fly ash

samples

*******
6
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar
Characters of Some Lead-Zinc Ores from the Benue Trough,
Nigeria

Obassi Ettu1 and B. Nayak2*

1
Raw Materials Research and Development Council, Maitama, 900271, Abuja, Nigeria
2
CSIR National Metallurgical Laboratory, Jamshedpur, 831007, Jharkhand, India

Abstract
Mining of solid minerals in Nigeria is very limited and insignificant. The ‘Pb-Zn sulfide deposits’
in the Benue Trough is being exploited in small-scales and in a crude method that needs attention
for sustainable mining development. In an attempt to characterize the ore, we have investigated
two samples of lead-zinc ore from the Enyigba and Arufu lodes belonging to the Lower- and
Middle Benue Troughs of Nigeria respectively using optical microscopy, XRD, and scanning electron
microscopy (SEM/EPMA) in order to delineate their mineralogy and mineral chemistry. The samples
were similar being dominated by galena and with subordinate sphalerite. While the mineralogy
in case of Enyigba is very straightforward and simple (galena + minor other sulfides + quartz), the
Arufu sample is a bit complex (galena + sphalerite + minor other sulfides + complex mixed sulfides
+ various carbonates + quartz). The minor sulfides are chalcopyrite and pyrite. While quartz is
found to be the main gangue mineral in Enyigba sample, the Arufu sample contains significant
carbonates. The richness of these Pb-Zn ores keeps promise for the Nigerian Government to
pursue for potential large-scale mining where copper, silver and gold can be recovered as by-
products in addition to lead and zinc.

Keywords: Mineralogy; Pb-Zn ore; benue trough; nigeria.

1. Introduction
Nigeria is one of the key member states of the
Economic Community of West Africa (ECOWA)
whose GDP is primarily dependent on the oil
and gas sector. Although the country possesses
a range of solid minerals that can generate
revenue, their exploration and exploitation are
very limited. Recently, the Ministry of Mines
and Steel Development of Nigeria has identified
* Correspending Author: Bibhuranjan Nayak, Principal
Scientist, Minera l Processing Division,CSIR National
Metallurgical Laboratory, Jamshedpur – 831007, Jharkhand,
India. Contact No.: +91-9431302530
Email: brn@nmlindia.org, brn69@rediffmail.com
some mineral commodities which has potential
for development. The ‘Pb-Zn sulfide deposits’
in the Benue Trough is one such commodity that
is being exploited in small-scales and in a crude
and non-organized method that poses some
dangers to the miners as well as to the
environment. However, these deposits keep
high promise for potential mining activities in
Nigeria. It is in this c ontext, we have
investigated two Pb-Zn sulfide samples from
two different locations: one from the Enyigba
lode of lower Benue in the Ebonyi state and the
other from the Arufu lode of Middle Benue in
the Nassarawa state (Fig. 1). Our prime

7

objective in this study is to c ompare the
mineralogical and geochemical aspects of the
Pb-Zn sulfides from Enyigba- and Arufu lodes
and assess their economic potentialities in
terms of valuable minerals/elements those can
be recovered as by-products in addition to lead
and zinc.
Fig. 1: Simplified geological map of Benue
Trough showing the major Pb-Zn
mineralizations (after Akande et al., 1989).
Samples were collected from Enyigba and
Arufu lodes.
2. Materials and Methods
Two hand-picked bulk grab samples of Pb-Zn
ore, each weighing about 10 kg were collected
from two different locations in the Benue
Trough: one from the Enyigba lode in the Ebonyi
state which is the largest mineralized body
stretc hing about 2km length and
approximately 30m wide and the other from
the Arufu lode in the Nassarawa state. The
constituent ore-pieces of each sample were
randomly collected from different locations of
8
MPT-2013
the mineralized vein in order to represent its
general characteristics. The samples were
massive (Fig. 2) and physically appear to be
dominated mainly by galena.
a
b
c d
Fig.2:Photographs showing the morphological
characters of some of the Pb-Zn sulfide samples
collected from Enyigba (a and b) and Arufu
lodes (c and d).
An integrated instrumental method of mineral
characterization using micro-balance with
attached specific gravity kit, optical microscope,
X-ray diffraction (XRD) and electron probe
mic ro-analysis (EPMA) was used to
characterize the samples. Polished mounts of
the lumps were prepared and studied under
polarized reflected light using Leica-make
optical petrological microscope and under a
JEOL-make EPMA (JXA-8230) having
attachments of both EDS and WDS. X-ray image
maps for elemental mapping was carried out
wherever felt necessary. Quantitative mineral
compositions were determined at a voltage of
20 kV, ~20 nA sample current and keeping the
probe diameter 2µm. Powder samples were
investigated by X-ray diffraction using a Seifert
X-ray diffractometer (model: XRD 3003 PTS)
with Cu-target.
3. Results and Discussion
 MPT-2013

The specific gravity measured on small broken

pieces of Enyigba sample varied from 4.65 to a
b
7.50 with an average of 6.59 (n=20). Few pieces
yielded sp.gr. > 7.3 which is very close to the
theoretical value of galena indicating the
richness of the sample with galena. In case of
Arufu, the specific gravity varied from 4.08 to
7.42 with an average of 6.35 (n=20). X-ray c d

diffraction studies on the bulk-powder samples

of both confirmed the dominance of galena with
minor association of sphalerite. While quartz
is the major associated gangue in the Enyigba
sample, presence of dolomite was recognized
in the Arufu sample. In addition, optical Fig. 3: (a): Secondary electron image of Enyigba
microscopy revealed the trace presence of
sample showing the association of supergene
c halc opyrite, pyrite, framboidal pyrite,
galena (gln) and quartz (qtz). The bar-scale in
marcasite veins in the Enyigba sample. Pyrite,
the photomicrograph equals to 50µm. (b to d):
chalcopyrite and various carbonates (dolomite,
X-ray image maps showing elemental
siderite, calcite) were recorded in the Arufu
sample. Semi-quantitative volume% estimates distribution of Ag, Cd and As respectively in
from the polished mounts indicate that while the area in figure (a). Note the irregular
the mineralogy in case of Enyigba is very distribution of arsenic within galena.
straightforward and simple (galena + minor Table 1: Chemical composition of galena
other sulfides + quartz), the Arufu sample is a from Enyigba sulfide samples (by EPMA)
bit complex (galena + sphalerite + minor other Element 1 2 3 4 5
Sb 0.01 0.02 0.06 0.03 0.02
sulfides + complex mixed sulfides + various Ge 0.31 0.04 0.28 0.32 0.30
carbonates + quartz). The complex mixed As 0.00 0.00 0.08 0.00 0.00
S 13.22 13.77 13.34 13.11 13.11
sulfides of Fe-Cu-Pb in Arufu sample were Fe 0.00 0.02 0.00 0.02 0.03
recognized only by EPMA. Mutual replacement Co 0.00 0.02 0.00 0.05 0.02
relationship between sulfides is a common Ni 0.04 0.00 0.00 0.04 0.00
Cu 0.00 0.01 0.00 0.00 0.00
feature. At many places chalcopyrite replaces
Zn 0.00 0.02 0.00 0.00 0.00
the carbonates too. Sr 0.00 0.00 0.05 0.00 0.00
Random point analysis by EPMA on different Ag 0.00 0.00 0.03 0.00 0.00
Cd 0.23 0.22 0.20 0.18 0.05
galena grains of the Enyigba lode analyzed trace
Au 0.00 0.00 0.00 0.00 0.00
quantities of iron, cobalt, nickel, copper and zinc Pb 86.03 85.97 85.59 86.18 86.19
(Table 1). However, germanium and cadmium Total 99.85 100.09 99.63 99.93 99.70

content are significant which occur up to the
first decimal level. Presence of strontium,
arsenic, antimony and silver was also recorded
in galena. Irregular and variable distribution
of arsenic in this type of galena is notable (Fig.
3).
Galena in the Arufu lode showed two
variations: one similar to that of the Enyigba
(Table 2, point-13); and the other containing
significant copper and higher iron (Table 2,
point-4). Sphalerite is more prevalent in the
Arufu sample. It contains significant iron (~4
wt.%), minor lead (~0.2 wt.%) and trace

9
 MPT-2013

quantities of cobalt, nickel, copper, strontium, Published data on the trac e element
and c admium. Point analyses indic ated distribution of the Pb-Zn sulfide ores in the
presence of silver and gold as well. Elemental Benue Trough are very scarce. Olade and
image mapping revealed loc alized Morton (1985) had presented trace element data
concentration of silver in sphalerite bordering only on few elements such as Fe, Mn, Cu, Cd,
chalcopyrite (Fig. 4). The associated dendritic Ag, Sb, and Ge from mineral concentrates
pyrite which is secondary in nature is arsenic (namely sphalerite and galena) using atomic
bearing and contains elemental gold (Table 2). absorption spec trometry (AAS) and
It also contains significant cobalt (>1 wt.%) colorimetry. The data were from lower Benue
along with traces of nickel, copper, zinc and lead. (Ishiagu, Abakaliki) and few from upper Benue
Elemental gold is also occasionally traced in the (Zurak-Wase). However, Pb-Zn sulfides from
lattices of other sulfides and siderite. the middle Benue were not analyzed. Recently
Olubambi et al. (2008) also presented very
a
b
limited data from the Ishiagu sulfides in the
lower Benue. Although our data are only from
two localities, it scans both lower and middle
Benue samples, covers more elements and are
expected to fill up the knowledge gaps on the
c d
trace element content of the Benue Pb-Zn
sulfides.

4. Conclusion

Both the studied samples from Enyigba and

Fig. 4: (a): Secondary electron image of Arufu
Arufu lode are galena-rich sulfides. Although
sample showing the association of sphalerite
broadly both samples appear to be similar,
(sph), chalcopyrite (chp), pyrite (pyt) and
significant differences exist between the two
dolomite (dol). The bar-scale in the
with respect to mineralogy that are due to
photomicrograph equals to 50µm. (b to d): X-
differences in the host rock contaminations,
ray image maps showing elemental
episodic mineralization and the reaction
distribution of Ag, Cd and As respectively in
between the earlier formed minerals and the
the area in figure (a).
late-stage minerals. Baring minor differences
Table 2: Chemical composition of minerals
between the Enyigba and Arufu samples, it can
from Arufu sulfide samples (by EPMA)
be conclusively stated that both the type of
Galena Sphalerite Chalcopyrite Mixed Sulfide Pyrite
Element 4 13 12 15 1 7 9 10 5 6 sulfides have formed following a similar type
Sb 0.02 0.03 0.00 0.00 0.00 0.00 0.01 0.02 0.00 0.00
Ge 0.40 0.40 0.00 0.00 0.00 0.00 0.12 0.10 0.00 0.00
of ore-genetic process although their associated
As 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.00 0.04 0.01 country rocks are different. It is significant that
S 13.04 13.21 35.40 32.26 33.57 35.25 30.85 18.10 51.07 52.56
Fe 3.65 0.02 3.50 4.17 30.94 29.85 20.71 5.42 45.68 46.01 the pyrite in Arufu is As bearing (0.4 wt.%) and
Co
Ni
0.02
0.00
0.00
0.00
0.08
0.03
0.06
0.02
0.01
0.00
0.05
0.00
0.00
0.00
0.00
0.00
1.57
0.35
1.01
0.32
contains elemental gold; and sphalerite/galena
Cu 0.57 0.00 0.05 0.18 33.71 34.49 20.22 7.45 0.35 0.12 is locally enriched in Ag (0.6 wt%). Chalcopyrite
Zn 0.02 0.00 59.18 62.66 0.03 0.00 0.06 0.03 0.22 0.10
Sr 0.00 0.00 0.03 0.05 0.00 0.02 0.01 0.00 0.00 0.00 also contains some elemental gold. Therefore,
Ag
Cd
0.02
0.12
0.00
0.26
0.00
0.07
0.01
0.10
0.01
0.02
0.00
0.00
0.01
0.11
0.03
0.23
0.00
0.00
0.00
0.01
in addition to lead and zinc, silver and gold can
Au 0.00 0.00 0.01 0.00 0.00 0.10 0.03 0.00 0.03 0.08 be recovered as potential by-products from
Pb 82.31 86.81 0.24 0.20 0.15 0.02 27.79 67.95 0.30 0.00
Total 100.16 100.72 98.58 99.69 98.44 99.77 99.91 99.32 99.60 100.21
these sulfide deposits. Since these sulfides

10

contain toxic contaminants like Pb, Cd, As, Sb
etc., their large-scale mining would warrant
systematic approach following environmental
stipulations.
Acknowledgement
This work was carried out at the CSIR-National
Metallurgical Laboratory, Jamshedpur, India
during the visit of Mr. Obassi Ettu through a
joint INSA-JRD Tata fellowship. Mr. Ettu is
grateful to the Centre for International Co-
operation in Science (CICS), the Director General
of Raw Materials Research and Development
Council (RMRDC), Nigeria and the Director,
CSIR-NML for extending support for the above
visit.
*******
11
MPT-2013
References
Akande, S.O., Zentelli, M. and Reynolds, P.H.
1989. Fluid inclusion and stable isotope
studies of Pb-Zn-fluorite-barite
mineralization in the lower and middle
Benue Trough, Nigeria. Mineralium
Deposita 24, 183-191.
Olade, M.A. and Morton, R.D. 1985. Origin of
lead-zinc mineralization in the southern
Benue trough, Nigeria – Fluid inclusion
and trace element studies. Mineralium
Deposita 20, 76-80.
Olubambi, P.A., Ndlovu, S., Potgieter, J.H. and
Borode, J.O. 2008. Mineralogic al
characterization of Ishiagu (Nigeria)
complex sulfide ore. International Journal
of Mineral Processing 87, 83-89.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Hydrocarbon Generation Potential of Shales from Raniganj

Basin, West Bengal, India
Atul Kumar Varma1*, Bodhisatwa Hazra 1, Vinod Atmaram Mendhe 2 and Itishree
Chinara 1
1
Coal Geology and Organic Petrology Lab., Dept. of Applied Geology, Indian School of
Mines, Dhanbad-826004, India
2
Central Institute of Mining and Fuel Research, Dhanbad-826001

Abstract
Shale gas, hailed by many as a game changer and even a ‘silent revolution’ in US, is drastically
altering the international energy landscape. Shales are unconventional gas systems where the
shale acts as both source and reservoir rocks for gas mainly methane. Organic matter in shale
typically ranges from below 1 wt % to more than 45 wt % and is responsible for in situ gas
generation as well as provides storage sites for shale gas in the organic matter micropore structure.
India has several potential shale gas basins. For the purpose of study authors have selected borehole
shale samples from different parts of Raniganj coal basin. Total of 70 samples were studied for
assessing the shale gas potentiality, out of which 2 belongs to Panchet Formation, 6 belongs to
Barakar Formation, while 24 and 38 samples belong to Barren Measures and Raniganj Formation
respectively. Depth varies from 755 to 812 m for the samples from Panchet Formation, 773 to 1070
m for samples from Barakar Formation, while for samples from Barren Measures and Raniganj
Formations it varies from 55.80 to 1480 m and 177.10-1370.00 m respectively.
TOC (total organic carbon) and Rock eval pyrolysis analysis of the samples were carried out for
determining their organic richness and hydrocarbon generation potential. Samples from Panchet
Formation are marked by low TOC content (0.02-0.29 wt %). The TOC content of the samples from
Barakar Formation varies between 4.49-7.23 wt %, while those from Barren Measures Formation
vary from 3.51 to 8.11 wt %. TOC content of the samples from Raniganj Formation are placed in the
range of 0.82 to 46.28 wt %. The hydrocarbon generative potential of the samples (S2; mg HC/g
rock) from Barakar, Barren Measures, Raniganj and Panchet Formations are placed within the
range of 2.07-3.91, 2.56-13.67, 0.37 to 71.94 and 0.02 to 1.90 respectively.
Tmax values of the samples from Barakar Formation shows that they are all in early to peak stage of
maturity. The samples from Barren Measures Formation are mostly in early to peak maturity
stage barring 3 samples, 1 of which falls in immature stage and other 2 falls in late mature stage.
Tmax of the samples from Raniganj Formation vary between 421-450 °C and shows that majority of
the samples are in early mature to peak mature stage while few are in immature stage. Tmax of the
samples from Panchet Formation varies between 340-463 °C. Hydrogen index (HI) of the studied
samples varies from 31 to 655.
Keywords: Total organic carbon, Rock eval pyrolysis, shale gas
* Correspending Author: Atul Kumar Varma, Coal Geology and Organic Petrology Lab., Dept. of Applied
Geology, Indian School of Mines, Dhanbad-826004, India, Contact no.: (+91)-326-2235271; Fax: (+91)-326-
2296563; Email: atulvarma@hotmail.com

12
 MPT-2013

1. Introduction are believed to have good shale gas potential. The

major basins are namely: Cambay Basin, Assam-
Shale gas, hailed by many as a game changer and
Arakan Basin, Krishna-Godavari Basin, Vindhyan
even a ‘silent revolution’ in US, is drastically
Basin, Cauvery Basin and Damodar valley basin.
altering the international energy landscape. Shales
For the purpose of study authors have selected
are unconventional gas systems where the shale
borehole shale samples from eastern part of
acts as both source and reservoir rocks for gas
Raniganj coal basin. Total of 70 samples were
mainly methane (Cipolla et al., 2009). Organic
studied for assessing the shale gas potentiality,
matter in shale typically ranges from below 1 wt
out of which 2 belongs to Panchet Formation, 6
% to more than 45 wt % and is responsible for in
belongs to Barakar Formation, while 24 and 38
situ gas generation as well as provides storage
samples belong to Barren Measures and Raniganj
sites for shale gas in the organic matter micropore
Formation respectively.
structure (Chalmers and Bustin, 2007, Ross and
2. Geological Setting
Bustin, 2009, Str¹poæ et al., 2010, Mastalerz et al.,
Raniganj coal basin, the easternmost intracratonic
2012). Shales are characterized by ultra low
rift basin of the Damodar Valley, has a semi-
permeability and hence gas flow is very slow.
elliptical, elongated shape, and covers an area of
However huge amounts of natural gas may be
1900 km2 between the Damodar and Ajay rivers.
held by shale. Proper understanding of pore
It is bounded by latitudes 23º03´N and 23º51´N,
structure, sorption characteristics and potential
and longitudes 86º42´E and 87º28´E. (Gee, 1932).
gas capacities of organic-rich shales are very
The Gondwana Supergroup is about 3,200m thick
significant (Montgomery et al., 2005, Bustin, 2005,
and is subdivided into six formal units. The
Pollastro, 2007, Ross and Bustin, 2007, 2008).
Gondwana formations were deposited in the
Generally pore spaces in organic shales are very
tectonic trough with faulted boundaries i.e.,
small. Natural fracture development is significant
northern and southern faulted boundaries, on the
in terms of recovery potentiality of shale gas
either side of the Damodar river which flows on
reservoirs and also determines the quality of shale
the faulted trough. The Raniganj coal basin is
gas reservoir and gas production (Montgomery
faulted down on the south and west, the southern
et al., 2005, Bowker, 2007, Nie et al., 2009). For any
boundary being a series of faults, shows an en
source rock assessment, the measurement of TOC
echelon pattern with a general strike of E-W
(Total Organic Carbon) is a priority and is the first
dipping towards the major faults mostly towards
step of quantifying organic richness, though it
more faulted southern boundary. The oldest beds
doesn’t indicate the quality (Lewis et al., 2004,
are found in the north, and are overlapped by
McCarthy et al., 2011). Likewise for shales also,
younger beds in a southward direction, the
their potential of hydrocarbon potential depends
original dip being also southward in major part
on their organic matter content (Tissot et al., 1978).
of the area. The dip of the strata varies from 5º to
Moreover shales can also be interesting target
10º. Besides the boundary faults, there are also
materials for storing of carbon dioxide (Krooss et
oblique and cross faults in the field with a general
al., 2003).
strike of NW-SE dipping towards north-east. The
After US, the shale gas revolution is knocking at
field is traversed by igneous intrusions of dolerites
the doors of the Indian gas market. India, like
or basalt and micaperidotites. Swarms of mica
many other countries around the world with shale
lampropyre ultramafic dykes and sills along with
gas potential recognizes the strategic importance
dolerite dykes are found as intrusives in all the
of developing its shale gas resources. The shale
Gondwana formations in the Raniganj Basin,
gas revolution can help India to meet the rapidly
except in the Supra-Panchet beds. Dolerite dykes
growing needs of a large and developing
extend beyond the basin into the granite gneiss
population, as well as minimize the need of
floor rocks and shows a definite NNW-SSW trend.
importing natural gas or liquefied natural gas. In
Similar trend is also followed by lamprophyre
India few major basins have been identified which

13
 MPT-2013

dykes, as well as a NW–SE trend, all over the

basin. The lampropyre dykes and sills are
dated at 105–113 Ma (K– Ar, whole-rock and
mineral dating; Sarkar et al., 1980).The lower
Gondwana formations were deposited over
the Archean basement. Raniganj Basin was
initiated as a sag basin, in which Talchir and
Barakar sediments were deposited (Fox, 1931
and Gee, 1932). Subsequently, the Raniganj
Basin developed homoclinal geometry, having
a nor mal depositional c ontac t wit h the
unconformity on the underlying granite gneiss Fig. 1 Geological map of Raniganj coalfield
in the north and becoming deeper towards the (after GSI, 2003)
south . T he gen eralized str at igr ap hic
succession and the geological map of Raniganj 3. Methodology
coal basin with the study area are shown Table Total of 70 bore hole shale samples were studied
1 and Fig. 1 respectively. for assessing the shale gas potentiality, out of
Table 1 Generalized stratigraphic succession of whic h 2 (P1 and P2) belongs to Panchet
Raniganj coal basin (after GSI, 2003) Formation, 6 belongs (B1-B6) to Barakar
Age Formation Lithology Maximum
Formation, while 24 (BM1-BM24) and 38 (R1-
Thickness(m)
Recent and
Quaternary
Alluvial and residual soils; lateritic capping. 90 R38) samples belong to Barren Measures and
----------------------Unconformity-------------------- Raniganj Formation respectively. Depth varies
------------------

Tertiary Light grey mudstone and siltstone with bands 300 from 755 to 812 m for the samples from Panchet
of marlstone; white, soft fine grained clayey
sandstone, mottled clay and loose sand with
pebbles of vien quartz; occasionally lignite at
the basal part.
Formation, 773 to 1070 m for samples from
-----------------------Unconformity-------------------
------------------
Barakar Formation, while for samples from
Cretaceous
Igneous
intrusive
Basic (dolerite) dykes; Ultrabasic (mica-
peridotite, mica-lamprophyre, lamprophyre)
___ Barren Measures and Raniganj Formations it
sills and dykes.
Cretaceous Rajmahal Greenish grey to black, fine to medium 120 varies from 55.80 to 1480 m and 177.10-1370.00
Formation grained vesicular porphyritic basalt and
volcanic breccia; weathered aphanitic basalt
at places; one to five inter-trappeans
consisting of grey shale, fine grained
m respectively.
sandstone and carbonaceous shale.
------------------------Unconformity------------------
------------------ Rock Eval-VI was used for carrying out Rock-
Upper
Triassic*
Supra-
Panchet/
Massive, very coarse to coarse quartzose
sandstone, conglomeratic at places; bands of
300
Eval Pyrolysis and TOC analysis of the samples.
Durgapur dark red silty shale.
Beds
------------------------Unconformity------------------
For this, the samples were washed, dried,
------------------

Lower Panchet Coarse grained greenish yellow and greenish 600

crushed to powder and screened through BSS
Triassic* Formation grey soft, micaceous, cross-bedded sandstone
with slump structures; khaki green fissile silty
shale; alternate bands of yellow coarse
60 mesh size. The crushed samples were well
grained immature sandstone and bright
reddish brown claystone with calcareous
concretions; conglomeratic at the base.
homogenized before carrying out experiments.
Upper
Permian*
Raniganj
Formation
Grey to light grey fine and medium grained
micaceous felspathic sandstone with
calcareous clayey matrix in the upper part;
1150
Rock-Eval analysis is essentially a two step
siltstones and shales, often interlaminated
with fine grained sandstone; carbonaceous
shales and coal seams.
proc ess, involving pyrolysis in an inert
Barren
Measures/
Dark grey to black micaceous or
carbonaceous, fissile shlaes with ferrugineous
600 atmosphere (nitrogen) and combustion in an
Ironstone laminae and thin bands of dense, hard,
Shales cryptocrystalline clay ironstones; rarely
interbanded with fine grained sandstone.
oxic atmosphere (air). The pyrolysis begins by
Lower
Permian*
Barakar
Formation
with
Very coarse to medium grained arkosic
sandstones, often cross-bedded; grey and
carbonaceous shales, at times interbanded
750
heating the sample at 300 ºC which releases the
Karharbari
Formation
(?) at base.
with fine grained sandstone; fire clay lenses
and coal seams; pebbly and carbonaceous in
lower part.
S1 frac tion (mg HC/g), releasing volatile
Talchir
Formation
Tillite or diamictite with sandy or clayey
matrix at the base; medium to fine grained
500
compounds, such as short chain lipids and other
khaki or yellowish green feldspathic
sandstone; siltstone, silty shale, needle shale
and rhythmite with dropstones.
small volatile compounds. This stage is followed
-----------------------Unconformity-------------------
------------------ by a temperature rise of 25 ºC/min until 650 ºC,
Precambria
n
Chotanagpu
r Gneissic
Complex
Granite gneiss with migmatitic gneiss,
hornblende schist, hornblende gneiss,
metabasic rocks, pegmatite and quartz veins
__
which releases the S2 fraction (mg HC/g). S1 and
etc.
S2 are measured by flame ionization detection
(Explanation: *= age ac c ording to (FID). Hydrocarbons which are released during
Mukhopadhyay et al., 2010)

14
 MPT-2013

this stage are due to cracking of heavier and

larger molecules (Taylor et al., 1998; Peters et
al., 2005). Hydrocarbons that form the S2 peak
represent the present hydrocarbon generating
capability of the rock (Taylor et al., 1998). During
the pyrolysis step, S3 carbon dioxide and carbon
monoxide (mg CO/g) are measured continuously
by infrared (IR) spectroscopy. The sample is then
transferred to an oxic chamber and heated to Fig. 2 Bar diagram showing TOC content of
850 ºC, burning off all remaining organic matter shale samples from Raniganj Formation
(OM). This produces the residual carbon (RC) TOC content of the shale samples from Barren
fraction (wt % measured by IR) and the TOC is Measures Formation varies between 2.56-13.67
derived from the sum of these fractions wt % (Fig. 3) with majority of the samples
(Lafargue et al., 1998). showing excellent TOC content. Almost all the
4. Results and Discussion samples fall under early to peak mature stage
barring three samples, one of which falls in
Samples from Panchet Formation are marked immature stage and the rest two falls under post
by low TOC content (0.02-0.29 wt %). The mature stage. The HI values show input of
hydroc arbon generative potential of the predominantly type III organic matter.
samples (S2; mg HC/g rock) varies from 0.02 to
1.90 respec tively. Sample P1 (Panchet
Formation) is marked by comparatively high
HI value and S1 peak which may be due to
probable migration of gas into the upper part of
the Panchet Formation (Lower Triassic) below
the unconformity separating it from the
overlying Supra-Panchet Formation (Upper
Triassic). Tmax values of the two samples indicate
that CG-801 (340 °C) falls in immature stage
while CG-802 (463 °C) falls in late mature stage. Fig. 3 Bar diagram showing the TOC content
The low TOC content of the samples from of shale samples from Barren Measures
Panchet Formation indicates smallest amount Formation
of organic matter availability for preservation All the samples from Barakar Formation are
during Panchet Formation. marked by excellent (>4 wt %) TOC content and
38 borehole shale samples from Raniganj varies within the limit of 4.49-7.23 wt % (Fig. 4).
Formation were collected with depths ranging The HI vs Tmax plot shows input of dominantly
between 177.10 to 1370.00 m. TOC content of type III organic matter and are in early to peak
the Raniganj Formation shales shows a wide stage of maturity.
variation (0.82 to 46.28 wt %; Fig. 2). However The HI vs Tmax plot is shown in Fig. 5 and easily
majority of the samples are marked by excellent depicts the type of organic matter input and the
(> 4wt %) to very good (2-4 wt %) TOC content maximum temperature suffered by the samples
and indicates higher organic matter supply and in course of maturation and hence can be used
its better preservation. The HI vs Tmax plot shows very effec tively as a plot to evaluate
that the shales from Raniganj Formation are in hydrocarbon prospect of shales.
early to peak mature stage while few are in
immature stage and indic ates input of
predominantly type III and IV organic matter.

15

Fig. 4 Bar diagram showing the TOC content
of shale samples from Barakar Formation
Fig. 5 HI vs TMAX °C plot of all the studied shale
samples excluding those of Panchet Formation.
In the index BMF represents samples from
Barren Measures Formation, RF represents
samples from Raniganj Formation while BF
represents samples from Barren Measures
Formation.
TOC shows a strong positive correlation with
S2 (r2=0.92; Fig. 6), indicating that TOC content
is mainly c ontrolled by the remaining
hydrocarbon content of the shale samples. The
16
MPT-2013
hydroc arbon generative potential of the
samples (S2; mg HC/g rock) from Barakar, Barren
Measures, Raniganj and Panchet Formations are
placed within the range of 2.07-3.91, 2.56-13.67,
0.37 to 71.94 and 0.02 to 1.90 respectively.
Fig. 6 Relationship between TOC content and
S2 content of all shale samples
5. Conclusions
The above results indicate that among the four
formations studied, apart from shales of Panchet
Formation, the shales samples from all the other
three formations viz. Barakar Formation,
Barren Measures Formation and Raniganj
Formation have very good to good hydrocarbon
generative potential. However shales from
Panchet Formation, especially those lying in the
vicinity of the unconformity with Supra-
Panchet Formation, inspite of having very small
TOC content may have migrated free gas
trapped in it and hence can be the zone of
interest. Rock Eval Pyrolysis and TOC analysis
shows that Barakar Formation, Barren
Measures Formation and Raniganj Formation
of Raniganj coal basin may be zones of potential
interest.
References
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production, Fort Worth Basin: issues and
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organic matter distribution and methane
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of maceral composition on geochemical
characteristics of immature shale kerogen:
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gas-shale play with multi-trillion cubic foot
potential. AAPG Bulletin. 89, 155–175.
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(unconventional) gas accumulation, Fort
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Member, northeastern British Columbia,
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integrated formation evaluation. American
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Sengupta, N. R., 1980. Lamprophyres from
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Strapoc, D., Mastalerz, M., Schimmelmann A.,
Drobniak A., Hasenmueller, N. R., 2010.
Geochemical constraints on the origin and
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(Devonian–Mississippian), eastern Illinois
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and Occurrence Part V, Ch. 1. Springer-
Verlag, Berlin, Heidelberg, New York.

******

18
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Characterization of Minerals in Coal - Development of A Novel

Device Thereof for Quick Isolation of Minerals

S. Kumari1, T. Gouri Charan2, S.C. Maji2, M.K. Saini2, G. Udayabhanu1 and A. K.

Bandopadhyay2*
1
Indian School of Mines, Dhanbad, 826004, Jharkhand, India
2
CSIR-Central Institute of Mining and Fuel Research, Dhanbad, 826015, Jharkhand,
India

Abstract
Characterization of minerals in coal provides data which are useful in various coal related pro-
cesses, viz mining, correlation of seams and sub-seams, beneficiation, combustion, gasification,
carbonisation and liquefaction. Indian coals are of drift origin and therefore, they are rich in miner-
als, which need to be characterized in detail for better utilization of coals. Minerals do not con-
tribute to the heat value of coal, but their deleterious effects in any coal conversion process make
their characterization indispensable for working out an abatement strategy. Isolation of minerals
intact from coal prior to characterization by instrumental techniques is essential as the carbon
matrix interferes in the process of quantitative estimation of minerals. But the existing process of
isolation by oxygen plasma, a standard technique used worldwide, is a cost-intensive and time-
consuming process, which stands in the way of its use as a routine tool.
The present communication reports a novel device, which oxidises rapidly the organic part of
coal in a flow of oxygen leaving behind the inorganic part almost intact. The device is robust, low
cost, rapid and less sophisticated requiring little maintenance. It has been found to be capable of
isolating the major minerals in Indian coals of diverse types, non-coking and coking. The time for
extraction of minerals depends on the instrumental parameters, viz the flow rate of oxygen and
temperature of oxidation. At a flow rate of 0.2 l/min and temperature of 3500C, time of isolation of
minerals could be as low as 8 hrs, which has not yet been reported. Investigations on composition
of the inorganic residues obtained under these conditions using FTIR and XRD have revealed that
kaolinite and quartz are the major constituents along with other minerals, viz illite and carbon-
ates, occurring in smaller proportions.
The low-temperature ash yields obtained from the device and from the oxygen plasma asher
have been compared. The results from the two methods are found to agree well when the results
from plasma ashing are corrected for the unburnt organic residues. Further, the XRD and FTIR
spectra of the low-temperature ashes obtained from the device compared favourably with those
from the plasma asher, justifying thereby the appropriateness of extraction of minerals using the
simple device. Notably, as the temperature of the device can be accurately controlled, moisture in
Corresponding Author: Dr. A.K. Bandopadhyay, Advisor to Silica Project and Ex-Chief Scientist , RPL Division,
CIMFR, Dhanbad-826015, Jharkhand, India Contact no. +919431377405 Email: akban2002@rediffmail.com

19

coals were determined and the results agreed with those from standard determination. The de-
vice, therefore, holds promise for application in industry for determination of mineral matter and
subsequent analysis of minerals along with other applications, viz moisture determination and
proneness of oxidation of coal.
Keywords: Coal; ashing; minerals; FTIR; XRD.
1. Introduction
Characterization of minerals in coal provides
data which are useful in various coal related
processes, viz mining, correlation of seams and
sub-seams, beneficiation, combustion, gasifi-
cation, carbonisation and liquefaction. More
than a hundred minerals are documented and
they are classified under clays (silicates),
sulphides, sulphates, phosphates and oxides
(Van Krevelen, 1993; Vassilev and Vassileva,
1996; Ward, 2002). However, the number of
minerals actually found in coals of a country
depends on their origin and geological forma-
tion. Indian coals are of drift origin and there-
fore, they are rich in minerals, which need to
be characterized in detail for their better utili-
zation. Notably, minerals do not contribute to
the heat value of coal, but their deleterious ef-
fects (Ward, C.R., 2002; Pinetown and Boer,
2006; Van Dyk et al., 2009) in any coal conver-
sion process make their characterization essen-
tial for knowing possible interference and
working out an abatement strategy.
At present the data on ash yield of coal and ash
analysis provide inputs to assessing coal from
utilisation point of view, as the deleterious ef-
fects induced by minerals can be predicted in-
directly (Raask, 1985; Van Krevelen, 1993;
Meenakshi et al., 1997; Tickner and Maier, R.W.,
2005; Ritz and Klika, 2010). However, direct
characterization of minerals is highly signifi-
cant for a number of reasons in coal science
and technology and for assessment of the envi-
ronmental effects of the minerals during min-
20
MPT-2013
ing and utilisation. First, the minerals are the
constituents of coal that participate in the coal
conversion processes. Hence their determina-
tion is essential for understanding both their
individual effects and collective alterations, if
any, during any process. For example, recently
it has been demonstrated (Bandopadhyay,
2010a, 2010b; Shobha et al., 2012) that direct
determination of quartz, one of the major min-
eral constituents in most coals, and its abun-
dance in Indian coals is useful for correlation of
abrasive propensity of thermal coals with
quartz contents. Secondly, the knowledge of
minerals helps in correlation of seams and sub-
seams (Ward, 2002). Thirdly, quantitative
analysis of the minerals present in coal also
helps to fix acid mine drainage problems
(Pinetown et al., 2007) and helps in prediction
of the presence of heavy elements that that are
known to cause environmental pollution
(Ward, 2002). Fourthly, for conversion of the
testing and analytical results of coal obtained
on air dried basis to dry mineral matter free
basis.
But characterization of minerals requires their
prior isolation from coal, as the organic matrix
of coal interferes in the analytical process us-
ing instrumental techniques, viz Fourier Trans-
form Infra-Red Spectroscopy (FTIR) and X-ray
Diffractometry (XRD). However, isolation of
minerals is not as easy as the determination of
ash at 8150C because of several problems. The
standard technique, that is universally ac-

cepted now, is the low-temperature plasma
ashing (Gluskoter, 1965; Mahajan, 1985; Ward,
2002; Pinetown et al. 2007; López and Ward
2008; Bond and Giroux, 2013). However, the
method is time consuming, cost intensive and
not so perfect as to produce exactly the same
minerals in unaltered form as are present in
coals. Therefore, with these limitations, the oxy-
gen plasma asher technique has remained con-
fined as a research tool for mineral investiga-
tions.
It is in the above mentioned context, develop-
ment of a device, which is low-cost, less time
consuming and less sophisticated requiring a
little maintenance so that it is readily accept-
able in coal industry as a routine tool, is essen-
tial. The present communication describes a
method which can rapidly oxidise coal (also
other carbonaceous substances) in a flow of
oxygen reducing the time of isolation of miner-
als significantly and compares the results with
those of plasma asher. Further, the applications
of this device as an aid to mineral character-
ization and determination of moisture content
of coals have also been discussed.
2. Materials and Methods
The various steps taken to accomplish this
work are detailed in the following paragraphs:
2.1 Selection of coal samples
Two coals of diverse nature, one non-coking
while the other coking, were selected for the
study. The former was c ollec ted from
Vasundhara mine of Ib Valley Coalfield and the
latter from Kathara mine of East Bokaro
coalfield. The coal samples after proper
sampling were crushed to -72 BS mesh and then
subjected to ash and moisture determinations
as per IS: 1360 Part1 [13]. The results are
included in Table 1.
2.2 Development of low-temperature asher
21
MPT-2013
The low-temperature asher was designed and
constructed in the laboratory. Figure 1 shows
its basic features. It is basically a modification
of high-temperature muffle furnace used for the
determination of ash. The muffle is made of sil-
limanite which can withstand a high tempera-
ture of 14000C The muffle is wound with im-
ported Kanthal A1 heating element, which has
high current carrying capacity and can main-
tain a high temperature of 10000 C within the
heating space of the muffle. The selection of
these materials endows high longevity to the
device as the experimental temperature for this
work never exceeds 4000C.
Fig.1: Basic layout of the furnace, showing
regulated supply of oxygen and electrical con-
nections with the digital controller
The muffle is surrounded by ceramic wool blan-
ket supported by refractory bricks. The tem-
perature inside the furnace is indicated and
controlled digitally. The preset temperature on
the control panel can be varied by rotating the
adjustable screw on the controller and simul-
taneously pressing the set bottom. The asher is
c onnected to the mains through a relay
contactor which is digitally controlled by elec-
trical signal from the control unit. Tempera-
ture inside the furnace is sensed by PT -100
sensor (class 2B as per IEC 751:1983). The out-
put of the sensor is fed to the controller to main-

tain the temperature of the asher at the set
point. The low-temperature asher has a hole
at the centre through which oxygen gas (com-
mercial grade) can be made to flow at a desired
rate measured by a flowmeter, as shown in Fig-
ure 1. The flowmeter can read gas flow rates
from 0 to 1 l/min. The asher was calibrated
against a standard Fluke 52 digital thermom-
eter with J-type thermocouple as sensor. It has
been found that the readings of the digital read
out of the furnace and the Fluke readings agreed
reasonably well (within ± 20C). The tempera-
ture inside the asher was found to be maxi-
mum in the middle and slowly varied up to a
maximum of 100C on either side of the middle
of the asher. The silica dishes (diameter 56 mm)
containing samples to be ashed were, therefore,
placed as close to the tip of the thermocouple as
possible so that the samples were heated to
temperature indicated by the digital thermom-
eter.
2.3. Low-temperature ashing of samples
The capability of the asher was tested with
various types of carbonac eous samples
including PVC membrane filter, rice husk, pitch
coke and coal samples. It was found that PVC
membrane filter could be ashed with no residue
at 4000C at an oxygen flow rate of 0.2 l/min. The
rice husk could be ashed in about 24 h at 4000C
with 0.2 l/m flow rate of oxygen. But in similar
conditions a longer time was required for pitch
coke. The selected coal samples of size -72 BS
mesh and weight 0.5g each were taken in silica
dishes of diameter 56 mm and spread over the
dishes uniformly with sample thickness of
0.0255 g/cm2. Each of the samples was taken in
four silica dishes so that the amount of ash
obtained was suffic ient enough for
characterization. The flow rate of 0.2 l/m and
temperature 350 0C were maintained for
oxidising the coal matrix and after every 2 hrs
the discs were taken out and weighed. After
22
MPT-2013
stirring the samples, they were put in the asher.
It was found that after 8 hrs the weights of the
dishes containing the samples were constant,
thus indicating complete ashing.
2.4. Effect of particle size
To study the effect of particle size on the
oxidation of coal taking place inside the asher,
powdered coal of -72 BS mesh size was further
ground to still lower sizes passing through 100
BS mesh and 200 BS mesh, respectively. The
coal samples with these sizes were then
subjected to ash and moisture determinations
following the IS specifications [13]. The three
samples were then ashed at 3500C for 8 hrs in
the asher till constant weight was achieved
for each. The process is illustrated in Figure 2.
Fig.2: Variation in weight of coal samples of
various sizes with time
The moisture and ash percentages are recorded
in Table 2 along with the low-temperature (LT)
ashes.
Table 1: Variation of moisture, ash and LT ash
of Ib Valley coal with particle size
Particle size Moisture (% wt./wt.) Ash (% wt./wt.) LT Ash (% wt./wt.)
-72 BS mesh 2.6 56.7 (58.2) 61.7 (63.4)
-100 BS mesh 2.5 56.8 (58.2) 61.46 (63.1 )
-200 BS mesh 2.7 56.8 (58.4) 61.76 (63.5)
*The results within the parentheses are on dry
basis
2.5. Plasma ashing
 MPT-2013

prior to taking XRD. The diffractograms are

The low-temperature plasma ashing of coal shown in Figure 4.
was done in a plasma asher (model K1050X by
EMITECH,UK) in an oxygen flow of 7 ml/min
with power 50W. 1.5 g coal was taken for ashing
80
and the sample was intermittently shaken for Plasm a Asher

Transmittance
removal of the organic matrix. It was found that 60

after 11 hrs there was no reduction of weight of

40
the sample. The weight was noted and this
weight was compared with low-temperature 20 LTA A sher

ashing done with laboratory developed asher, 600 800

W ave num ber (cm )

1000
-1
1 200

as shown in Table 2. In either case of ashing

technique, powdered coal of 72 mesh size was Fig.3: FTIR spectra of the low-temperature
used. ashes from LT asher developed in the labora-
tory and the plasma asher
Table 2: Comparison of mineral matter
obtained from LT asher and plasma asher q

along with moisture and ash values of the 400

Lin (Counts)

k
200
selected coals q
q

0
Mineral matter from low-
P la s m a L T A
Ash Mineral matter from
Coal
Moisture tem- perature ashing
plasma ashing 600 0 20 q 40 60 80
(%wt./wt.)
Lin (Counts)

(%wt./wt.) (% wt./wt.)
(%wt./wt.)
400
Ib Valley 2.7 56.8 (58.4) 61.8 (63.5) 67.5 (69.4)
200
k q
Kathara,E 1.8 28.2 (28.7) 30.3(30.9) 31.1 (31.7) q
ast
0
Bokaro LTA Asher
0 20 40 60 80
2 -T h e ta - S c a le

*The results within the parentheses are on dry

Fig.4: XRDs of the low-temperature ashes
basis
from LT asher and the plasma asher (K- ka-
olinite and q- quartz)
2.6. Characterization of minerals by FTIR and
XRD
Investigation of minerals in LT ash and plasma
2.7. Moisture determination for coals using the
ash was done by FTIR and XRD, which are ex-
LT asher
tensively used in mineralogic al analysis
As the asher could be adjusted accurately at
(Huggins, 2002). The FTIR spectra were re-
the set temperature within ± 20C, it was used
corded on Perkin-Elmer model Spectrum RXI
for moisture determination of coal samples
at a resolution of 2cm-1. The spectra were taken
taken in standard moisture crucibles. The LT
on KBr matrix with a concentration of 0.5% wt./
asher was set at 1080C and coal samples with a
wt. The spectra are shown in Figure 3. Identifi-
range of moisture contents (1-10%) on air dried
cation of the minerals in the samples were car-
basis were kept in the asher in duplicate. The
ried out using D8 Foc us Bruker X-ray
moistures determined were compared with
Diffractometer with copper target and a scan-
those obtained following IS specifications [13].
ning rate of 0.2 sec/step and increment of 0.030
The results are shown in Figure 5.
degree. Each of the ash samples was ground

23
 MPT-2013

Therefore, the mineral matter determined from

the low-temperature ashing is reasonable.
Similar agreement between results was also
obtained for Kathara coal.
It is to add here that the LT method may suffer
from a drawback, similar to that of plasma
asher, viz., alterations of minerals like pyrite.
But since most of the Indian Permian coals
contain very low sulphur (less than 1% and
hence pyrite still less), the device is, therefore
Fig.5: Results of moisture determinations
appropriate for Indian coals.
Table 1 shows the variation of moisture, ash
3. Results and Discussion
and LT ash of Ib valley coal with particle size
Air oxidation of coal at temperatures below
obtained after sieving with various sieves (72
4000C as an alternative to plasma ashing for
BS , 100 BS and 200 BS). It is observed that the
extraction of minerals from coals has been in
ash and moisture of the samples have not prac-
vogue since 1959, when it was demonstrated
tically changed and so also the LT ash. This re-
(Brown et al., 1959) that direct determination
flects that LT ashing is little influenced by par-
of mineral matter in Australian coals was
ticle size for the sizes of particles considered.
possible by heating coals at 3800C in a muffle
Therefore, coal of -72 BS mesh size can be used
furnace for protracted periods (H”120 hrs).
for low-temperature ashing.
Since then many workers (Mukherjee and
Prima fac ie the low-temperature ashes
Srivastava, 2005; Pinetown et al., 2007) applied
determined by the low-temperature asher and
this technique at temperatures around 3500C
the plasma asher do not tally and the results of
for isolation of minerals for their
the plasma asher are higher (Table 2). The
characterisation. In this work, temperatures
reason for the discrepancy was investigated
lower than 3500C were tried. It was found that
and it was found that the ashes obtained with
in controlled flow of oxygen (0.2 l/min) at 3000C
plasma asher contain organic matter (i.e.,
a time of 24 hrs was required to completely
complete oxidation has not taken place), 6.2%
oxidise coals. The same results were obtained
in Ib Valley coal and 1 .0% in Kathara coal,
when the coals were heated at 3500C for 8 hrs
respectively. Such incidence of carbonaceous
in an oxygen flow of 0.2 l/min. Therefore, this
residue remaining after ashing by plasma asher
set of experimental conditions was followed for
was reported earlier (Mahajan, 1985). If the
all experimental works. The efficacy of this set
weights of the carbonaceous organic residues
was tested with the selected Indian coals. For
are subtracted from ashes of plasma asher, the
example, Ib valley coal has a high ash yield
weights of ashes obtained for both the coals
(58.2%). Using a conversion factor of 1.1, as is
are in excellent agreement with those from LT
done for Indian coals to convert ash to mineral
asher. This gives credence to the results
matter, the coal would yield 58.4*1.1= 64.2%
obtained with the LT asher developed in the
mineral matter. The actual yield, as shown in
laboratory.
Table 1, is 63.5%. The discrepancy between the
The minerals found in the coals studied are
experimental and the theoretical mineral
mainly kaolinite and quartz, as shown in Fig-
matter yields is very small (within 1%).
ures 4 and 5. The composition of minerals is

24

such that they do not undergo change at low
temperature heating (< 4000C), thus favouring
ash to be produced at 3500C without any ap-
preciable alteration. The supply of oxygen rap-
idly oxidises the coaly matrix, making it fea-
sible for rapid isolation of minerals to take place.
The FTIR spectra shown in Figure 4 are not only
similar but of nearly equal in intensity with
respect to bands at 915 cm -1 due kaolinite and
800 cm-1 due to quartz. This indicates that the
composition of the minerals in the LT ash that
of plasma is identical. Further, the XRDs of the
LT ash and the plasma ash are similar indicat-
ing the minerals in both samples are identical.
It is encouraging to note that the low-tempera-
ture device developed has opened up scope for
investigation on minerals in Indian coals.
Another interesting point to note is that results
of moisture determination of a number of coals
with the LT asher tallied well with those of
plasma asher (Figure 5). This, however, is not
the main application of the LT asher, but a job
that may be tried in case of necessity. The de-
vice is very flexible. In the absence of oxygen,
air oxidation of coal for protracted periods de-
pending on selected temperature can be car-
ried out for mineral extraction. This is an ad-
vantage if time is not a factor for mineral analy-
sis to be carried out.
4. Conclusions
Mineral characterisation of coal is an integral
part of coal c harac terisation for proper
utilisation of coal. Isolation of minerals intact
is essential prior to characterisation by FTIR
and XRD. The laboratory developed low-tem-
perature asher has shown promise for isola-
tion of minerals in Indian coals rapidly, accu-
rately and at a significantly low cost compared
to the standard plasma ashing technique. Pow-
dered coal of size 72 BS mesh has been found to
be useful for ashing in 8 hrs in the low-tem-
perature device. The major minerals in the
25
MPT-2013
ashes prepared are found to be kaolinite and
quartz in the two Indian coals studied. Abun-
dance of these minerals together with low per-
centage of pyrite (< 1%) has been main reason
for the success of the laboratory developed
asher as at the ashing temperature (3500C) no
significant alterations of the minerals are likely
to take place. The device is flexible as it can be
operated for ashing without any flow of oxy-
gen, but in this case the ashing time will be
more.
Acknowledgements
The authors are grateful to CSIR-CIMFR for
encouragement and permission to publish the
paper.
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Characterisation of PGE Mineralisation at Boula Nuasahi Igne-

ous Complex, Odisha, India
M. S. Jena1*, D. Dash1, J. K. Mohanty1, N. R. Mandre2 and R. Venugopal2
1
CSIR - Institute of Minerals & Materials Technology, Bhubaneswar
2
Indian School Mines University, Dhanbad

Abstract

PGEs are of strategic importance due to their growing use in advanced technology and rarity in
occurrence. PGE mineralization is found in various rock types, stratigraphic levels and geotec-
tonic set up. Most important deposits occur as reefs in layered intrusions of Archean to Protero-
zoic age. Boula Nuasahi Igneous Complex is the only proven PGE deposit in India. PGE mineral-
ization is confined to a 3 km long breccia zone. This breccia zone is the manifestation of late
intrusion of Bangur Gabbro at the contact of ultramafic and mafic rocks in the eastern part of the
complex. This zone is a heterogeneous assemblage of randomly oriented angular to sub-rounded
blocks/ fragments of chromite, ultramafic rocks which are pervaded by the leucogabbro and
clinopyroxenite. PGE minerals are associated with oxide, sulfide and silicate facies. Chromite and
base metal sulfides are principal hosts for PGE mineralisation. Pt dominant PGE mineralisation
in chromite is pronounced in the southern part and Pd dominant PGE mineralization in base
metal sulfides is prevalent in the northern part of the breccia zone. The mineralisation has both
magmatic and hydrothermal signatures. The mineralisation in the southern part is presumed to
be magmatic where as mineralisation in northern part is hydrothermal in nature.

PGMs are mostly present as inclusions and exsolution in chromite and BMS. PGE contents of the
rocks of the breccia zone vary from <1 ppm to 5 ppm. PGMs are mostly associated with sulphides,
arsenides, tellurides besides present in alloy form such as Isoferroplatinum. Important minerals
are sudburyite, braggite, laurite, sperrylite, merenskyite, hollingworthite, malanite,
isoferroplatinum etc. Grain size varies from <2 µ to 50µ with an average size of around 15µ. The
grade of mineralization is very poor compared to world scenario. Magnetic separation and flota-
tion methods of beneficiation can be tried upon to pre-concentrate PGE values from this low
grade ore.

Keywords: PGM; ferritchromite; sulfide; BNIC; Odisha.

1. Introduction
PGEs comprise a group of six grayish to silver
Corresponding Author: E-mail: white elements. These elements have similar
msjena@immt.res.in geochemical behavior and tend to be concen-

27

trated together geologically. They don’t occur
as independent natural ores but are mostly
found as tellurides, arsenides, antimonides,
sulphides and various complicated mineral
phases. They are divided into two groups: IPGE
(Ir, Os, Ru) and PPGE (Pt, Pd, Rh) depending on
their refractory nature and temperature of for-
mation. Out of the six, platinum, iridium and
osmium are very heavy (sp.gr.>12) where as
palladium Rhodium and ruthenium are light
(sp.gr.<12) metals. They all have commonality
of extreme rarity in occurrence on the surface
of the earth and attractive appearance with
noncorrosive qualities even with long use and
normal exposure to the ambience and the envi-
ronment. Their crustal abundance is very low
(less than sub-ppb level to maximum 10 ppb)
and PGE deposits are too few in number com-
pared to other metalliferous or more specifi-
cally other precious metal deposits of the world.
PGE and Au are strongly siderophile and
chalcophile and exhibit different associations.
Because of an aversion to bonding with oxy-
gen, PGE-Oxide mineral is rare and the PGEs
are scarce in the crusts and concentrated in the
core-forming Fe–Ni alloy.
With ever increasing application of the mod-
ern technologies at various industries, the de-
mand of the PGEs has increased many folds.
They find application in chemical and petro-
chemical industries, electrical and electronics,
glass, jewellery and medical sciences. Utility
in electronic sector is increasing day by day
where the elements are used to increase the ef-
ficiency of many storage devices and chips.
With high melting point and resistance to
chemical attack, these elements find uses in
production of high purity single crystals for a
variety of applications, high quality optical
glasses. Owing to their biocompatibility, high
electrical conductance and resistance to corro-
sion, Pt and Pt-Os alloys are essential compo-
28
MPT-2013
nents of implant devices used for treatment of
heart ailments. Platinum and palladium are
mixed with ruthenium and/or iridium to pro-
duce alloys for dental restorations.
Multifarious applications have increased the
demand for PGE at a faster rate. Due to rare
occurrence, discovery of new PGE deposits/
mineralized zones as well as recovery from
very low grade sourc es by suitable
beneficiation-extraction processes will enhance
the resource base of PGE in world. The total
world reserve is 66110 t with metal content of
2125 million oz tr (Table 1). Economically min-
able world resources of PGM in mineral con-
centrations are estimated to total more than
100,000 t (3.2 million troy ounces) (USGS, 2011).
Table 1: World reserve of PGE
Country PGM, t PGM, M oz tr Share, %
South Africa 63000 2025 95.3
Russia 1100 35 1.7
USA 900 29 1.4
Canada 310 26 0.5
Others 800 10 1.2
Major PGE deposits are mainly confined to S.
Africa and Russia. South Africa is the leading
producer (58%) followed by Russia (28%) and
Canada (5%) of Pt+Pd. South Africa production
centers on the Bushveld Complex where the
PGM bearing ores are being primarily mined
for the recovery of these metals. Canada’s PGE
are by-products of nickel–copper mining, pri-
marily from Falconbridge’s and Inco’s deposits
in the Sudbury area. The major deposits and
occurrences are shown in Fig. 1.
The total Indian demand is met by export. In-
dian lacks any deposit of significance till date
except a very low grade deposit at Odisha. This
paper describes style of PGE mineralisation,
mode of occurrence of PGE and the problems
associated with beneficiation of such ore from
a mineralogical perspective.
 MPT-2013

Norlis’k Talnakh East Chuarv i

Portimo-Penicat
Com plex (Finland) (Russia) Kola Peninsular
(Russia)
2. Boula Nausahi Igneous Complex
Sudbury(Canada ) *
Jinchuan Intrusion
Ni-Cu-PGE deposit
(China)

*
* PGE mineralisation at Boula area was first re-
ported by Nanda & Patra (1993) and later on
... .
Stillwater Shimoga schist
Complex,Montana (USA) belt
Baula-Nausahi
confirmed by detail geological and geochemi-
Sittam pundi-Karungalpatti
Anorthosite Com plex cal work, jointly carried out by GSI and BRGM,
Great Dyke
(Zimbabwe) *
*
France. It is estimated the reserve to be around
Index

.
* Major Deposit
Reported occurrences
Kalgoorlie 14.2 million tone having 24935 kg of Pt+Pd. But
Bushveld
Coronet Hill
Complex
(Australia) the grade is very poor (“PGE H”1.5 ppm). This
concentration is too low for any commercial
Fig. 1: Important PGE deposits of world exploitation.

India is very poor in PGE resources. However 2.1. Geological setting

c ontinuous endeavour by GSI for PGE
mineralisation in different parts of the country Boula Nuasahi ultramafic-mafic complex lo-
has resulted in finding out some possible lo- cated in the south eastern part of the Singbhum
cales that need detail investigation. Among Craton in the Eastern Indian shield hosts one of
them, the important ones are Sittampundi An- India’s most significant chromium reserves.
orthosite Complex, Tamil Nadu (“PGE - 0.5-18 This complex, pitted on the western flank of the
ppm ,Nathan et al., 2009), Channagiri - 55 km long ENE-WSW trending Nilgiri-
Hanumalapura complex, Karnataka(“PGE ~2 Nausahi belt, is bounded between 21º15' N to
ppm to 6.25 ppm, Devaraju et al. ,2009), Ikauna- 20º18' N latitudes and 86º18' E to 86º20' E longi-
Dangli area, Lalitpur District (“PGE > 1.5 ppm) tudes (Fig. 3). The complex represents a well
and Madwara Igneous Complex, Bundelkhand differentiated rock series represented by ultra-
massif, Central India (Singh & Farooqui , 2009). mafic, mafic and felsic rocks. The ultramafic
In Orissa, PGE occurrences have been reported body is a 3km long and 0.5km wide pluton that
from Boula-Nuasahi igneous complex (Nanda trends in a NNW-SSE direction in northern part
and Patra, 1993; Mondal and Baidya, 1997; and N-S direction in southern part and hosts
Auge et al., 2002), The possible prospective PGE three chromite lodes. The estimated chromite
deposits as envisaged by geological Survey of reserve is around 8.2 MT of all grades. Dunite,
India are shown in the Fig. 2. peridotite and pyroxenite are the major rock
types of the ultramafic unit. The ultramafic
rocks are extensively altered to serpentinite,
Madw ara-Ikauna Ultramafic Naga-Manipur Hills
Complex in Lalitpur
Dist.,UP
Ophiolite Belt
(>0.3  g/g Pt)
talc-serpentine schist and talc-serpentine-chlo-
rite schist. Magnesite is commonly present in
Deccan Traps
these altered rocks. The mafic rocks represented
(>0.05  g/g  PGE
Baula-Nuasahi
Layered
by gabbro, norite and anorthosite host Ti-V-
Ultramafic
Complex magnetite ore bodies. With the discovery of PGE
Hanumalpur (Shimoga) (>9.7g/g Pt)
Silicate + Chromite Type
PGE-mineralisation
mineralization in 1993 the complex became
(>1.2 g/g Pt & >3.4 g/g Pd) Sittampundi Layered
Complex (>4.67 g/g
 PGE)
very important in mineral map of India. Since
then geoscientist from various disciplines are
Fig. 2: India map showing PGE occurrences engaged in exploration and resource evaluation

29

of PGE in this complex (Mondal et al., 2001; Auge
et al., 2002). The PGE mineralization is confined
to a breccia zone lying to the east ultramafic
unit. The complex has been affected by later
faulting, shearing and open folding. ENE-trend-
ing faults and shear zones are more prevalent
than NNW-trending faults.
Fig. 3: Geological map of Boula Igneous
complex
2.2. Chromite mineralization
The complex hosts three chromite lodes viz.
Durga, Laxmi and Ganga-Shankar composite
lode from south to north within the ultramafic
rocks. The ultramafic suit consists of inter lay-
ered sequence of chromite bearing ultramafic
rocks. The Durga and Laxmi lodes occur in the
chromite bearing dunite-peridotite while the
Shankar-Ganga composite lode is hosted in
pyroxenite. The lodes exhibit a continuum from
disseminated chromite to layered chromite fol-
lowed by massive chromite. Chromites of
Durga and Laxmi lode are normal chromite
where as chromite from the Ganga-Shankar
composite lode is magnetic in nature. Later in-
trusion of Bangur gabbro has severely affected
the chromite lodes.
Chromite, the major primary mineral, occurs
as euhedral to subhedral grains. The chromite
30
MPT-2013
grains form a compact granular mosaic in
chromitite and show a variety of cumulus tex-
tures. Chromite also exhibits different primary
and secondary textures like granular, foam
(auto-annealing), brecciated / mylonitised,
banded, pull apart, corrosion and alteration
textures. Based on physical & optical proper-
ties, two types of chromite are identified viz.,
normal chromite and ferritchromite. Normal
c hromite has lower reflec tivity and
ferritchromite has higher reflectivity. The mi-
cro-hardness of the chromite varies from 1200
to 1458 (VHN). The normal chromite is non-
magnetic with very low magnetic susceptibil-
ity whereas the ferritchromite is highly mag-
netic in nature. The chromite grains contain
inclusions of various shape, size and composi-
tion. The normal chromite has olivine and
enstatite as inclusions where as ferritchromite
has diopside, amphibole and muscovite inclu-
sions. Ferritchromite also contains ilmenite
exsolution and vermicular chalcopyrite. Sec-
ondary sulfide minerals (millerite and pyrite)
are confined to the matrix and formed due to
alteration of the ultramafic host rocks. The two
types of chromite show different alteration
characters. Normal chromite may have formed
at an early stage where as ferritchromite crys-
tallized at a late stage of chromite crystalliza-
tion.
2.3. Breccia Zone
In the eastern part of the ultramafic belt, on the
hanging-wall side of the orthopyroxenite unit,
a NNW-SSE trending breccia zone is developed
due to intrusion of coarse grained Bangur gab-
bro. The breccia zone is 1 to 40 m thick, almost
continuous over a length of 2000 m and shows
marked vertical and lateral variations. It cuts
obliquely across the ultramafic succession, in
particular at the level of Ganga-Shankar
chromite layer.

Fig. 4: Schematic diagram showing irregular
distribution of rocks & chromite in the
breccia zone
The Breccia Zone is characterized by a hetero-
geneous assemblage of randomly oriented an-
gular to sub-rounded blocks of chromite/
chromitite, dunite, peridotite, serpentinite, py-
roxenite whic h are pervaded by the
leucogabbro and clinopyroxenite (Fig. 4). Sul-
phide enrichment is found in the matrix mate-
rial. The breccia matrix is predominantly py-
roxene-rich gabbro showing hypidiomorphic
texture formed of cumulus plagioclase and py-
roxene which are hydrothermally altered.
Coarse grained gabbroic rock encloses ran-
domly disposed dunite and pyroxenite frag-
ments (Fig. 5a). Fine grained, rounded massive
and disseminated chromites of earlier genera-
tion are embedded in an altered pyroxenite and
gabbroic matrices (Fig. 5b). Towards the south-
ern part of the breccia zone, chromite nodules
of varying sizes are engulfed within coarse
grained gabbro (Fig. 5c). Presence of vermicu-
lar chalcopyrite in ferritchromite is a striking
textural feature indicating late stage formation
for the chromite of Ganga-Shankar lode (Fig.
5d). The matrix rock is mineralized with vari-
able PGE concentrations in both sulphide and
non-sulphide carriers.
31
MPT-2013
Fig. 5.a. Random distribution of fragments of
dunite and pyroxenite in a gabbroic rock, b.
Rounded chromitite of different size in a py-
roxenite matrix, c. Nodule shaped chromite as
enclaves in a coarse grained gabbro, d. ver-
micular chalcopyrite in ferritchromite
The Pegmatitic gabbro in the southern part of
the Breccia Zone is porphyritic with large
subhedral to anhedral crystals of pyroxene and
plagioclase. The primary texture is obliterated
by hydrothermal alteration, with the forma-
tion of amphibole. Clinopyroxene, amphibole
(tremolite-actinolite, cummingtonite) and pla-
gioclase are the principal minerals. Plagioclase
shows granular texture with deformed twin-
ning and strain effect. The gabbro with
c hromite nodules is c omposed of large,
euhedral, c umulus plagioc lase c rystals,
poikilitically overgrown by clinopyroxene, lo-
cally showing pegmatoid texture. Plagioclase
(labradorite), augite and hypersthene are es-
sential minerals. Chromite of different sizes is
present with interstitial plagioc lase,
c linopyroxene and partly altered
orthopyroxene.
Sulfide mineralization occurs in the matrix of
the breccia zone and more commonly within
the chromitite fragments. Sulfides occur as
veins, stringers, and irregular pockets in the
matrix rocks of the breccia zone. The gabbroic
rocks in the hanging wall portion of the breccia
 MPT-2013

zone contain disseminated sulfides in intersti- of Naldrett (2004) and closely similar to Lac
tial spaces of silicates. Concentration of sulfides des Iles deposit (Hinchey et al., 2005).
in chromite-sulfide assemblage is more in the Broadly speaking, two types of mineralization
northern part than the southern part of the have been identified in the breccia zone de-
breccia zone. pending on the prime PG element, principal
host mineral and the environment of
Primary sulfide minerals viz.. chalcopyrite, mineralisation. They are type 1 and type 2.
pyrrhotite, pentlandite and pyrite occur in Type-1 mineralisation has taken place in a sul-
ferritchromite- and sulfide- rich breccia zone. phide poor magmatic environment within the
(Mohanty, 1994). PGE bearing sulfide minerals Bangur gabbro, near its contact with the ul-
have been reported from matrix materials of tramafic complex. This is characterized by high
altered pyroxenite in the Breccia Zone of the platinum (upto 14ppm) and low Pd contents
composite Ganga- Shankar lodes of Boula- (between 0.8 and 1 ppm) and high Pt/Pd value
Nausahi Complex. It is observed that the brec- (8-9) and prominent towards southern part of
cia zone consists of varieties of rock types in- the breccia zone. The mineral assemblage is
cluding chromite. The rock types are analysed dominated by isoferroplatinum, braggite,
for their PGE content to find out the major host malanite, sperrylite and laurite. In this asso-
and the data are given in Table 2. ciation, PGM occur mainly as inclusions in
ferritchromites and associated silicates (plagio-
Table 2: PGE in different rock types of the clase, pyroxene). Type-2 mineralisation is re-
breccia zone (in ppm) stricted to the hydrothermally altered matrix
Elements Gabbro Pyroxenite Dunite BMS Normal Ferritchromite of the breccia zone towards its northern part
(N= 20) (N=10) (N=5) (N=5) Chromite (N=10)
(N=5) and associated with the base metal sulphides
Pt 0.003 -.290 0.003 - 1.580 0.012 0.644 - 1.245 0.008 - 0.102 0.265 - 2.395
Pd 0.002 -.44 0.007 - 2.876 0.011 1.417 - 2.876 0.007 - 0.050 0.228 - 2.672 and ferritchromite. Depending on base metal
Ru 0.002 - 0.114 0.001 - 0.218 0.046 0.04 - 0.171 0.023 - 0.074 0.054 - 0.31
Ir 0 - 0.052 0.0002 - 0.110 0.011 0.01 - 0.062 0.001 - 0.066 0.015 - 0.039 sulfide content, this is divided into two sub-
Rh 0.0002 - 0.013 0.0002 - 0.049 0.001 0.037 - 0.132 0.0004 - 0.005 0.004 - 0.613
Os 0.0004-0.039 0.0002-0.063 0.010 0-0.048 0.002-0.060 0.012-0.016 types; Type-2A & B. Type 2A mineralization is
∑PGE 0.02-0.661 0.026-0.293 0.02-0.15 0.75-3.756 0.02-0.143 0.882-4.583
Ag 0.078-0.544 0.070-6.094 0.321 0.232-18.142 0.051-0.468 0.083-6.975 associated with BMS without ferritchromite.
Au 0.003-0.064 0.006-0.665 0.011 0.66-0.75 0.003-0.022 0.006-0.162
It is Pd dominant (Pt/Pd <1). The sulfide min-
(N= No. of analyses) eral assemblage consists of chalcopyrite, pyr-
From the above data, it is observed that rhotite, pentlandite, violarite, millerite and
ferritchromite and BMS are important hosts for pyrite. The PG minerals are mainly sudburyite,
PGE mineralisation. It is also observed that pres- sperrylite, and Pd-Bi-Te-Sb minerals. Miner-
ence of BMS/ferritchromite enhances the PGM als of cobaltite-gersdorffite solid solution se-
c ontent of the rocks. Roc ks with BMS/ ries are found to be present (Mondal et al.
ferritchromite have more PGM than rocks with- 2001).The sulfide minerals generally occur in-
out them. terstitially to hydrothermal silicates. Type-2B
is mostly free of BMS and platinum dominant
2.4. Style of mineralization (Pt/Pd – 2-3). PGE mineral phases are from the
The PGE mineralization in the Baula Nuasahi Pt-Sb-As system (geversite, sperrylite) coexist
complex is restricted to the breccia zone with Pd antimony (mertieite-II).
(Mondal and Baidya 1997). It is a discordant From the above discussion, it is clear that the
type of mineralization akin to discordant type sulphide-rich rocks (± ferritchromite) are domi-
nated by Pd whereas the ferritchromite bear-

32

ing sulfide- free rocks are systematically Pt-
rich. The PGMs are found in association mostly
with ferritchromite and BMS (Base metal sul-
phide) and less prominently in silicate matrix.
2.5. Mineralogy
The PGMs are present as tiny grains in almost
all the lithounits of the breccia zone. Because of
their extreme small size, they are identified and
analysed by EPMA (Table 3). Some of the im-
portant PGMs are discussed below:
Sperrylite: Sperrylite is present in sulfide bear-
ing pyroxenite. It is anhedral in nature. The
grains are fine and occur within chromite and
at the silicate-chromite interface (Fig. 6a ). It is
also reported from sulfide and silicate environ-
ments (Fig. 6 b & c). Sperrylite is found to be
associated with geversite as two-phase grains
and more abundant in hydrothermal BMS rich
mineralization. It shows coupled substitution
of Sb+S for As similar to sperrylite from
Sudbury c omplex, Canada (Cabri and
Laflamme, 1976). Pd, Rh, Fe, Ni, Cu and Co are
present in minor to trace amounts.
Sudburyite: Sudburyite is reported from sul-
fides present in rocks (gabbro and pyroxenite),
ferritchromite and silicates associated with
BMS. It occurs as subhedral grains marginally
included within euhedral chromite grain (Fig.
6d) and exsolution in ferritchromite (Fig. 5e)
Sudburyite grains ranges from fine size to
(25x50) µm. Pd content is almost in equal pro-
portion with Sb and composition approaches
very c lose to the ideal PdSb with minor
amounts of Ni and traces of Pt, Cu and As. Te
(upto 5.37 wt %) and Bi (upto 5.56 wt %) substi-
tute Sb as in the case of nickeloan variety of
sudburyite (Cabri and Laflamme ,1974).
Braggite: Braggite occurs in ferritchromite
with sulfide association in breccia zone (Fig.
6f). However, Auge et al. (2002) have reported
braggite from BMS free environment. The grains
are of very small (25 x 15µm) size and anhedral
33
MPT-2013
in nature. Braggite contains lower values of Fe,
Cu, Co and Rh, Ir, Os. Under SEM, braggite is
found to be homogenous in composition. Auge
et al. (2002) described zoning in braggite where
the concentration of Pt is more in the core and
Pd is more in the rim. Veryn and Merkle (1994)
concluded that the Ni content of braggite de-
pends on the temperature of formation. Braggite
with a lower Ni content indicates a lower tem-
perature of formation in S-rich environments.
Laurite: Laurite is mainly found in silicate ma-
trix of ferritchromite with grain size ranging
from very small to 15 x 20 µm (Fig. 6g). It is
reported from both the types of mineralization
(Auge et al.,2002). Laurite is present as well de-
veloped euhedral to subhedral crystals. Minor
amounts of Fe, Ni, Cu, Rh and Sb are present in
laurite.
Merenskyite: Merenskyite is found in base
metal sulfide assemblage. It shows little varia-
tion from the ideal composition of PdTe2 with
considerable amounts of Pt upto 6.5 wt % and
Bi upto 30.83 wt %. Auge et al. (2002) also have
reported Pt and Bi upto 6.15 and 22.52 wt %
respectively. The present composition as almost
similar to the composition reported from other
complexes.
Testibiopalladite: Testibiopalladite is present
in silicate vein in ferritchromite (Fig. 6h) and
also included in a pentlandite vein. The grains
are euhedral to subhedral with very fine grain
size to around 15-20 µm. Ni, S, Fe, Ag and Bi are
present in fairly considerable amounts while
Co, Ir and As are present in trace amounts.
Hollingworthite: Hollingworthite is found as
small crystals of the size <1 µm in ferritchromite
(Fig. 6i). It is found in both types of mineraliza-
tion in the form of discrete and complex asso-
ciation. It contains appreciable amounts of Pd
which may have substituted Rh. Pt and Fe are
present in the range of 1.65-6.15 and 2.83-4.57
wt % respectively. It contains minor amounts
 MPT-2013

of Ru (0.16-0.98), Ir (0.84-2.09) Co (0.48-1.49), Ni exsolution texture in ferritchromite, f. Anhedral

(0.29-1.43) and Sb (0.06-0.07) wt % respectively. braggite in ferritchromite, g. well developed
Michenerite: Michenerite is found as subhedral laurite in altered silicate., h. Anhedral
to euhedral grains in ferritchromite in sulfide tesibiopalladite in a silicate vein that is present
bearing pyroxenite of the breccia zone. The with in two ferritchromite grains, i. rounded
grains range upto 25 µm size. Appreciable grain of hollingworthite as included grain in
amount of Sb (upto 6.28 wt %) s present which ferritchromite.
is similar to michenerite from Sudbury com-
plex (1.20-5.40 wt %). Besides, some complex associations and com-
pounds are also identified from the
Malanite: Malanite occurs as tiny crystals in ferritchromite and base metal sulfide associa-
the silicate matrix of sulfide bearing pyroxen- tions of the breccia zone. They are Rh-Ni-S, Pd-
ite. Fe and As is present in fairly considerable Pt-As-Sb-Te-Bi, Pt-Rh-Ni-S, Ag-Nugget, Elec-
amounts. Ni, Rh, Pd and Te are present as trum and Argentite.
traces.
Isoferroplatinum: Isoferroplatinum occurs as Table 3: EPMA of important PG minerals
subhedral c rystals in silic ates and from Boula area
ferritchromite. It is essentially homogenous in
composition close to the ideal composition of
Pt3Fe. Size of the crystals ranges from 10-15 µm Sudb-
uryite
Laurite Sperrylite Brag gite Merens-
kyite
Holling-
worthite
Testi-
biopa-
Mich-
enerite
Malan ite Isoferrop-
latinum
lladite

in size. S, Ni, Cu, Rh and Pd occur as minor S 0.13 35.94 2.01 16.34 0.08 14.64 3.09 0.00 28.47 2.28

Fe 0.62 0.12 0.13 0.16 1.52 3.57 3.90 0.00 11.27 9.13

elements. Ni 0.10 0.11 0.20 4.29 0.10 0.86 5.34 0.00 0.39 1.05

Cu 0.31 0.05 1.4 0.02 2.18 0.00 0.01 0.00 21.16 1.56

Ru 0.00 49.70 0.12 0.56 0 0 0 0.07

Rh 0.02 2.32 0.47 0.25 0.00 36.10 0 0.00 0.26 1.62

Pt 1.16 1.70 49.96 62.51 5.56 3.90 0 0.00 25.35 82.14

0.98 0.21 0 0 0.00

Co 0.00 0.18 0.25 0.01 0.01
29.45 0.02 0.00 11.64 0.00
As 0.05 0 42.89

Os 0 8.20 0.07 0.17 0.22 0.12 0 0.00 0.06 0.19

Ir 0.20 0.89 0.33 0.18 1.45 0.05 0.00 0.0 0.02

Pd 47.10 0.53 0.10 15.68 23.25 7.74 25.38 25.96 0.15 1.70

0.06 13.64 6.28 0.60 0

Sb 45.11 2.54
0.11 41.64 33.58 0.15 0
Te 1.72 0.09 0.00 36.30
6.52 6.15 33.85 0.0 0
Bi 4.04 0.00 30.83
100.04 99.43 99.67 99.50 99.76
Tota 100.56 99.74 100.29 99.76 100.23
l

From the above chemical data, it is observed

Fig. 6. a. Euhedral sperrylite at the grain bound-
ary of apatite and tremolite, b. Sperrylite in
chalcopyrite, c. sperrylite as inclusion in a sili-
cate surrounded by ferritchromite, d. Anhedral
sudburyite is included at the margin of a
ferritchromite grain, e. Sudburyite showing
that a lot of crystallochemical substitutions
have taken place in the minerals resulting in
deviation from the ideal stoichiometric com-
position. The substitutions may have been ef-
fected due to temperature and chemical envi-
ronment during mineral formation.
Because of their siderophile & chalcophile
behaviour, the PGMs in general, exhibit affini-
ties towards As, S, Fe/Cu/Ni and Sb/Bi/Sn/Te.
Besides they are also present as native and al-
loy form. From the mineralogical study, it is

34

observed that PGMs in the breccia zone of BNIC
exhibit different elemental affinity. However,
affinity towards Sb/Bi/Sn/Te is more pro-
nounced.
3. Discussion
Mineralogical characterisation of an ore deposit
has dual importance as it (i) provides genetic
information i e., about the source and physico-
chemical environment of formation of a deposit
and (ii) plays a critical role in optimum utiliza-
tion of scarce natural resources. It helps in the
selection of suitable recovery method and dic-
tates the process flow sheet and plant flow
sheet optimization (Petruk and Hughson, 1977,
Cabri, 1981b, Henley, 1983, Xiao and Laplante,
2004). Although advanced ore characterisation
techniques are available, there is a distinct
problem in characterizing the PGM because of
their low tenor as well as fine grain size. This
problem can be overcome by pre-concentra-
tion techniques such as gravity, magnetic or
flotation or a combination of these techniques.
Hence mineralogy plays a critical role in selec-
tion of suitable beneficiation technique(s) for
processing of such ores.
From the mineralogical study, it is observed
that two types of PGE mineralisation is present
in the breccia zone of the BNIC. Type 1 is mag-
matic in nature and prominent in the southern
part of the breccia zone. In this type, PGM are
present as inclusions in pyroxene and plagio-
clase that suggest early crystallization in the
evolution of the magma. As there is no signifi-
cant PGE anomaly in the ultramafic rocks of
the complex and chromitite layers, it is pre-
sumed that the source of PGE may be the gab-
bro itself with precipitation of PGM being pro-
voked by sudden changes in physic-chemical
conditions due to incorporation of partial di-
gested ultramafic materials. The PGM miner-
alogy is characteristics of high temperature and
magmatic sulfide free and shows striking simi-
35
MPT-2013
larities to occurrences at UG2 and Platreef of
S.Africa and Great Dyke, Zimbabwe. Type 2 is
hydrothermal in nature and prominent in the
northern part of the breccia zone. PGM is con-
fined to hydrothermally altered matrix of the
breccia zone. PGM and BMS are associated with
hydrous silicates such as amphibole, mica, chlo-
rite, apatite and ferritchromite etc. The hydrous
minerals were formed during late magmatic
evolution of Bangur gabbro without introduc-
tion of external fluids and with deuteric fluids.
Abundance of hydrous silicates indicates that
residual phase was dominated by fluid. BMS
are related to a fluid rich hydrothermal stage
with crystallization temperature in the range
of 300-500oC. Contribution from the country
rock is negated by isotopic study (O/H for sili-
cates and S for BMS). The fluid was generated
by the crystallization of silicates at a magmatic
stage in the gabbro and became concentrated
in the breccia zone at the top of the magmatic
system.
The low grade PGE mineralisation in the brec-
cia zone of the Boula Nuasahi igneous complex
is related to late intrusion of Bangur gabbro
and is a cumulative effect of both magmatic and
hydrothermal processes.
Sulfides occur as veins, stringers, and irregu-
lar pockets in the matrix of the breccia zone.
The gabbroic rocks in the hanging wall side of
the breccia zone contain disseminated sulfides.
Chalcopyrite, pyrrhotite, pentlandite and py-
rite are the common sulfide minerals. The PGE
mineralogy in sulfide rich assemblages is domi-
nated by Pd, Pt, Sb, Bi, Te, S and/or As bearing
phases, e.g., sudburyite, mic henerite,
testibiopalladite, sperrylite, merenskyite and
palladium bearing melonite, irarsite and
hollingworthite. These minerals are present as
tiny inclusions in sulfides.
Like many other deposits, PGMs at BNIC are
associated with ferritchromite with or with-
out BMS (Razin et al. 1965, Naldrett and

Cabri,1976; Vermaak and Hendriks,1976, Cous-
ins and Vermaak,1976). The mineral assem-
blage is dominated by isoferroplatinum,
braggite, malanite, sperrylite and laurite. In
this association, PGM occur mainly as inclu-
sions in ferritchromites and associated silicates
(plagioclase, pyroxene).
It is a difficult proposition to assess the asso-
ciation of PGEs in silicates. Exact quantifica-
tion of PGMs in different hosts is a very diffi-
cult task as the rocks and ores in the breccia
zone are thoroughly mixed due to intrusion
and brecciation resulting in a hybrid assem-
blage. As is the case with Sudbury, Merensky
reef and Plat reef where a significant portion
of minute PGMs, occur as interstitial grains
and as solid solutions in silicates (Sizgoric,
1984; Kinloch, 1982; Merkle, 1992; Maier et al.,
1999, Peyerl, 1982; Bryson, 2008), at BNIC the
PGMs are also found as discrete grains in the
silicate matrix (often as clusters). The silicates
may be with or without ferritchromite asso-
ciation. Some of the PGM are reported from
secondary silicates such as apatite, tremolite
etc.
As PGMs are associated with ferritchromite
which is magnetic in nature, pre-concentra-
tion of PGM can be tried by magnetic separa-
tion by reducing the size of the ROM by stage
grinding. Similarly, the sulfide hosted PGM can
be pre-concentrated by flotation technique.
These pre-concentrated materials can be used
to extract PGE values.
4. Conclusion
The breccia zone that hosts PGE mineraliza-
tion has resulted due to intrusion of coarse
grained gabbro into the preexisting ultrama-
fic-mafic sequence. This intrusion has resulted
in dismemberment of the rocks/chromite of
earlier formation. Due to brecciation, the rocks
36
MPT-2013
and chromite are mixed up to form a hybrid
matrix. Two types of PGE mineralisation have
been identified in this breccia zone represent-
ing both magmatic and hydrothermal milieu.
Two types of mineralisation exhibit contrast-
ing mineralogical characteristics. Pt is domi-
nant in southern part where chromite is the
principal host and Pd is dominant towards
north with BMS as the important host. PGM
are reported from all the matrices such as
chromite, sulfide and silicate in the breccia zone.
The PGM are very fine grained and display
various textural dispositions in chromite, sul-
fide and silicate. PGM are mostly present as
included grains in sulfide, inclusions and
exsolutions in ferritchromite. Some PGM are
also present as inclusions within silicates
whic h are in turn present within
ferrochromite. The sulfide assemblage is rep-
resented mainly by chalcopyrite, pyrrhotite,
pentlandite and pyrite. Minor amounts of mil-
lerite, bravoite, cubanite, geversite, cobaltite are
also found to be present. The southern part is
predominated by ferrochromite with very less
inter granular BMS.
Any scheme to recover/pre-concentrate PGE
values from this complicated matrix material,
needs thorough assessment of the different fa-
cies; both qualitatively and quantitatively for
PGE content and a combination of beneficiation
techniques may be adopted to concentrate the
PGE values from such a low tenor hybrid ma-
trix material of the breccia zone of BNIC. The
chromite (± BMS) can be concentrated by a
combination of processes such as gravity sepa-
ration followed by magnetic separation (as
chromite is highly magnetic). As in practice at
UG-2, where chromite is being concentrated
by flotation, flotation can be tried upon for the
concentration of chromite at BNIC.
The spatial distribution of PGM in this breccia
zone is very complex because of the intimate
association of three major hosts viz. chromite,

sulfide and silicate. The intermingling of sili-
cates has resulted in a low tenor and needs pre-
concentration before recovery of PGM from
this complex matrix association. Looking at the
complexity of the PG mineralization and host
rock/mineral association, the low grade ore of
this breccia zone can be processed by a combi-
nation of processes depending on specific
physical characters to recover/pre-concentrate
the PGE values.
Acknowledgement
The authors are thankful to Prof. B. K. Mishra,
Director, CSIR-IMMT, Bhubaneswar for his
kind permission to carry out this work. The
financial support by Ministry of Mines, Govt.
of India, is highly acknowledged.
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Geology of “Eklama Iron Ore Complex” With Special Emphasis

on Geochemistry of Iron Ore
Mofid Ali
Project Assistant (Level II)
CSIR-CIMFR Bilaspur Unit
Abstract
Iron ore is very important in modern industrial world, as it is necessary for making different
alloys of steel, and is an important commodity for the industrial development of any country.
Chhattisgarh State is blessed with the occurrence of Banded Iron Formations in a number of
localities like Bailadila and Dalli-Rajhara. It has been seen that the same type of formation continues
northward which, with ongoing exploration, revealed occurrence of BIF.
In Kabirdham (Kawardha) district of Chhattisgarh recently several iron ore deposits are found
including those of Eklama-chelikama block. This block is situated in the west – central part of
Chhattisgarh state. This iron ore deposit known as Eklama Iron Ore Complex (EIOC) after the
name of village Eklama where it has been found. It is associated with the dolomite, ferruginous
pink and white quartzite, shale and volcanic slate/argillite. EIOC is high grade iron ore deposit
hosted within the Meso-Proterozoic banded iron formations. The general trend of EIOC is N-S to
NE-SW with strike length 15 Km and average width is 5 Km. It is of tabular shaped due to well
developed joint hosted within the Chilpi Ghat Group of rocks trending N-S and has similarity
with the Bailadila Group but differ in geological setup being younger in the stratigraphic order.
EIOC exist with massive hard and compact iron ore. This iron ore complex is dominated by
hematite with presence of some amount of magnetite.
The present study deals with Geochemistry of this high grade iron ore which is characterized by
high Fe content (av. 66.54 wt% ) and very low amount of S, Na2O and K2O . Amount of SiO2 and
Al2O3 are also low, 1.9 and 1.16 respectively. This high grade iron ore shows SiO2 and Al2O3 as main
impurities and Fe shows generally negative correlation with the other major oxides.

Keywords: BIF; iron ore; EIOC; geochemistry; inter elemental correlation.

1. Introduction periods. BIFs are widely distributed in the state

of Karnataka, Chhattisgarh, Jharkhand and
According to James 1983 iron ore associated
Odisha.
with BIF world over has been found within Mid-
Archaean age (3500-3000 Ma), Late-Archaean Iron ore occurrence near Eklama village are also
similar to the deposits of Bailadila, Rowghat,
age (2900-2600 Ma), Early-Proterozoic age
Hahaladdi, Aridongri and Dalli-Rajhara, as the
(2500-1900 Ma), and Late Proterozoic – Early
regional strike of iron ore bodies is similar and
Phanerozoic age (750-450 Ma). However in India
are bounded almost between longitudes 800 45’
BIF are restricted to the Mid-Archaean (3500-
and 810 15’. Hence, it is inferred that iron ore of
3000 Ma) and Late-Archaean (2900-2500 Ma)

39

EIOC may be regional linear structural ridge,
starting from Bailadila iron ore deposits in
south (average altitude 1200 m) and in north
(average altitude 550 m) through Rowghat,
Hahaladdi, Aridongri and Dalli-Rajhara iron
ore deposits of Chhattisgarh. This iron ore
deposits are known as Eklama Iron Ore Complex
(EIOC) because of this iron ore deposits
encountered near village of Eklama. EIOC is
present in Tahsil Sahapur, Lohara, Kabirdham
district falling under the SOI topo sheet no. 64
G/1.
EIOC is hosted within Chilpi Group of rock and
associated with the ferruginous pink and white
quartzite, shale and volcanic slate/argillite
rocks. EIOC is possesses similarity with the
Bailadila iron formation although Chilpi Ghat
Group is younger than Bailadila Group and as
such no detailed literature is available on the
geochemistry and geology of this deposits.
C. Tripathi et al (1973-74) eluc idated
stratigraphy and structure of the Chilpi Ghat
rocks. Although fragmentary information is
provides by (Tripathi et al 1981; Rao 1981), there
is a scarcity of published literature regarding
the stratigraphic status and other genetic aspect
of the Chlilpi Ghat Group rocks.
The present study embodies the result carried
out on the geological characteristic of iron ore
deposits, and geochemistry of EIOC.
2. Geology of the area
The Chilpi group of rocks occur along the
eastern flank of the Maikal range from
Kabirdham (22 0 0’:810 15’) in the North to
Lohara (210 50’:810 08’) in the South. The beds
strike N-S with moderate dips towards East.
The rocks of the Chhattisgarh Super group lie
to the East of the Chilpi group of rocks and in
the Chilpi Ghat series are c onfined by
horizontal to sub-horizontal infra-trappeans
and the Dec c an basalts. A low grade
metamorphic impress is observed in the Chilpi
group of rock.
40
MPT-2013
The Chilpi Ghat series is divisible in to two
groups, the older meta-volcanic and the
younger meta-sediments. The meta-volcanics
are primarily composed of tuffaceous rock of
intermediate composition. The passage from
volcanics to the sedimentaries is apparently
without any hiatus, as no separating
conglomerate beds are noted. In Chilpi-Borla
section a sandstone horizon with wave type
ripple marks and thin intercalation of chert
bands immediately overlie the metavolcanics.
The metasedimentary sequence is dominantly
composed of interbedded sequence of phyllite
and shales. Sandstone is found mostly at top of
the sequence and in narrow zones in the lower
parts. Lenses of quartzitic composition mostly
of unmappable dimension occur within the
phyllites. A zone of hematite-Jasper occurs as a
narrow, nearly continuous bed toward the
lower part of the metasedimentary sequence.
The basement rocks exposed in the area are
mostly andesite and rhyolite of Pitepani
volcanic belonging to Nandgaon Group of
Dongargarh Supergroup. Chilpi Group
comprises of quartzite, shale, slate, phyllite,
argillite, ferruginous sandstone, jasperoid,
massive iron ore, B.H.Q., B.M.Q., jaspilite (B.H.J.),
limestone, dolomite and basal conglomerate etc.
Most of the limestone and dolomite of Chilpi
Group of rock are crystalline in nature and at
places spec ks of pyrite and c halcopyrite
recorded. The rocks of Chilpi occur in the area
in North-South trending two distinct flanks,
which are divided by the Pitepani volcanics and
Deccan trap in the central portion. The general
strike direction is NNE-SSW with high dips up
to 450 towards East. At places, fold and fault
have been also occurring. The rocks of Chilpi
Group rocks is have steep dips towards the west
however at places change in dip direction is
also observed which may be due to folding.
Sarkar (1957) reported canoe shape folding in
this area. By the nature of contact of different
 MPT-2013

units and sudden change in lithology many 3.2 Iron Ore

small and large scale fault are inferred.
The Geological sequence of the area is as EIOC is existing in the form of massive and also
below: floating ore type within Chilpi Group rocks.
BHQ is constituted of alternate bands of
LITHLOGY
FORMATION
STRATIGRAPHIC STATUS
GROUP SUPER
AGE
quartzite and hematite. Bands of quartzite are
GROUP
Alluvium ……. ……. ……. RECENT fine grained, white in colour. Hematite is also
Laterite with Bauxite ……. ……. ……. CENOZOIC
Basaltic flows Unclassified ……. Deccan Trap UPPER fine grained and steel blue to metallic grey in
CRETACEO
US TO colour. BMQ contains alternate band of
PALEOCEN
E quartzite and magnetite. Bands of quartzite are
Limestone, arkosic sandstone,
calcareous & conglomeratic ……. Lameta Group ……. CRETACEO fine grained, white to greyish in colour.
sandstone and clay at places US
Limestone and dolomite with
intercalation of shale and Chandi Raipur Group Chhattisgarh MESO TO
Magnetite is medium to fine grained and
glauconitic sandstone
Calcareous shale with
Formation Super Group NEO
PROTEROZ
metallic grey to dark brown in colour.
limestone, dolomite and arenite Gunderdehi OIC
intercalations Formation
Glauconitic arenite, arkose and
conglomerate …….
Chanderpur
Group
3.3 Mineralogy and Morphology
Quartz vein/reefs ……. Intrusive …….
(Multiple MESO
injection of PROTEROZ In Ekalma Iron Ore Complex is dominated by
various phases) OIC
Basic intrusive hematite mineral but some amount of
Quartz, shale, slate, phyllite,
argillite, ferruginous ……. Chilpi Group ……. magnetite is also present. Under the
sandstone, limestone,
jasperoid, B.H.Q., B.M.Q., microscope hematite is showing white to
jaspilite, ferruginous shale,
crystalline limestone & bright white colour in plane polarised light.
dolomite and basal
conglomerate The iron oc c urrenc e is mostly in the
Hornblende bearing Malanjkhand
granodiorite, biotite granite ……. Granitoids ……. PALEO
PROTEROZ
inaccessible rugged hilly and densely forested
Meta-basalt (Pitepani ……. Nandgaon …….
Volcanics)
Amphiblite …….
Group
……. …….
OIC
ARCHEAN
terrain. Iron ore is display tabular shape due
Granite and gneisses
to well development of joint planes. The iron
(After GSI. 2004 & 2005) ore in this area is generally exposed at hillock
of lower altitudes ranging between 400 to 650
3. Description of the ore deposits
m. The iron ore is mostly exposed in hilltops,
3.1 Structure and stratigraphy of ore body escarpment, eastern hill slopes and foothill.

The iron ore occurrence of “Eklama Iron Ore 4. Geochemistry

Complex” (EIOC) in general dipping NE-SW,
NNW-SSE amount is 150 to 300E. The strike 4.1 Major oxide geochemistry
length of iron ore occurrences is about 15 km In the order to assess the major element bulk
and about 5 Km wide. EIOC iron ore layer is 8 composition of the iron ore, 7 samples of the
to 11m thick. The massive iron ore exist with iron ore were analyzed. The geochemical data
well developed joint planes. EIOC are situated is presented in Table.1 .The data reveal that
within the Chilpi Ghat group of rocks and it is
the bulk composition of iron ore is dominated
Meso-Proterozoic age. Massive, medium by Fe oxide, SiO 2, and Al2O3, which make
grained quartzite occurs as the cap rock up on approx 98.2 wt.% of the iron ore. In iron ore Fe
the iron ore bands. The iron ore band is varies between 64.95 - 68.10 wt.%, with an
discontinuously exposed along NNE-SSW. Iron average of 66.54. Major element analytical
ore occurs in the dip slope of the hills in the E to result reveal that the iron ore contain very little
SE direction exposing itself at different contours.
amount of S, P, TiO2, MnO, CaO, MgO, Na2O,

41
 MPT-2013

and K2O in wt.%. The marked enrichment of iron high value of the CaO+MgO. It is suggested a
in all ore sample is attributed to the effective near absence of calcite and dolomite. TiO2 bears
removal of SiO2, MgO and CaO (Gutzmer et al a positive moderate correlation (0.5) with Al2O3
2008). in iron ore (Fig no.1). Aluminium and titanium
In iron ore TiO2 concentration ranges between are considered to be generally immobile during
0.073 to 0.121 wt.% with an average 0.098 wt.%. hydrothermal, digenetic and weathering
High grade iron ore is depleted in CaO+MgO, processes (MacLean and Kranidiotis 1987).
only one sample (R-21) shows exceptionally Alkali content (K2O+Na2O) in iron ore represents
less amount.
Table No.1: Bulk composition of EIOC irons ore R-3 and R-19 is BIF.
sample Al 2 O3 LOI Na2 O
Fe % SiO2 % S% P% TiO2 % MnO % CaO% MgO% K 2 O%
ID % % %
R-6 68.10 1.12 0.69 0.006 0.066 0.121 0.037 0.47 0.008 0.009 0.004 0.006
R-8 67.47 0.88 0.94 0.006 0.159 0.090 0.027 0.48 0.226 0.032 0.014 0.021
R-10 67.35 0.87 0.96 0.007 0.178 0.110 0.014 0.48 0.441 0.039 0.021 0.013
R-15 65.11 2.62 2.14 0.008 0.076 0.120 0.035 1.48 0.011 0.016 0.009 0.012
R-20 67.60 1.12 0.84 0.006 0.064 0.070 0.011 0.66 0.021 0.014 0.011 0.009
R-21 64.95 1.76 1.78 0.007 0.275 0.110 0.041 0.92 1.36 0.139 0.019 0.026
R-22 65.18 4.74 0.78 0.006 0.115 0.070 0.024 0.64 0.022 0.032 0.018 0.021
R-3 27.63 53.64 3.80 0.007 0.075 0.112 0.009 2.40 0.018 0.022 0.016 0.009
R-19 34.43 45.13 3.47 0.008 0.075 0.110 0.058 1.82 0.011 0.009 0.006 0.008

4.2 Inter Element Geochemistry: c oeffic ient). Fe shows strong negative

correlation with SiO2 (- 0.73), Al2O3 (-0.71), and
Major element oxide of iron ore is plotted on
K2O (-0.62), while, it shows moderate negative
the scattered diagrams to find out inter-element
correlation with S (-0.56), MgO (-0.53) and MnO
relation with each other (Fig.1A to H). Al2O3 and
(-0.43), and weak negative relationship with the
SiO2 show insignificant and very weak positive
CaO (-0.39) and Na20 (-0.38). Al2O3 and TiO2
correlation with each other (0.12 correlation
exhibit moderate positive correlation (0.5).

(A) (B)

(C) (D)

42

(E)
(G)
(I)
Fig.1. Interrelationship between major oxides of EIOC.
5. Conclusion
The massive iron ore exists with well
developed joint planes, which generally leads
to produce large tabular shape blocks. Iron ore
is of high grade containing average iron percent
66.54%.
Geochemical investigation reveal SiO 2­ and
Al2O3 is main gangue constituents in ore. Fe
generally shows negative correlation with
other major element oxides. Geochemical
studies indicate detritus free precipitation of
iron oxide.
Eklama Iron Ore complex is found within Meso
–Proterozoic age BIF. Hydrothermal solution
is main source of silica for this BIF and iron
43
MPT-2013
(F)
(H)
(J)
oxide is delivered due to c ontinental
weathering and leaching. Iron oxide was
transported though river and reached the
depositional site in form of solution. Eklama
iron ore complex possesses similarity with Lake
Superior Iron Formation.
References
Bhattacharya, H. N., Chakraborty I., Ghosh, K.
K., 2007. Geochemistry of some banded
iron-formations of the arc hean
supracrustals, Jharkhand–Orissa region,
India, J. Earth Syst. Sci., pp. 245–259.
Bhattacharya, T.K., 1993. Sedimentology and
Geochemistary of Bailadila Group rocks
 MPT-2013

around Bacheli, Dist. Bastar, C.G., Phd thesis, geochemistry of the high-grade iron ores
pp148. of the Aguas Claras Mine and
comparison with the Capao Xavier and
Dasgupta, D.J., Pal, R.N., Roy, S.K., 1982. Chilpi
Tamanduá iron ore deposits,
Ghat group of Roc k along some
Quadrilatero Ferrifero, Brazil, Miner
Selected Traverses in the Balaghat at M.P.,
Deposita, Springer, pp.229–254.
GSI project progress report.
Spierra, C. A., Maria, S., Rosiere, C. A., 2003.
Mukharjee, A., 1999. Ore Genesis (A holistic
Geology and geochemistry of the A´ guas
approach), allied Pub., Ltd, pp. 637.
Claras and Pico Iron Mines, Quadrilatero
Roy, S., Venkatesh, A. S., 2009. Mineralogy and Ferrýfero, Minas Gerais, Brazil,
geochemistry of banded iron formation Mineralium Deposita , Springer, pp.751–
and iron ores from eastern India with 774.
implications on their genesis, J.Earth Syst.
Tripathi, C., Ghosh, P.K., Chandra, S., (1973-74).
Sci. 118, pp.619–641.
Eluc idation of Stratigraphy and
Spierra, C. A., Maria, S., Rosiere, C. A., Ardisson, Structure of the Chilpi Group, Balaghat,
J. D., 2008. Mineralogy and trace-element GSI project progress report.

*******

44
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Mineralogical Characterisation of the Iron Ores having Varying

Degrees of LOI from Gua and Kiriburu Mines, SAIL

Sanjay Hembram* and Ram Pravesh Bhagat

Mineral Processing Division; CSIR- National Metallurgical Laboratory, Jamshedpur-
831007
Abstract
Depletion of high grade iron ore reserves coupled with increasing market pressure for good grade
iron ore and the threat of environment pollution has made one to realize the need to exploit large
tonnage of low grade haematitic iron ores with high LOI and goethite ore.. The sintering based
agglomeration technique, for the obvious reason of unfavorable granulometry, does not work as
this type of ores need intense beneficiation in their sub-sieve range. In view of this a suitable
pelletisation based agglomeration techniques need to be developed. The LOI content of ore
(concentrate) does affect the crushing strength of the indurated pellets due to the emission of
bonded water molecules during heat hardening. The paper describes the mineralogical
characterization of the iron ores having varying degrees of LOI namely, (a) The concentrate of
from the slimes and rejects of Gua ore mines, and (b) Highly goethitic ore, from the Kiriburu mines
of SAIL. The XRD studies on both the samples show the presence of hematite mineral as major
phase. Besides, the presence of goethite and gibbsite in minor phase was observed in both the
samples, but with varying degrees. Photomicrographs of different size fractions of the Gua Ore
Concentrate show: (a) hematite crystallites coalesce forming larger polygonal grains in a matrix
of goethite along with clay matter, (b) Trace amount of magnetite in smaller size fraction (-200
mesh) and goethite grain along with Hematite grain along with the clay matters. The mineralogical
investigation also shows the alteration of iron-ore due to dehydration of goethite in changing
hematite in -200 mesh size fraction. The microscopic examination of the Kiriburu Goethitic Ore
shows the early stage of formation of colloform which has taken place due to dehydration of
goethite in the first stage. Subsequently, colloform due to dehydration of goethite which gets
altered into hematite was observed. In the later stage lateralized portion of the hard ore having
intermingling of clayey matter was observed. Due to metamorphism different stages of alteration
of goethite was observed through the present microscopic study. The study also reveals the presence
of hematitic-goethite crystals which were scattered and trapped within the clay matters. The
mineralogical study has also revealed the appearance of hematite crystals within the hard
laminated goethite.

Keywords: Gua ore, Kiriburu goethite, XRD, liberation study, petrological study
* Correspending Author: : Sa nja y Hembram, Mineral
Processing Div ision, CSIR- Na tio nal Metallurgical
Laboratory, Jamshedpur-831007
Email: snjhembram@gmail.com

45
 MPT-2013

1. Introduction The present paper is based on the results of the

projec t ac tivity on the development of
India ranks the sixth among producers of iron
pelletisation process for Indian Goethitic/
ore, with a 28.52 BT (IBM Report, 2012) of
Hematite Ores with varying degree of fineness,
hematite (Fe2O3) and magnetite (Fe3O4) reserve
supported by the Ministry of Steel,
base. The majority of Indian iron ore deposits
Government of India having the objective to
occur in the eastern, central and southern parts
optimize the parameters for the process of
of India in the regions of Jharkhand (10%),
pelletisation of the concentrate and induration
Orissa (34%), Karnataka (22%), Chhattisgarh
of the green pellets with respec t to high
(15%), Goa (14%) and others (5%). Amongst
c rushing strength (CCS) with optimized
these reserves, the iron ores of Eastern India
reduction properties.
are of high quality and mostly hematitic in
nature with varying degrees of LOI and gangue 2. Experimental
contents. 2.1. Materials
The blast furnace (BF) based iron making
proc ess requires c alibrated lumps & Mines of Steel Authority of India Ltd. (SAIL) (Fig.
agglomerates, pellets and sinters, having rich 1) area it is located in the boarder of Jharkhand
in Fe value and low in their gangue (SiO2 and and Orissa.
Al2O3) contents. It is reported that an increase
in 1% Fe in BF burden increase the productivity
by 2% and decreases the Coke rate by 3%.
Besides, reduction in slag volume by 60 kg/
THM could be attained when the burden with
15 % reduced silica is charged into the furnace
(Sampath, 2012). However, increasing demand Fig. 1: Mines of Kiriburu, SAIL from where
of iron ore has been compelling the ferrous the sample was collected
sector to utilize low-grade ores, albeit after their 2.1.1. Gua iron ore concentrate
intense beneficiation.
One important factor that has not gained its The hydro-cycle underflow was generated
importance in Indian Iron & Steel Industries, as during the pilot plant studies of gue iron ores
following the treatment of slimes and rejects
yet, is the LOI content of these ores and its effect
from lump and fine iron ore. This was further
on their agglomeration characteristics. The
beneficiated using the wet high intensity
goethite enriches along with hematite ore
magnetic separation (WHIMS) to yield the
during the process of beneficiation, which concentrate sample. The concentrate assayed
results in an increased percentage of LOI in the 64 wt. % Fe and 3 wt. % LOI.
concentrate by 2.5 % or more. The existing
technology in pelletisation has its limitation in
respect of the usage of fine concentrate of
hematitic ore with high LOI and higher blain
number. The LOI content of ore (concentrate)
does affect the c rushing strength of the
indurated pellets due to the emission of bonded
water molecules during heat hardening. Fig. 2 (E, F & G) Photographs of Samples E, F
& G showing different Colors

46

E: Fe: 61.4% LOI : 3.1% F: Fe: 64.7% LOI:3.5%, G:
Fe: 61.4%, LOI : 2.7%,
(a) +210 µ crushed to -74 µ (b) +149 µ crushed to
-74 µ
© +105 µ crushed to -74 µ (d) + 74 µ crushed to
-74 µ
(e) + 63 µ (f) +38 µ (g) -38 µ
Fig. 3: Sieve vis-à-vis chemical analyses
of the concentrate
2.1.2. Kiriburu goethitic ore
Highly goethitic ore where c ollec ted
handpicked and collected from the Kiriburu
mines of SAIL was studied. Samples were
collected from the mine site in form of run-of-
mine ore (ROM) which consists of boulders,
lumps. The color of the ore generally varies from
Grey to shades of reddish brown to pale white.
All the ores have a distinct earthy luster and
are granular to angular in form.
The sample thus collected for beneficiation
studies at NML was crushed to below 30 mm
and was characterized. It is found that the
normal crushing operation yielded ~64 wt.%
lumps (-30+10 mm), ~28 wt.% fines (-6+0.15
mm) and ~ 8 wt.% ultra-fines (-0.15mm).
2.2. Methods
2.2.1. XRD study
XRD studies of the samples ,ground to -200 #
size was carried out with Co- Ká radiation
using X-ray diffraction machine in 2è range
10- 120 degrees.
2.2.2. Petrological study
The ore was studied under Petrological optical
microscope and Petrological zooming stereo
microscope.
47
MPT-2013
Preparation of Polish Section
The concentrate sample from Gua mine was
studied in microscope the sample were size
fraction of (+250#), (+350#), (-350#). Sample
were mounted for polishing. The rough surface
of the sample ground initially with 80 meshes
for 30 minutes, then further ground down using
600 mesh c arborandum powders for 30
minutes. Eac h sample were ground with
Manual Polishing Machine using different
silicon carbide water-proof paper (400, 600, 800,
1000, 1200 mesh) for 20 minute each to achieve
a topographically relief free surface. The
samples were polished using Disc Polisher with
1 micron diamond grit for 30 minutes, followed
by ¼ micron diamond grit papers for another
30 minutes to achieve a good reflectance and
scratch free surface.
Polished sections were prepared from selected
samples for ore petrographic studies. Fresh Iron
ore samples from Kiriburu were cut as polish
section for microscopic studies. The section was
further cut down to required size using
Logitech cutting and lapping machine (10 inch
diameter diamond saw) desired size. The rest
procedure polishing adopted for the Gua ore
concentrate was subsequently followed.
Microscopic Study
Polished sec tions were studied and
photographs were taken using a Leica-make
optical petrological microscope having both
reflected and transmitted light facilities using
5x, 10x, and 20x, 50x dry-objectives and with
oil objective.
2.2.3. Liberation study
Screen Analysis
The specimen samples of Kiriburu goethitic ore
were crushed manually using iron mortar to a
size of around 10#. Then crushed sample were
homogenized by conventional coning-
 MPT-2013

quartering method. Half of the sample were kept Major Phase: Hematite [2.70 (100), 2.52 (60), 1.69
as head sample and another half were sieved (45), 1.84 (35)]
(Both Wet and Dry sieving) to different micron Minor Phase: Gibbsite, Al(OH)3 [4.85 (55),
size (-10+14) mesh, (-14+20) mesh, (- 2.45(20)]
20+30)mesh, (-30+48)mesh, (-48+65) mesh, (- Minor Phase: Goethite, áFe(OH) [4.18(37), 2.45,
2.69, 1.72(16)]
65+100) mesh, (-100+150) mesh, (-150+200)
mesh, (-200+250) mesh, and (-250+300) mesh. He
High LOI Goethatic Iron ore

d=2.70105
using vibratory sieve shaker. Weight percent
1800

1700

1600

of different sieve fraction were calculated taking 1500

1400 Go

d=4.18016
1300

weight of the individual fraction (Table 1). 1200

d=2.51802
1100

Lin (Counts)
G

d=4.85394
b He
1000

d=3.68454
He

Individual sieve fractions were studied under

d=1.69577
d=2.44740
900

d=4.99208
800 He

d=1.84140
He

5005393
88410645
700

a petrological zooming stereo-microscope to

d=1.45
Go

d=1.71497

d=1.48649
d=2.1d=2.2
d=2.58173
600 Go Go He

d=1.4

d=1.31139
d=2.25215

08
d=1.60014
607
622
500

d=1.79906

d=1.05573
d=1.10309
d=1.5

d=0.96029
d=0.95151
d=1.25547
d=1.5
delineate the liberation characteristics of the
400

300

200

ore in terms of free iron mineral, free gangue 100

6 10 20 30 40 50 60 70 80 90 100 110 120

2-Theta - Scale

mineral and interlocked grain by manual grain High LOI Goethatic Iron ore - File: High LOI Goethatic Iron ore.raw - Type: 2T h/Th locked - Start: 6.000 ° - End: 120.009 ° - Step: 0.020 ° - Step time: 86.4 s - Temp.: 25 °C (Room) - Time Started: 9 s - 2-Th
Operations: Import

counting method.
Fig. 4b: XRD of Kiriburu high LOI iron ore
Major Phase: Goethite [4.18(71.7)), 2.58 (26.5),
Table 1: Weight percent of different sieve
fraction 2.25 (21.7), 1.60 (21.2)]
1St LOT 2nd LOT
Minor Phase: Gibbsite, Al(OH)3 [4.85 (51.2)
Size in mesh Wt. in gm Wt. % Wt. in gm Wt. % Avg. Wt. % Minor Phase: Hematite, áFe(OH) [3.68(48.7),
(+10) 440 91.10 817 83.45 87.27 2.70(100), 1.84(34.6), 1.31(22)]
(+14) 14.9 3.08 54.74 5.59 4.34
(+30) 5.2 1.08 23.07 2.36 1.72
(+48) 6.1 1.26 29.17 2.98 2.12
3.2. Morphological characteristics
(+65) 2.6 0.54 5.89 0.60 0.57
(+100) 1.6 0.33 11.38 1.16 0.75 a) Gua Ore Concentrate
(+150) 1.4 0.29 5.16 0.53 0.41
(+200) 1.3 0.27 5.73 0.59 0.43 Fig. 5 shows the view of grain having size
(+250) 1.2 0.25 2.25 0.23 0.24
(+300) 0.2 0.04 1.01 0.10 0.07
fractions, -74 µ and -40 µ in zooming stereo-
(-300) 8.45 1.75 23.65 2.42 2.08 microscope in 50x pix.
Total 482.95 99.99 979.05 100.00 100.00

3. Results and Discussion

3.1. XRD
Figures 4a and 4b respectively show the XRD
of Gua ore concentrate and high LOI Kiriburu
iron ore. gua iron ore
d=2.70024

600

(a) (b)
500
d=2.51735

Fig. 5 (a) & (b): Views of -74 µ (left slide) and -

400
d=4.84414
Lin(Counts)

d=1.69582
d=3.68322

d=1.45002 d=1.45368

40 µ iron ore concentrate

300
d=4.18318

d=1.84185
d=2.20673

d=1.48628

200
d=2.44865

(I: Interlocked, G: Goethite, F: Hematite)

25
d=1.71751

5
d=1.59901

19

d=1.10337
08
31

d=1.13775

d=1.02339
d=1.80099

.3

d=1.00094
1
==
dd 1.

100

0
b) Kiriburu Goethitic Ore
6 10 20 30 40 50 60 70 80 90 100 110 120

2-Theta - Scale
gua iron ore - File: gua iron ore.raw - Type: 2Th/Th locked - Start: 6.000 ° - End: 120.009 ° - Step: 0.020 ° - Step time: 21.6 s - Temp.: 25 °C (Room) - Time Started: 8 s - 2-Theta: 6.000 ° - Theta: 3.000 ° -
Oper ations: Impo rt
The ore samples where lumpy, rough to touch,
and laminated with an iron, silica, kaolinitic
Fig. 4a: XRD of Gua iron ore concentrate clay, quartz, gibbsite and limonitic matter.The

48

ores where crystalline in nature. The colors of
the ore generally vary from shades of yellows,
reddish brown. The streak of the ore was found
to be reddish brown in color. The ore has a
distinct earthy luster and granular in form. The
ores sample was not fresh and weathering effect
was visible to the naked eye. Photographs of
the samples studied are presented in figure
(Fig.6a and 6b).
(a) (b)
Fig. 6 (a) & (b): Photographs of the samples
3.3. Microscopic characteristics
a) Gua Ore Concentrate
The microscopic examination shows that the
hematite crystallites coalesce forming larger
polygonal grains in matrix of goethite along
with clay matter. Photomicrograph also shows
trace amount of magnetite in size fraction of -
200 mesh., The petrological investigation also
reveals the alteration of iron ore due to
dehydration of goethite which has changed into
hematite in same size frac tion. Besides,
lateralized portion of the hard ore was observed
showing intermingling of clayey matter within
the pit.
b) Kiriburu Goethitic Ore
It was observed that the Kiriburu goethtic ore
was mineralogic ally very c omplex and
consisted of high-grade hematitic ore pieces to
iron-rich and aluminous laterites. Under the
microscope hematite and goethite minerals
were found to be the major ore-minerals. The
gangue minerals consisted of kaolinitic clay,
quartz, gibbsite and limonitic matter. In a hard-
massive ore piece, hematite was the dominating
mineral phase and occurred as fine crystals
49
MPT-2013
often showing a layered appearance. Minor
impurity in form of c lays oc curs in the
weathering pits and micro-fractures. However,
majority of the ore fall in the category of
lateritized-type which was of varied character.
They vary from iron-rich hard lateritic ores to
alumina-rich soft lateritic ores and are porous.
In the lateritic ores goethite is the major ore
mineral and occurred in various forms such as
vitreous, colloform bands, fine crystals, spongy,
and earthy etc. The pores had been often filled
with clays. The minerals, clays, silica, gibbsite
and limonitic matter were found to be very
intricately bound by goethite. Sometimes this
intricacy occurred in very fine sizes (in micron
levels) that has put restric tion on their
liberation behaviour.
Therefore, it is expected that very fine grinding
may be required to release liberate these grains
from the hematite. Conversely, the silica also
contains iron minerals. Clay impurities being
mainly confined to fractures and cavities can
be easily exposed and removed by washing.
The microscopic examination shows the early
stage of formation of colloform which has taken
plac e due to dehydration of goethite.
Subsequently, colloform due to dehydration of
goethite which gets altered into hematite was
observed. In the later stage lateralized portion
of the hard ore having intermingling of clayey
matter was observed. Due to metamorphism
different stages of alteration of goethite was
observed through the present microscopic
study.
3.4. Liberation result
I: Interlocking, Ge: Goethite, H: Hematite,
Q: Quartz, C: Clay material
Fig. 7: Photograph showing the liberated and
inter-locked grains of the minerals
 MPT-2013

(Grain Size (-10+14 mesh) in 25 pixel lens under 4. Conclusion

zooming stereo microscope In the Gua ore concentrate hematite crystallites
It is observed that the size distribution patterns coalesce forming larger polygonal grains in
in the samples after communition were almost matrix of goethite along with clay matter. The
similar (Table 2). Maximum quantity was concentrate also consists of a trace amount of
generated in the (-10+14#) size fraction and then magnetite in size frac tion of -200 mesh.
there was a decrease of material in the finer Alteration of iron ore due to dehydration of
fractions. However, in the finest fraction (i.e.,- goethite has been observed which has changed
300#) there was an increase in the material. This into hematite in same size fraction. Besides,
may be due to the release of clayey material in lateralized portion of the hard ore was observed
this fraction. showing intermingling of clayey matter within
Table 2: Data showing the weight percent the pit.
distribution in different size fractions The Kiriburu high LOI iron ore sample contains
goethite as the major iron mineral which
(size) Goe He Int. Gang Total Fe. appears to be an altered product of original
(-10+14#) 15.92 5.10 77.07 1.91 21.02 hematite. The subordinate iron mineral is
(-14+20#) 19.76 6.85 67.74 5.65 26.61
(-20+30#) 20.04 7.84 62.75 9.37 27.89 mainly goethite. Major gangue present is the
(-30+48#) 21.14 9.19 57.71 11.96 30.33 silica with a very low percentage of clay
(-48+65#) 23.80 10.43 52.94 12.83 34.22
(-65+100#) 25.62 12.30 46.60 15.48 37.92 minerals and also containing gibbsite and
(-100+150#) 26.02 13.78 42.34 17.86 39.80 Limonitic. Liberation of free iron from gangue
(-150+200#) 27.04 14.27 38.09 20.60 41.31
(-200+250#) 27.71 15.05 35.60 21.65 42.75 is best achieved at below 250 # size. Therefore,
(-250+300#) 30.44 19.08 28.32 22.16 49.52 it is proposed to simple crush the sample below
250# and adopts any suitable beneficiation
Fig. 8 shows the weight percent distribution method to separate the iron bearing minerals
indifferent size fractions of the Kiriburu iron from the gangues. Such desilicification process
ore samples vis-à-vis their mineral content. A shall enrich the iron content significantly and
marginal improvement in liberation can make the ultra-fines suitable for preparing
characteristic was observed below +65 mesh
pellets that can be utilized in blast furnace iron-
size fraction. An effective liberation of iron was
making. It is expected that the ultra-fines
obtained in the -250 + 300 mesh size fraction.
concentrate may contain slightly higher silica.
Also the fine-grinding of the material will
demand more consumption of energy.
Acknowledgement
Ministry of Steel and CSIR-NML for supporting
the research
Reference
IBM Report, 2012.
Fig. 8: Graphs showing the liberated free Sampath, M. K., 2012. Issue relating to Raw
hematite, free goethite, free gangue minerals materials, Beneficiation and Pelletisation of Iron
along with inter-locked grains at different size Ore for Iron & steel Making in India; IMPC 2012,
fractions of the goethitic ore New Delhi.

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50
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Characterisation of Eluvial Ruby (Corundum) From umerpadar,

Kalahandi, Odisha
S.K. Das* and J.K. Mohanty
CSIR-Institute of Minerals and Materials Technology, Bhubaneswar-751013, Odisha,
India

Abstract
Ruby is found in and around Jhilingdhar and Dumerpadar area, Kalahandi district, Odisha.
Corundum (and ruby) occurs in eluvial zone of altered metapyroxenite below the alluvial
overburden/soil of 0.5 to 4.0 m thickness. This paper describes mineralogy and textural
characteristics of eluvial corundum (and ruby) grains collected from different pits and trenches
within alluvial soil horizons at Dumerpadar.
Corundum is rose red, carmine or purple red in colour with well developed crystal faces and
mostly exhibitsbasal partings. The corundum grains contain inclusions of zircon and rutile, and
often surrounded by dark coloured spinel exhibiting corona texture. The corona thickness varies
from sample to sample and also within the same grains. Thick and thin veinlets of goethite and
diaspore traverse spinel aggregates. Sapphirine grains occur as rim around spinel and also as
fracture filing and in direct contact with corundum grains. Semi-quantitative chemical analysis
by energy dispersive spectrometer (EDS) attached to scanning electron microscope (SEM) indicated
that (i) corundum contains trace amounts of Fe and Cr, (ii) spinel is pleonaste-hercynite (Al-Mg-
Fe oxide) type with trace amounts of Cr, Mn, and Zn and (iii) sapphirine contains about 10% silica.
The corona textural feature suggests that under high P-T gradient in granulite facies
metamorphism and low fO2 corundum reacted with annite (or Fe-rich biotite) to form spinel:
3 Al2O3 + K(Mg,Fe)3AlSi3O10(OH)2 = 3 (Fe,Mg)Al2O4 + KAlSi3O8 + H2O
Corundum + Annite = Spinel + K-feldspar + Water
Keywords: Ruby, Corundum-spinel corona texture, Sapphirine

1. Introduction habits such as tabular, barrel shaped, columnar,

Corundum is typically found in aluminous
metamorphic roc ks, igneous roc ks
undersaturated with respect to silica and in
aluminous xenolith in igneous roc ks.
Corundum crystals show large variety of
* Correspending Author: S.K. Das, Chief scientist, Mineral
Processing Dep t., CSIR-IMMT, Bhubaneswar- 75 101 3,
Od ish a, Ind ia. E-mail: subir@immt.res.in; Mo b: +9 1-
9861724682
rhombohedral, prismatic and pyramidal.
Crystals from eluvial and alluvial deposits are
much water worn, broken and rounded and
subrounded. The c oloured varieties of
c orundum suitable for gemstones are
distinguished under the names of ruby for the
red variety and sapphire for the blue variety.
In India the production of corundum was 6600
tonnes in the year 2009-2010, and there was no

51

ruby production (Indian Bureau of Mines, 2011).
The entire resource of ruby (5348 tonnes) is
located in the state of Odisha, mainly in the
districts of Kalahandi and Nuapada.
At Jhillingdhar area, Kalahandi district, Mishra
and Mohanty (2006) reported occurrences of
ruby and corundum at the contact between
metapyroxenite and granite gneiss and also
eluvial placer ruby in the surrounding soil
horizons. In this paper, we report preliminary
investigation on eluvial corundum (ruby)
grains from Dumerpadar area, Kalahandi
district area, Odisha.
2. Materials and Methods
Corundum (ruby) samples were collected by
hand picking from different pits and trenches
dug within alluvium zone near Dumerpadar
village. The size of the samples ranges between
20 to 3 mm. In the laboratory the samples were
washed with dil. HCL to remove the
ferruginous coatings followed by cleaning with
water in ultrasonic machine. Thin sections of
the grain mounts were prepared. Polished
sections were made for study under ore
microscope and Scanning Electron Microscope
(SEM). Semi-quantitative analaysis of the
mineral phases were done by EDS attached to
SEM.
3. Results
3.1. Megascopic description
The colour of the ruby grains vary from rose
red, purple red and pale pink. Basal parting is
prominent with conchoidal fracture, and thin
fractures are also noted within ruby grains
(Figs. 1 and 2).
3.2. Microscopic description
Under thin section the colour of ruby is purple
red to faint pinkish to colourless. The grains
are mostly fractured and the fracture patterns
are perpendicular to each other and also
anastomising in character (Figs. 3 and 4). Ruby
52
MPT-2013
grains frequently contain inclusions of rutile
(Fig. 5). Rutile is blood red in colour. Often
zircon grains are also noted within ruby grains
(Fig. 5 and 6). Corona texture is well observed
in which spinel partially surrounds the host.
Spinel is translucent, light blue in colour and
occurs as polygonal to subhedral grains. In a
few samples, subhedral sapphirine grains are
noted. It exhibits prominent pleochroism from
blue, pale yellow to sapphire blue and strong
second order interference colour. It occurs as
partial rim around spinel (corona texture), as
veinlets, fracture and cavity filling within
c orundum and spinel. The textural
characteristics indicate that sapphirine is
formed at the expense of the spinel and replace
the latter minerals. Ore microscopic studies
indicate fine veins of goethite within spinel and
sapphirine.
3.3. SEM studies and mineral chemistry by EDS
The SEM micrographs of ruby grains are shown
in different images (BSE images) (Figs. 7-12). In
BSE images the contrast between the different
minerals is distinct. Corona texture shown by
corundum-spinel is distinct in Fig. 7 while Fig.
8 shows suc c essive rims of spinel and
sapphirine around corundum grain. Sapphirine
occurs as fracture filling and cavity filling
within corundum grain (Figs. 9 and 11). Fig. 12
shows direct contact between sapphirine and
corundum with fine veins of diaspore within
sapphirine. The dendritic pattern in spinel
grains is illustrated in Fig. 10. Fine veinlets of
goethite and hematite are observed within
spinel grains.
The semi-quantitative analysis of corundum,
spinel and sapphirine is given in Table 1.
Corundum contains minor to trace amounts of
Fe and Cr which occur in the crystal structure
of corundum. The incorporation of these
elements imparts red colour to corundum
(Bowles et al., 2011). Spinel contains high
amounts of alumina (Al2O3= 66.15%) and
 MPT-2013

moderate amounts of Fe and Mg and minor The textural observation in the studied
amount of chromium. The analytical data corundum (ruby) grains suggests that the
indicate that the spinel is of hercynite-pleonaste spinel is derived from reaction between
c omposition. Sapphirine c ontains high corundum and other silicate mineral. In the
amounts of alumina (Al 2 O 3= 66. 46%), eluvial corundum grains, no other silicate
moderately high amounts of Mg (MgO=18.34%), mineral, except sapphirine, is found. This is due
moderate amounts of silica (SiO2=9.46%) and possibly to transportation, reworking of the
iron (FeO= 5.24%) and minor amount of grains and weathering conditions in which the
chromium. other primary silic ate minerals were
Table 1: Semi quantitative analyses of destroyed. Spinel grains contain significant
corundum (Crd), spinel (Spl), sapphiine (Spr) amounts of Fe and Mg suggesting that spinel
and diaspore (Dias). Analyses are recalculated might have been formed by reaction of
to 100 corundum and Mg-Fe containing silic ate
mineral, biotite. Sapphirine is a reaction
Crd Spr Dias Spl
MgO 0 18.34 0 19.73 product of spinel and other silica bearing
Al2 O3 99.35 66.46 97.89 65.15 mineral.
SiO2 0 9.46 0 0 3 Al2O3 + K(Mg,Fe)3AlSi3O10(OH)2 = 3
FeO 0.42 5.24 1.95 13.77 (Fe,Mg)Al2O4 + KAlSi3O8 + H2O
Cr2 O3 0.23 0.50 0.16 1.35 Corundum + Biotite
100 99.99 100.00 100.00 = Spinel + K-feldspar + Water
3.4. Discussions 4. Conclusions
Many authors have noted that spinel -
(1) The eluvial corundum (ruby) grains are
corundum intergrowth formed due to reactions
purple red in colour but mostly highly fractured
at high temperature and pressure metamorphic
and contain inclusions of rutile and zircon.
conditions involving:
(2) Corundum-spinel corona texture is well
Biotite + Corundum = Spinel + K-feldspar
developed in a few grains suggesting reaction
+water
of corundum and biotite to form spinel during
Corundum + Sillimanite = Spinel (hercynite) +
high grade metamorphic episodes. Sapphirine
Quartz
occurs in contact with corundum and also as
Corundum + Garnet = Spinel
partial rim around spinel. Sapphirine is formed
Sapphirine ((Mg,Fe2+,Fe3+Al)2O2[(Al,Si)6O18] is
by reaction of spinel and silicate mineral under
mostly reported from aluminium rich silicon
metamorphic conditions.
poor rocks of the high grade metamorphic rocks,
granulite and hornblende granulite. Sapphirine Acknowledgements
is formed by reaction of: (i) Spinel (Mg, Fe) Al2O4)
+ Silica (SiO 2), (ii) spinel (Mg, Fe) Al 2O4) + Authors are grateful to Prof. B.K. Mishra,
sillimanite (Al2O3.SiO2), (iii) spinel + garnet, (iv) Direc tor, IMMT, Bhubaneswar for his
Spinel (Mg, Fe) Al2O4) + Cordierite and (v) encouragement and kind permission to publish
Cordierite + Spinel + Corundum (Bowles et al., this paper. The authors thank Mr. M.K. Senapati,
2011 Prakash et al, 2013). Prakash et al. (2013) Joint Director of Geology, Directorate of Geology,
also reported different generation of sapphirine Govt. of Odisha for discussion and Mr. Mund at
in granulites of Eastern Dharwar Craton. Bhawanipatna for sample collection.

53
 MPT-2013

References Mishra, B,.P and Mohanty, B.K. 2006.

Bowles, J.F.W., Deer, R.A., Vaughan, D.J. and
Zussman, J. 2011: Rock Forming Silicates:
Non Silic ates (Oxides, Hydroxides,
SulphidesI. 5A, 2 nd Ed., The Geological
society.
Indian Mineral Year Book, 2011. Published by
Indian Bureau of Mines, Nagpur. Govt. of
India.
Gemstones. Geology and Mineral
resources of Orissa. SGAT publication
(Bhubaneswar), 246-262.
Prakash, D., Singh, P.C. and Hokada, T. 2013. A
new occurrence of sapphirine-spinel-
corundum-bearing granulite from NE of
Jagtiyal, Eastern Dharwar Craton, Andhra
Pradesh. J. Geol. Soc. India, 82, 5-8.

Fig. 1: Columnar ruby with Fig. 3: Fractures in ruby

Fig. 2: Pink ruby with
pits and basal partings. perpendicular to each other.
fractures.

Fig. 4: Ruby with Fig. 5: Ruby with rutile

anastomising fractures. Fig. 6: Ruby with tabular
and zircon inclusions.
inclusions.
Crd
Crd Crd
Spr
Spl
Spl
Spr

Fig. 8: Corona texture: Fig. 9: Sapphirine (Spr) as

Fig. 7: Corona texture: corundum (Crd) is surrounded
corundum (Crd) surrounded fracture filling vein within
by spinel (Spl) and further by corundum grain (Crd).
by spinel (spl). sapphirine (Spr).

54
 MPT-2013

Crd Dias
Crd
Spr

Spr

Fig. 10: Spinel grain showing Fig. 11: Sapphirine (Spr) Fig. 12: Contact of
dendritic texture. Veins of within spinel as inclusion. corundum (Crd) and
goethite in spinel sapphirine (Spr). Diaspore as
veins.

*******

55
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Heavy Mineral Distribution and Characterisation of Ilmenite of

Astaranga and Ersama Coastal Tracts, Odisha
S. K. Das*, B.K. Nayak and S. Aich
Mineral Processing Department, CSIR-Institute of Minerals and Materials Technology,
Bhubaneswar-13, Odisha
Abstract
Twenty two placer samples were collected by hand drilling upto 2 m depth at different locations
along Astaranga and Ersama coastal tracts, Eastern Odisha. The percentage of total heavy minerals
in Astaranga and Ersama sectors varies from 2.26 to 13.64 and 3.88 to 23.07% respectively. The
heavy minerals are garnet, sillimanite, ilmenite, rutile, zircon, monazite and pyriboles with trace
amounts of magnetite, goethite, biotite, apatite, chlorites etc. In all the samples, the bulk raw
sands are mostly distributed between 500 and 125 µm sizes and the silt size fraction (<63 µm) is
negligible (<0.1%). The heavy minerals in both the sectors are concentrated between 500 to 63 µm.
The heavy minerals occur as free grains. Ilmenite constitutes 31.91-39.95% (av. 34.82%) and 32.62-
47.11% (av. 41.80%) of total heavy minerals of Ersama and Astaranga sectors respectively. Ilmenite
is finer grained compared to garnet and sillimanite and predominantly concentrated below 125
µm size. There is variation of ilmenite grains from pure ilmenite to impure ones having intergrowths
with alteration phases and inclusions of other oxide and silicate minerals. The ilmenite of both the
area is sparsely altered to secondary phases such as pseudorutile, leucoxene and rutile along
fractures, cavities and grain boundaries. The altered phases occur as coarse to fine irregular
patches, bands, flames, streaks and rims around ilmenite grains. Chemistry of ilmenite and its
altered phases (pseudorutile and leucoxene) was investigated by energy dispersive spectometer
(EDS) attached to scanning electron microscope (SEM). Significant concentrations of coarse and
free heavy minerals in the placer samples suggest that Astaranga and Ersama coastal belt forms
a potential deposit for exploitation of heavy minerals.

Keywords: Total heavy minerals; mineral chemistry; resource Odisha.

1. Introduction
The Indian coastline of 6500 km stretch is
marked by accumulation of various types and
grades of placer deposits. Heavy mineral
deposits are mostly concentrated in the states
of Kerala, Tamil Nadu, Odisha and Andhra
* Correspending Author: S. K. Das, Chief Scientist, Mineral
Processing Department, CSIR-Institute of Minerals and
Materials Technology, Bhubaneswar-13, Odisha, E-mail:
subir@immt.res.in
Pradesh. The beach placer sand deposits of
Chavara in Kerala, Manavalakurichi in Tamil
Nadu and Chhatrapur in Odisha are under
active exploitation by Indian Rare Earth Ltd.
(IREL), Govt. of India.
The beach placer sand deposits serve as a major
source of economic minerals due to their easy
mineability, the availability of cost effective
mining technology and beneficiation practices
and better profit ratio. The state of Odisha is

56

well known for its huge reserve of placer
deposits of about 116 million tonnes and the
Chhatrapur deposit has about 62.06 million
tonnes deposit (Padhi and Mishra, 2006).
Besides Chhatrapur deposit, the other
important localities along the coasts are (a)
Ramayapatna, (b) Markandi, (c) Mayurpada, (d)
Niladripur, (e) Paluru, (f) Malud, (g) Astaranga
and (h) Ersama. The c oastal trac t near
Astaranga and Ersama area, located on either
side of confluence of Devi River with the Bay of
Bengal (Fig. 1), contains significant quantity of
placer deposits. The Eastern Ghats Mobile Belt
consisting of charnockite, khondalite and
migamatite acts as provenance for coastal
placer deposits of southern coast of Odisha
(Bhattacharya and Sengupta, 1994; Dwivedy,
1995; Mohanty et. al., 2004).
This paper focuses on the evaluation of (a) heavy
mineral concentrations in beach and dunes in
22 nos. of vertical profiles of 2 m depth of
Astaranga and Ersama coastal belts, (b)
concentrations of heavy minerals in sizes, (c)
individual heavy mineral phase distribution
in different sizes and (d) c hemic al
characteristics of ilmenite and its alteration
products. This study will help in understanding
in selecting beneficiation strategy of the coastal
sands.
2. Materials and Methods
Placer sand samples (22 nos.) were collected by
hand auger drilling upto a depth of 2 metre from
the beaches and dunes southeast of Astaranga
and Ersama towns, Puri and Jagatsinghpur
districts respectively, Odisha (Fig. 1). The
samples were dried, thoroughly mixed and
about 1 kg sample obtained by repeated coning
and quartering method. In the laboratory, the
dried samples were reduced to about 200 gm
by coning and quartering, treated with dilute
HCl to remove the shell materials followed by
repeated washing with water to remove the
57
MPT-2013
ultrafine slimes. Bulk samples were prepared
by thoroughly mixing the samples of the two
sectors separately. The samples were wet
sieved into different size fractions, viz., +1, -
1+0.5,-0.5+0.25, -0.25+0.125, -0.125+0.063 and -
0.063 mm sizes. From each size fractions, heavy
minerals were isolated by gravity separation
(sink-float method) using a heavy liquid
(bromoform; d=2.89) and total heavy mineral
content (THM) in the samples was determined.
In some selected bore hole samples, the
distribution of individual heavy mineral
phases in each size fractions were determined
by grain counting (min. 300 grains) using
stereo- and petrological microscopes. Semi-
quantitative mineral c ompositions were
obtained by EDS (M/S. Bruker) attached to SEM
(M/s. ZEISS) operating at 25 kV and beam
current of 11 µA.
Fig. 1: Location of the bore holes samples
along the coastal tracts southeast of Astaranga
and Ersama, Puri and Jagatsinghpur districts,
Odisha
3. Results and Discussion
3.1. Total heavy minerals (THM) in bulk
samples and heavy mineral (HM) in size
fractions
The total heavy mineral (THM) concentrations
in samples of each drill hole of two sectors are
 MPT-2013

shown in Fig. 2. In this figure, HM contents of 10.31 (av. 5.38) and Astaranga: 0.45-1.85 (av.
different size fractions of each sample are also 1.64), 0.85-3.34 (av. 1.63) and 0.84-4.13 (av. 2.78).
given. The THM contents in the samples of The maximum percents of rutile, zircon and
Astaranga and Ersama sectors vary between monazite of Ersama and Astaranga samples are:
2.26-13.64 (av. 6.80%) and 3.88-23.07% (15.43%) 0.14, 0.35, 0.09 and 0.06, 0.15 and 0.08
respectively. The heavy mineral contents in respectively (Table-1). The distribution of
different size fractions of the samples indicate garnet, sillimanite and ilmenite in each size
that heavy minerals are strongly distributed fractions are given in Figs. 3 and 4. The results
between 0.25-0.125 mm (av. 0.185 mm), followed indicated that (a) in all samples, ilmenite
by 0.125 -0.063 mm (av. 0.094 mm) and 0.5-0.25 percents in the THM are high to very high in
mm (av. 0.375 mm) sizes (Fig. 2). The HM 0.125+0.063 mm constituting 49-75.4 (av.
concentrations in +0.5 mm and below 0.063 mm 60.5%) and 52.8-69.75 (av. 63.79%) respectively
sizes are in negligible amounts. for Ersama and Astaranga samples. The data
25 23.07 22.79 22.70 suggest that ilmenite is finer grained compared
W t.%

21.69
20 17.04 17.71
15.43
Ersama and Astaranga to garnet and sillimanite. (b) Garnet and
13.64
15
11.34 10.98 10.58
12.66 12.88
sillimanite are predominantly concentrated in
10
4.24
7.69
4.62
6.29 6.90 6.06 6.80 coarse sizes, -0.5+0.25 and -0.25+0.125 mm, and
3.88 3.28
5 2.26
1.96
the distribution is variable (Figs. 3 and 4). (c)
0
E-1 E-2 E-3 E-4 E-5 E-6 E-7 E-8 E-9 E- E- E- A- A- A- A- A- A- A- A- A- A- A- A- Zircon and monazite are concentrated below
10 11 Av. 12 13 14 15 16 17 18 19 20 21 22 Av.
0.125 mm. (d) In the coarsest size fractions
Fig. 2: THM contents (wt.%) and HM (+0.50 mm) goethite and limonite percents are
distribution (%) in different sizes. Index: E-1 high.
etc. – Ersama, A- Astaranga; Av. Average. Open Table 1: Mineral contents (wt.%) in the samples
bar- THM with contents (wt.%); Filled triangle: of Ersama (E) and Astaranga (A) sectors
0.500+0.25 mm; Filled square: 0.250+0.125 mm;
Ersama
Filled diamond shape: 0.125+0.063 mm. Rutil Mo
Sample Gar. Silli Ilm e Zir n Pyx Lim Oth. Total
E-1 4.81 5.34 5.75 0.08 0.35 0.05 0.48 0.04 0.15 17.09
3.2. Individual heavy mineral distribution E-2 4.56 2.56 3.62 0.04 0.08 0.06 0.30 0.08 0.04 11.34
(wt.%) in different size fractions and in total E-3 1.03 1.01 1.55 0.02 0.10 0.02 0.11 0.01 0.03 3.88
E-8 4.33 5.46 6.69 0.11 0.06 0.03 0.58 0.06 0.38 17.70
sample E-9 8.89 8.02 10.31 0.14 0.13 0.09 0.88 0.15 0.42 29.04
E-Av. 4.63 4.42 5.38 0.08 0.14 0.05 0.47 0.07 0.20 15.45
Twelve samples (6 nos. from each sector) were Astaranga
A-12 1.85 1.58 3.59 0.03 0.14 0.01 0.33 0.01 0.08 7.62
taken for determination of different heavy A-15 0.79 0.87 1.17 0.03 0.05 0.01 0.16 0.03 0.03 3.28

mineral species (Table-2). The dominant heavy A-16 4.37 3.34 4.13 0.06 0.15 0.05 0.51 0.05 0.01 12.66
A-20 1.26 1.30 2.67 0.02 0.13 0.03 0.61 0.00 0.04 6.06
minerals identified are garnet, sillimanite, A-22 0.45 0.85 0.84 0.02 0.04 0.01 0.07 0.00 0.00 2.27
A.-Av. 1.64 1.69 2.78 0.03 0.10 0.02 0.33 0.02 0.03 6.65
ilmenite, rutile, zircon and monazite with small
amounts of magnetite, goethite, apatite, epidote, 100 Ersama

sphene, pyriboles etc. Quartz is the dominant

% mineral distr.

80
60
lighter mineral constituent. Amongst the HM, 40
20
garnet, sillimanite and ilmenite constitute the 0

major percentages. For Ersama and Astaranga 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

E-1 E-2 E-3 E-8 E-9 E-A

samples, range and average of garnet,
sillimanite and ilmenite are (Table-1): Ersama: Fig. 3: Mineral distribution (%) in different size
fractions and the average of Ersama sector. E-1
1.03-8.89 (av. 4.63); 1.01-8.02 (av. 4.42) and 1.55-
etc. denotes Sample Nos..

58
 MPT-2013

E-A- Av. of 11 Ersama samples. Index: leaching of hematite lamellae from ilmenite (Fig.
1,4,7,10,13: -0.500+0.250 mm; 2,5,8,11,14,17: - 6). Hematite also contains exsolution laths and
0.250+0.125 mm; 3,6,9,12 ,15,18: -0.125+0.063 streaks of ilmenite. Ilmenite grains variously
mm. alter to pseudoilmenite, pseudorutile,
100
leucoxene/rutile along frac ture, margins,
Astaranga
cavities and structural weak planes (Figs. 7-8
% mineral distb.

80

60
and SEM BSE images: Figs. 9-12). The alteration
40

20
products are present as coarse to very fine
0 bands, veins, granules, dots, flames, and
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18

A-12 A-15 A-16 A-20 A-22 A-A

irregular patches within ilmenite host (Figs. 7-
12). The altered products are spongy, fine
Fig. 4: Mineral distribution (%) in different size grained, dark grey, grey, grey white and white
fractions and average of Astaranga sector. A- in colour and exhibit moderate to strong
12 etc. denotes Sample Nos.. A-A- Av. of 11 interference colour in shades of brownish and
Astaranga samples. Index: 1,4,7,10,13: - yellowish tints (Fig. 8). Few ilmenite grains are
500+0.250 mm; 2,5,8,11,14,17:-0.250+0.125 completely altered to a fine grained mass
mm; 3,6,9,12,15,18: -0.125+0.063 mm. consisting of pseudorutile, leucoxene, rutile and
3.3. Mineralogy goethite. The alteration products are also
frequently intimately associated with each
The mineralogical characteristics of heavy other.
minerals in the two sectors are similar. Garnets
are mainly represented by almandine and 3.4. Mineral chemistry of ilmenite and its
subordinately by pyrope. Garnet is mostly alteration products
subrounded and sub angular, with buff red to Semi-quantitative analyses of ilmenite and its
brown c olour and conc hoidal frac ture. alteration products, obtained by EDS attached
Inclusions are noted within garnet. Sillimanite to SEM, are given in Table 2. The leucoxene
is tabular, rectangular and squarish and some (points- A-3, A-5, E-1 to E-4, E-6) is highly
times stained by iron hydrooxides. Monazite enriched in titanium (TiO2= 80.09-97.94%) and
grains are rounded to elliptical, whereas zircon depleted in iron (FeO(t)= 1.11-17.71%) contents
grains are generally elongated with edges. Some (Table-2). Silica (SiO 2) and alumina (Al2O3)
of the zircon grains are rounded to sub rounded contents in leucoxene phase vary between 0.00-
indicating long distance transport. Inclusions 9.23% and 0.00-9.36%. In pseudorutile phase the
of ilmenite, quartz and monazite are observed FeO(t) and TiO2 percents are significantly higher
in zircon grains. Rutile grains are tabular. and lower than leucoxene phase and vary
Ilmenite grains are tabular, sub rounded and between 30.13 to 40.04 and 59.96-66.12
show complex internal structure. They vary respectively. Several authors have studied the
from pure ilmenite (without any inclusions and alteration characteristics of placer ilmenite
alteration parts) to impure varieties containing grains from India and abroad (Frost et al, 1983;
exsolution lamellae of hematite and complex Chernet, 1999; Nair et al, 2006). The chemistry
alteration products (Figs. 5-10). The ilmenite of alteration is controlled by processes such as
grains are sparsely altered. Microscopic studies (a) simultaneous leaching and oxidation of
under reflected light reveal exsolution bands, ferrous iron from ilmenite to form
lamellae, blebs, spots of hematite in ilmenite pseudoilmenite and pseudorutile and (b)
grains (Fig. 5). The linear cavities indicate subsequent leaching of iron during the

59

transformation of pseudorutile to leucoxene. The
latter proc ess is also assoc iated with
hydrolysation. Frost et al. (1983) noted that
alumina and silica were introduced to the
altered phases of ilmenite from surrounding
environment during alteration process. The
reactions for transformation of ilmenite to
pseudorutile and leucoxene phases are (Frost
et al., 1983):
6FeTiO3 (ilmenite)+1.5O2+3H2O 2Fe2Ti3O9
(pseudorutile)+2Fe(OH)3
Fe2Ti3O9 (pseudorutile) +3H2O 3TiO2
(leucoxene or rutile)+2Fe(OH)3
4. Conclusions
 The heavy minerals of Ersama and
Astaranga coastal sectors predominantly
consisted of ilmenite, garnet, sillimanite,
rutile, zircon and monazite. The total heavy
mineral percents varied from 3.88-23.07 (av.
15.43%) and 1.96-13.64 (av.6.80%)
respectively for Ersama and Astaranga
sector respectively.
 The heavy minerals are mostly concentrated
between 0.50 mm to 0.063mm sizes
 Ilmenite is finer grained compared to garnet
and sillimanite and predominantly occur
below 0.125 mm size. Ilmenite constitutes
31.91-39.95% (av. 34.82) and 32.62-47.11% (av.
41.80) of total heavy minerals of Ersama and
Astaranga sectors respectively. Ilmenite is
sparely altered to pseudorutile and
leucoxene which occur as fine to coarse
irregular patches, blebs, streaks, laths, veins
and rims.
 In the coastal tract placer samples of Ersama
and Astaranga sectors, the heavy minerals
occur in liberated form and relatively coarse
grained (>0.063 mm) and therefore, can be
benefic iated by adopting suitable
c onc entration techniques to obtain
individual heavy mineral phases.
60
MPT-2013
Acknowledgements
Authors are grateful to Prof. B.K. Mishra,
Direc tor, IMMT, Bhubaneswar for his
encouragement and kind permission to publish
this paper.
References
Bhattacharya, S., Sengupta, R., 1994. Surface
microstructures of heavy minerals from
Bay of Bengal off Gopalpur, Orissa. J. Geol.
Soc. India, 44, 175-184.
Chernet, T., 1999. Applied mineralogical studies
on Australian sand ilemnite concentrate
with special reference to its behaviour in
sulphate process. Mineral. Engg., 12, 485-
495.
Dwivedy, K.K., 1995. Reserves, resources and
geology of titanium deposits. Titanium, 1,
16.
Frost, M.T., Grey, I.E., Harrowfield, I.R., Mason,
K., 1983. The dependence of alumina and
silic a c ontents on the extent of the
alteration of weathered ilmenite from
western Australia. Min. Mag., 47, 201-208.
Mohanty, A.K., Sengupta, D., Das, S.K., Saha, S.K.,
Van, K.V., 2004. Natural radioactivity and
radiation exposure in the high background
area at Chhatrapur beach placer deposits
of Orissa. India. J. Environ. Radioact, 75,
15-33.
Padhi, S.K., Mishra, P.C., 2006. Beach Sand
Minerals. Geology and MineralRresources
of Orissa. Society of Geoscienists and
Allied Technologists (SGAT) Publication,
168-180.
Nair, A.G., Suresh Babu, D.S., Vivekanandan,
K.L., Vlach, S.R.F., 2006. Differential
alteration of ilmenite in a tropical beach
placer, Southern India: Mic roscopic
studies and electron probe evidences.
Resource Geology, 56, 75-81.
 MPT-2013

A-5
A-1
A-2

A-6
A-4
A-3

Fig. 9: Ilmenite with altered phases (grey) as

Fig. 5: Fine exsolution lamellae of hematite in lines and irregular patches. A-1- Hercynite, A2-
ilmenite grain. Astaranga. diaspore. EDS points shown. BSE image.
Astaranga.

80 µm 12
A-12

11
A-11

Fig. 10: Ilmenite (white) showing alteration

Fig. 6: parallel arrangements of linear pits rims, lines and flames (grey) with EDS points.
within ilmenite grain. Astaranga BSE image. Astaranga.

Er-1
Er-2

Fig. 11: Altered phases (grey) occur as slender

Fig. 7: Leucoxene as irregular patch and as needle and angular bodies within ilmenite
partial rim around ilmenite grains. Ersama. (grey white). EDS points shown. BSE image.
Ersama.

Er-4

Er-5

Er-6

Er-3

Fig. 12: Altered phases (grey) occur as thick

Fig. 8: Leucoxene showing strong internal re- partial rims around and lines within ilmenite
flection. Crossed nicols. Ersama. grain. EDS points shown. BSE image. Ersama.

61
 MPT-2013

Table 2: Semi-quantitative analyses (wt.%) of ilmenite and the alteration products. (A)- Astaranga;
(B)- Ersama. Index: Herc.- Hercynite, Dias.- Diaspore, Leuc.- Leucoxene, Ilm.- ilmenite, Pseu.-
Pseudorutile.

(A) A-1 A-2 A-3 A-4 A-5 A-6 A-11 A-12

Herc. Dias. Leuc. Ilm. Leuc. Pseu. Ilm. Pseu.
Al2 O3 58.70 97.84 1.54 0.00 2.42 0.81 0.00 1.44
MgO 4.98 0.00 0.00 0.00 0.00 0.00 0.00 0.00
CaO 0.00 1.13 0.00 0.00 0.00 0.00 0.00 0.00
SiO2 0.00 0.00 0.98 0.00 0.63 0.00 0.00 0.00
TiO2 0.00 0.00 92.61 48.21 80.92 66.12 48.88 64.69
MnO 0.00 0.00 0.00 0.00 0.00 2.94 0.00 0.00
FeO 36.32 1.03 4.87 51.79 16.02 30.13 51.12 33.88
Total 100.00 100.00 100.00 100.00 100.00 100.00 100.00 100.00

(B) E-1 E-2 E-3 E-4 E-5 E-6

Leuc. Leuc. Leuc. Leuc. Pseu. Leuc.
Al2 O3 2.82 3.23 0.00 9.36 0.00 1.25
SiO2 2.84 2.97 0.00 9.23 0.00 0.84
TiO2 93.22 82.80 97.94 80.09 59.96 78.64
Cr2 O3 0.00 0.00 0.00 0.00 0.00 0.18
FeO 1.11 11.00 2.06 1.32 40.04 17.71
MnO 0.00 0.00 0.00 0.00 0.00 1.38
Total 100.00 100.00 100.00 100.00 100.00 100.00

*******

62
 MPT-2013

COMMUNITION & CLASSIFICATION

63
 MPT-2013

64
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Exploring New Grinding Aids to Improve the Energy Efficiency

of Dry Grinding Process

Veerendra Singh1*, P. K. Banerjee1, V. K. Saxena2 and R. Venugopal2

1
Research and Development, Tata Steel, Jamshedpur-831001, India
2
Indian School of Mines, Dhanbad, Jharkhand-826004, India

Abstract
Grinding is an age old techniques of size reduction but most of the milling technologies are energy
inefficient. Various studies have been carried out to improve energy efficiency of grinding processes
but limited success has been achieved. Use of additives is common practice in wet as well as dry
grinding operations but it is much difficult to understand the underlying mechanism for dry
grinding process. This study has been carried out to estimate the effect of five different types of
grinding additives (Expansive Solids – Split AG, Disintegrators- Agar Powder, Sublime Solids-
Naphthalene, Acicular Particles- Wollastonite, and Swelling Solids- Alginic Acid) on dry grinding
process. Manganese ore samples of 0-1mm was properly mixed, characterized and subdivided for
test work. Experiments were conducted in a laboratory scale ball mill. Additive dosages were
kept 3, 5 and 7% of ore weight. Size analysis of grinding products was compared using D36.8, D50
and D80 calculated using Rosin Rammler equitation. Effects of additives on fracture pattern and
particles surfaces were analyzed using SEM and QEMSCAN mineralogy analyzer. It was found
that lime based additive Split AG is most effective dry grinding additive and it is able to reduce
coarser fraction (>150microns) by 5% using 5% additive dosages. Algenic Acid and Wollastonite
also shown positive effect on size reduction and reduced the coarser fraction by 2 to 5%. D36.8
particle diameters were reduced by 50, 27 and 19 micron for Algenic Acid, Split AG and Calcium
Silicate, respectively. Naphthalene and Agar powder create glue effect on particle surfaces and
did not affect grinding significantly. It was found that Split AG, Algenic Acid and Calcium Silicate
have the potential to develop as the dry grinding additives and other organic additives can be
explored to develop the dust reducing agents for dry grinding.

Keywords: Grinding; additives; size distribution; disintegrator; swelling solid; fracture.

1. Introduction size reduction and bigger part of energy is

consumed by machine itself (Somasundaran
Grinding is an age old techniques of size
and Lin 1972). Grinding is an important unit
reduction but most of the milling technologies
operation in mineral, cement, metallurgy,
are considered as energy inefficient which
pharmac eutic al and c hemic al industry.
consumes only smaller amount of energy in real
Literature review of subject indicates that

65

various attempts has been made to improve
the energy efficiency and these can be broadly
c lassified into two c ategories i.e., (a)
Tec hnologic al advancement (b) Material
pretreatment. Technological advancements are
focused to design and develop energy efficient
grinding mills and crushers. High Pressure
Roller Mill (HPRM), Sala Agitate Mill (SAM),
Eccentric Vibrating Mills (ESM) and Jet Mills
are commercially available new technologies
(Daniel, 2006; Marmor, 1993; Gock and Kurrer
1998; Thaler 2000). The major pretreatment
methods developed are chemical, thermal,
ultrasonic, microwave treatment and electric
disintegration (Klimpelm and Austin 1982;
Singh et al. 2012; Gaete-Garreton et al. 2000;
Kumar, et al, 2010, Wang et al. 2011). Most of
these methods still not commercialized mainly
because of the cost economic problems.
High grade natural resources are depilating and
mineral industry is facing challenges to process
the low grade ores and process tailings to
Table 1: Different grinding additives and working mechanism (Fuerstenau 1995; Paramasivam
and Vedaraman, 1992a; Hasegawa et al. 2006; El-Shall 1984; Paramasivam and Vedaraman 1992b;
Wang and Wang 2009)
S. No. Effect
1. Modification of the flow of pulp in the
grinding mill
2. Influence on re-agglomeration of the
freshly produced fines
3. Modification of frothing characteristics of
the pulp during grinding;
4. Influence of interactions between mineral
particles and balls and mill wall and
among particles themselves
5. Influence on the strength of the material
due to:
 Effect on crack initiation and crack
extension
 Energy retardation of rejoining or
sealing of the freshly created cracks
MPT-2013
recover values. Comminution is required to
liberate the valuable minerals from gangue in
finer sizes. Grinding additives are most simple
and easy to implement improvement method
for industries. But the major problem is
contamination of the product and it can be
addressed by proper selection of the grinding
additive. Rose and Sullivan have summarized
most of the work reported prior to 1950, and
Fuerstenau reviewed the efforts made prior to
80s about grinding additive literature (Rose et
al. 1958, Fuerstenau 1995). Literature review
reveals that effect of grinding additives can
classified in five major categories and these are
presented in table 1. Flow properties, particle
agglomeration, frothing, media-partic le
interactions and softening of the material are
the main area of interest for researcher to
develop a grinding additive but still low
availability and popularity of grinding
additives indicate the research gap in the area.
Additives
Water
Alcohol, Glycol (Ethylene glycol, propylene glycol,
butylenes Glycol, Triethanol amine. Carbon
tetrachloride, Methyl cyclohexane, Nitrogen, HCI
and NaCH.
Flotigam P (C12-C14) , Amine, Coconut oil, Oleic
acid, Sodium oleate, Amine acetate, sodium silicate,
Dodecyl ammonium chloride, caustic soda and soap
Amine dodecylammonium chloride, Ferric salts
(MgCI2, CaCI2, and FeCl2, and FeCI3),
Tripolyphosphate
Hardness reducers- NaCl, NaOH, Na2CO3, MgCl2,
CaCl2 and AICIJ, AlCl3, Na2CO3
Organic chemicals- With polar molecules xylene and
benzene, oleylammonium acetate, alcohol
66

Dry grinding is now being reconsidered due to
emerging water and tailing disposal constrains.
But development of grinding additives for dry
grinding is more challenging than wet
processing. Wet grinding provided proper
mixing and dispersion of additives in materials
and these additives can change the flow
properties to improve grinding characteristics.
But these advantages are not with dry grinding
and measurement of the effect of these additives
on particles is difficult to measure. Cement
industry commonly opt the dry grinding
process and first dry grinding additive was
explored almost 60 years back. Commonly used
dry grinding additives are amines, glycol,
resins, cod oil, kojic acid, carbon black wool
grease, calcium sulphate, urea, asphaltenes, etc
(Fuerstenau, 1995). However, grinding aids have
scarcely been utilized in fields other than the
cement industry, because of the undesirable
contamination of the product and the lack of
instruction in application of grinding aids. Use
of grinding additives on other than cement has
also been mentioned in literature. Some of the
examples are wool grease for gypsum, limestone
and quartz, effect of hydrocarbons in milling of
aluminum powder, the sue of silicones in ball
milling of quartz, and the use of acetone, carbon
tetrachloride, benzene and nitromethane for
grinding of glass, marble and quartz
(Fuerstenau, 1995). The mechanism behind the
effect of dry grinding additives has been studies
by Paramasivam and Vedaraman 1992 and
they concluded that the additive action depends
on the nature of the additive used, the size
distribution of the mill c ontent and the
adsorption phenomena of additive molecules
on particle surfaces which alters the powder
flowability and particle breakage mechanisms.
The surface tension and dipole moment of the
liquid are assumed to influence the solid-liquid
67
MPT-2013
surface interactions, whereas the kinematic
viscosity and vapor pressure are expected to
influence the drag force acting over the particles
during grinding (Paramasivam and
Vedaraman, 1992a; Hasegawa et al. 2006; El-
Shall 1984; Paramasivam and Vedaraman
1992b; Wang and Wang 2009). These effects can
be broadly classified into four areas:
(a) Solid flow properties: Dry grinding additives
can increase the surface smoothness and
c an reduc e or increase the partic le
agglomeration during milling. These
phenomena can increase the uniformity of
grinding feed and will provide the equal
opportunity to all kinds of particles for
grinding.
(b) Abrasion and erosion: Dry grinding additive
can modify the surface hardness and
surfaces charges. The variation in this can
help for particle erosion and abrasion
which may result in increased particle size
reduc tion. This phenomenon c an be
increased by acidic additives as well as
additives with acicular particles.
(c) Fracture propagation: The additives can
accumulate in the fractures and pores on
partic les surfac es due to available
moisture. The polar additives can affect the
surface energies at fracture openings.
Swelling of these additives can impact the
pressure on the fracture and it can break
the partic les. Various kinds of super
disintegrator used by pharmaceutical
industry can be used for these purposes.
(d) Heat effect: During the milling an additive
will be heated due to energy release due to
collision of grinding media. Whereas some
additive release the energy during
hydration and some absorb the heat
during sublimation. These additives can
change the environment inside the mill

whic h c an affec t the grinding proc ess
significantly.
Present study is carried out to find new
grinding additives and tried to study the effects
of additives on frac ture patterns using
conventional techniques. Despite large number
of research papers it is not clearly understood
that how the additives affect the grinding. We
tried to explore some new additives which can
enter into the pre-existing cracks in the solid
particles and can widen these cracks using the
unique properties of these additives. These
phenomena can be related with artificial
weathering phenomena of rocks (Faria and
Bieniawski 1984). The five additives (Expansive
Solids, Disintegrators, Sublime Solids, Acicular
Particles, and Swelling Solids) were selected
from literature survey and experiments were
carried out using laboratory scale ball mill and
effect on size reduction is studied. Their effect
on pre-existing cracks and particles surfaces
were studies using SEM and QEMSCAN
mineralogy analyzer.
2. Experimental work
Dry grinding is again getting popularity due to
water crises and environmental concerns. But
effective of additives on dry grinding is not
explored fully. Present study is carried out to
know effect of additives on dry grinding. These
Figure 1 : Micro-cracks in the broken manganese ore particles (a) Visible cracks in bigger
particles (b) Pores and Cracks in coagulated ore particles (c) Microcraks in small particles
68
MPT-2013
additives either use the moisture present in the
cracks and microspores on the material surfaces
or it erode the particle surfaces due to nature of
additive. Five different additives were tested
with three different quantities. Usually, dry
grinding additive dosages are kept less than one
percentage but in current test work we kept
the dosage slightly higher for easy estimation
of the effect using SEM and mineralogical
analysis. Details of these additives are described
in next section.
Manganese ores found in Joda region, India
were selected and collected for the studies. These
ores mainly c ontain pyrolusite, quartz,
hematite and kaolinite as main mineral phases.
Initial size reduction by roll crusher upto <1mm
generate significant amount of cracks on particle
surface and lower brittleness of ores help to
carry many fractured particles for next stage
experimentation as shown in Figure 1. Two kg
of sample was grounded in a laboratory scale
ball mill (Length: 0.56mm Diameter: 0.5m, No.
of lifter: 2) for 30 minutes with 6kg balls of 30mm
diameter.
a) Expansion additives: Expansion additives
are powdery materials that expand
considerably when mixed with water through
chemical hydration, by the formation and
development of ettringite crystals (Taylor,
1997). Under confinement, this expansion can

generate significant expansive pressure, which
causes cracking of rock or concrete, when it
exceeds the tensile capacity of materials.
Objective of our study to use utilize these
additive to widen the pre-existing cracks in the
material and help in size reduc tion. In
experimental work we added 3, 5 and 7% Split-
AG (SG) (D80 :50mm) in the manganese ore and
carried out the grinding experiments.
b) Super disintegrators: Disintegrates are
substances or mixture of substances added the
drug formulation that facilitates the breakup
or disintegration of tablet or capsule content
into smaller particles. Recently new materials
termed as superdisintegrant have been
developed to improve the disintegration
processes. These  additives  mainly  work  on
Capillary action, swelling properties and
chemical reactions of chemicals (Paramasivam
and Vedaraman 1992b). In current study we
used the Agar Powder (AP) as an additive for
grinding. Agar is the dried gelatinous substance
obtained from Gelidium Amansi. Ito et al
investigated the use of agar powder as a
disintegrating agent for the development of
rapidly disintegrating oral tablets. Agar was
chosen because it absorbs water and swells
significantly but do not become gelatinous in
water at physiological temperature (Taylor,
1997). Current  research  work  explored  the
possibilities of these additives to reach in cracks
and support the fragmentation process during
grinding process.
c) Sublime solids: substance directly from
the solid phase to the gas phase without
passing through an intermediate liquid phase.
Sublimation is an endothermic phase transition
that occurs at temperatures and pressures
below a substance’s triple point in its phase
diagram. Naphthalene (NP, C10H8, Crystalline)
is commonly available solid and used in this
69
MPT-2013
study for experimentation. Three different
dosages of these powders were added during
grinding to support the grinding process. The
D80 of the particles was 38 micron.
d) Acicular particles: Autogenous grinding
got much popularity in last few decades. These
additives are selected to explore the same
concept for using acicular particle solids to
assist the grinding process. CaSiO 3 (CS,
Hardness: 4-5) is a commonly available solid
with acicular particles with D80:50mm. During
crushing, wollastonite breaks into lath-or
needle-shaped (acicular) particles because of its
unique cleavage properties. It is used as an anti-
caking agent in food preparation and an
antac id. It absorbs water and makes the
material free flowing. Three different dosage of
the material is tested for grinding additive.
e) Swelling solids: Various solids have a
strong ability to absorb the water and swell
quickly. Alginic acid (AlA, (C6H8O6)n, Density:
1.60 g/c m³; pH :2-3) is a c ommon
superdintegrator and we tested it in the current
study. The swelling can impart the pressure on
the cracks and can help in sizing process. It is
capable of absorbing 200-300 times its own
weight in water (Ito and Sugihara 1996). Three
different quantities of the additive were tested
for grinding applications. The D80 of the particles
was 38 micron.
3. Results and discussion
Five different additives were ground in the ball
mill. The product achieved after ball milling
was screened at different sizes and plotted
using Gaudin-Schumann Plots. These plots are
presented in Figure 2. These plots indicate that
cumulative passed material using different
additives shown increasing trend but the
pattern was different for different additives.
Split AG did not shown any significant
 MPT-2013

difference for 3% addition of additive but it was Table-2: Estimated particle sizes using Rosin-
similar for 5 and 7% and both were significantly Rambler distribution
different from the head sample. There was
almost 10% reduction in 100 micron size Additive C1 T1 (3%) C2 T2 C3 T3
(5%) (7%)
particles. The disintegrator did not shown any D36.8 213 209 208 181 203 177
SG D50 143 169 129 113 117 111
significant effect and rise in fine particles were D80 32 38 29 25 26 25
D36.8 212 221 206 219 201 219
uniform with increased additive dose and it NP D50 133 163 116 124 101 101
was between 3 to 5% weight rise in 100 micron D80 30 36 26 28 23 23
D36.8 212 211 206 217 200 212
partic les. Sublime additive shown very AP D50 125 175 106 212 90 111
D80 28 39 24 47 20 25
interesting result and rise in fines were uniform D36.8 213 198 208 228 208 189

and signific ant. It was inc reasing with CS D50

D80
143
32
192
43
129
29
117
26
129
29
89
20
increased additive does. There was 5 to 10 % D36.8 212 202 206 189 200 150
AIA D50 125 139 106 108 90 116
reduction in 100 micron size particles. Calcium D80 28 31 24 24 20 26

silicate has acicular particles but abrasive effect

of this material was not visible up to 5% doses.
It shows that there was notable difference in
fine generation when additive dose was 7%. The
swelling solid shows that fines generated
increased but this effect was not uniform for all
the sizes but particles more than 100 micron
did not get affected by this and weight of these
fractions remain same for all the additive doses.
Figure 2 show that some of the additives show
the significantly different size distribution
whereas some show only marginal change. This
difference was studied using Rosin-Rammler
distribution plots. Values of D 36.8, D50 and D80
were estimated and compared with composite
head sample size distribution. Table 2 shows
the values of different D 36.8, D50 and D80 for
different products. Analysis of this data
indicates that there are two main factors which
reduce the D 36.8, D50 and D80 particles sizes values.
The additives are fine and increase the finer
fraction without affecting the grinding and this
trend increase with increased doses. This
problem was addressed by calculating the
composite size distribution after adding the
additive and it was compared with product size
distribution.
Analysis of the data given in table 2 reveals
that there were two kinds of trends can be
observed. Dp < Dc indicates increased coarser
fraction whereas Dc >Dp indicates increased
finer fraction. In case of use of SG additive, it
was found that initially there was increase in
coarser fraction and it was mainly due to slight
agglomeration of fine particles of additive and
ore particles. This can be seen that D80 and D50
shown reducing trend which mainly due to
lower agglomeration. It shows that significant
variation in particle diameter was seen for 5%
dosages and it did not vary significantly for
increased dosage.
Agar is organic material and during milling its
behaviour is expec ted to be as a super
disintegrator using the inherent moisture. It is
hydrophilic and it also creates the jelly particle
surfaces which work as a glue and increase the
material coarseness rather than fineness. This
phenomenon is not expec ted at room
temperature but during grinding a lot of heat
is generated and it might cause agar to behave
in this way. This c an be explored as an
antidusting additive to reduce fine generation
during milling.

70

Naphthalene is an organic sublime solid and
during milling its particles behave complexly.
Some of particles convert into very fine powered
and coat the particles. It was the main reason
that with all the three dosage levels the product
is coarser than the feed. It indicates that its effect
on grinding is not effective for size reduction.
But the coating phenomena can be used to
minimize the fine generation during milling of
materials.
Calcium silicate has acicular particles and
should has generated autogenous type of
milling characteristics. It was found that
initially coarser fraction of material get reduced
due to lower dosage and finer frac tion
increased. This phenomenon was observed with
increased dosage and found that for 7% dosage
there was a significant difference in material
size distribution and fines were more than the
head sample for all the measures.
Alginic ac id (AlA) is known as a
superdintegrator and swells with moisture
content. It was seen that for all three dosage (3,
5 and 7%) coarse material reduced significantly
and has an increasing trend. But for finer
fraction this effect was not very significant. It
might be due to fracture pattern in the particles.
Bigger particles carry cracks and moisture
which help in size reduction but in fines it was
not having this support to affect the grinding.
It was found in comparative analysis that most
of the organic additives (AP & NP) create glue
effect on the particle surface during dry grinding
and its effect on size reduction cannot be
quantified. Bec ause finer partic les get
agglomerated and D50 or D80 shown higher
values than the feed composite sample. It was
found that AlA, CS and SG shown some ray of
hope for additive development. Their effects
were much significant on coarser sizes (D36.8)
than the finer sizes (D80). Their performance can
be sequentially arranged in following manner:
Effect on D36.8: AIA > SG >CS
Effect on D80: SG >CS > AIA
71
MPT-2013
Micorscopic studies were carried out to study
the effect of these additives on particles surface
and fractures. The mean particle sizes of
additives were <38micron. It was observed in
microscopic analysis of ground product that
during milling the harder additives (SG, CS and
AP) did not get fully grounded and some
particles of these additives were seen in the
product. Uncrushed coarese particles of softer
additives (NP and AlA) were not seen in the
products. Micrographs are shown in Figure 2.
Figure 2 indicate that there is difference in
particle brightness in all the samples and it was
mainly due to slight coating of different
additives on particles surfaces. It was expacted
that these additives will approach the pore and
fractures on particles surfaces. This phenomena
was checked using QEMSCAN and SEM-
element mapping technque at addiferent pore
and fractures on particle surface and shown in
Figures 4 & 5.
QEMSCAN provided automated mineralogical
analysis of ore samples using a Scanning
Elec tron Mic roscopy and spec ified
mineralogic al database. A sample was
prepared using the product obtained by
grinding of ore with calcium silicate (CS). The
frame captured using QEMSCAN is presented
in Figure 4. The mineral list attached was
modified to see the distribution of Ca and Si
bearing materials and new minerals (Mn
Others) was added in it. It shows that most of
the particles have coating of this material as
well as it was finally distributed in the sample.
Comparison of head sample particle view and
product ground using additive shown that
particles grounded using additives were having
small particles adhering to the surface of big
particles. It was distributed on open pores and
grain boundaries. It indicates that there is a
 MPT-2013

Figure 2 : Size distribution of products using different grinding additives

Figure 3: Microscopic analysis of products using

different additives

Figure 4 : QEMSCAN analysis of Additive Figure 5: Elemental distribution on grinding

grinding product products using additives

72

probability that the additive was able to
produce the erosion effect.
Elements which were considered as a prime
part of material compsition were selected for
mappling. Ca, O, C, Si and C are the majour
elemnts found in SG, AP,NP,CS and AlA,
respectively. Figure 5.a indicate that Ca is
distributed on the particles surface but it is not
c onc entrated in the frac ture but O
concentration was observed in this crack. This
might be due to widgth of crack which less than
5micron. Agar powder contain a chain of O
and OH moluecular and it was observed that
distribution of oxygen was thicker in the cracks.
It indicate presence of additive in the cracks.
Naphthalene is an organic sublime solid and it
was found that concentration of C was higher
in the pores which were not very useful for size
reduction. Figure 5.d also indicates a uniform
distribution of Ca and Si in the materials and
particle surfaces. Allergenic acid is also a
hydrocarbon and carbon distribution was
observed on particles surfaces.
4. Conclusion
Identifying the additives for dry grinding is a
challenging subject and its importance will
increase in coming years due to water scarcity.
There are various possible mechanism by
which the dry grinding additives can improve
the milling performance but success of these
additives depend on material characteristics,
additives properties and their interaction.
(a) Five different types of materials were
tested and found that a lime based
expansive material (SG) is most effective
dry grinding additive and it is able to
reduce coarser fraction (>150microns) by
5% using the 5% additive dosages. It
reduced the D36.8 particle diameter by 27
micron.
(b) The organic additive Naphthalene and
Agar powder were not found suitable and
73
MPT-2013
these were creating glue effect on particle
surfaces which were adversely affecting
the size reduction as well measurement
process.
(c) Algenic acid and Calcisum silicate shown
positive effec t on size reduction and
reduced the coarser fraction (>150microns)
by 2 to 5%. D36.8 particle diameters were
reduced by 50 and 19 micron for Algenic
Acid and Calcisum Silicate, respectively.
(d) QEMSCAN and SEM element mapping
techniques is very useful tool to measure
the effect of additives on the dry grinding
process.
References
Daniel, M., 2006. Energy efficient mineral
liberation using HPGR technology. AMIRA
P9N Project, Review, 15th Nov [9].
El-Shall, H., 1984. Physico-Chemical aspects of
grinding: a review of use of additives.
Powder Technology, 38, 275 - 293.
Faria ,Santos, Bieniawski, C.A.F., 1984. Effect of
artificial weathering on properties of
LOYALHANNA Sandstone, Proceedings
of the 27th US Symposium on Rock
Mechanics, 1984, Tuscaloosa, AL, USA.
Fuerstenau, D.W., 1995. Grinding Aids. KONA,
13, 5-17.
Gaete-Garreton, L.F., Vargas-Hermandez, Y.P.,
Velasquez-Lambert, C., 2000.
Applic ation of ultrasound in
comminution. Ultrasonics, 38, (1-8), 345-
52.
Gock , E., Kurrer, K.E., 1998. Increased efficiency
of the vibratory milling process with the
eccentric vibratory mill. Aufbereitungs-
Technik, 39 (3), 103–111.
Hasegawa, M., Kimata, M., Yaguchi, M., 2006.
Effect and behavior of liquid additive
molecules in dry ultrafine grinding of
limestone, KONA, (24).

Ito ,A., Sugihara, M., 1996. Chem. Pharm. Bull.
44(11), 2132 – 2136.
Klimpelm, R.R., Austin, L.G., 1982. Chemical
additives for wet grinding of minerals,
Powder Technology, 31, 2, 239–253.
Kumar, P., Sahoo, B.K., De, S., Kar, D.D.,
Chakraborty, S., Meikap, B.C., 2010. Iron
ore grindability improvement by
microwave pre-treatment, J. of Industrial
and Eng. Chemistry. 16 (5), 805-812.
Mangal, M., Thakral, S., Goswami, M., Ghai, P.,
2012. Superdisintegrants: An Updated
Review, Inter. Journal of Pharmacy and
Pharmaceutical Science Research. 2(2) 26-
35.
Marmor, F., 1993. Energy-saving fine-grinding
using the Sala-Agitated-Mill SAM.
Aufbereitungs-Technik, 34(10), 506-511.
Paramasivam, R., Vedaraman, R., 1992a. Effects
of the physical properties of liquid
additives on dry grinding. Powder
Technology. 70 (1). 43-50.
Paramasivam,R., Vedaraman, R., 1992b. Studies
in additive grinding of minerals.
Advanced Powder Technology.3(1),31-37.
*******
74
MPT-2013
Rose, H., Sullivan, R., Bail, 1958. lkbe and Rod
Milk. Chemical Publishing Co., New York,
236 - 251.
Singh, V., Tathavadkar, V., Denys , M. B.,
Venugopal, R., 2012. Application of
quartz inversion phenomenon in mineral
processing – A case study of siliceous
manganese ores. Mineral Engineering,
32, 8-11.
Somasundaran, P., Lin, I. J., 1972. I and EC
Processes Des. Dev. 11, 321.
Taylor, H.F.W., 1997. Cement Chemistry, 2nd ed.,
Thomas Telford, London. 313-316.
Thaler, H., 2000. Ultrafine jet mill grinding.
Industrial Mineral. 389, 39-45.
Wang, E., Shi F., Manlapig, E., 2011. Pre-
weakening of mineral ores by high
voltage pulses. Mineral Engineering. 24
(5), 455-462.
Wang ,D., Wang, Z., 2009. Research and
Application of Func tional Polymer
Grinding Aids. Materials Science &
Tec hnology 2009 Conferenc e and
Exhibition. 1974-1983.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Mass Balance Studies on the Grinding-Classification Circuit of

H.Z.L’s Rampura Agucha Mines
Jayseh B. Gakare, T. S. Anil Kumar Nistala, Ajit Swain and Dr. K. D. Sharma*
Central Research and Development Laboratory, Hindustan Zinc Ltd, Udaipur 313024,
Rajasthan, India
Abstract
The performances of the size reduction and classification operations of a mineral beneficiation
circuit are a pinion duo for the excellent performance of succeeding beneficiation operation. Unless
the feed to the beneficiation operation is of a desired optimum size distribution the optimum
grade and recovery is not possible. Therefore, regular auditing of the circuit is must to realize and
sustain the performance of the circuit. Usually the auditing includes the mass balance of the
circuit.
The mass balance can be done on the size data obtained from sieving the samples collected during
the circuit audit. Thus using any mathematical tool (like Microsoft Excel), one can estimate an
approximate tonnages in the operating circuit. But, in order to know the accurate and more
reliable data regarding the circuit instantly, JK SimMet (version 5.2) software is used.
Out of all the circuit audits we conducted, we had selected a case in which the importance of the
regular circuit auditing was revealed. This paper reveals the facts regarding the circuit during the
sampling period.

Keywords: Modeling; simulation; grinding; classification

1. Introduction
The grinding in any mineral beneficiation
plants, in most of the cases doesn’t get paid of
full attention. But, this grinding is the very
energy ineffic ient and very c ruc ial unit
operation on which the performance of the
mineral beneficiation plant depends for the
successful metallurgy achievement. Also the
grinding is the last stage of the size reduction
operation.
The reason behind for attaining the optimum
mesh of grind (MOG) for the particular ore is
nothing but getting the required degree of
* Correspending Author: : Dr. K. D. Sharma, Head-C.R.D.L,
Central R&D Laboratory, Hindustan Zinc Ltd, Udaipur
313024, Rajasthan, India. E-mail: kd.sharma@vedanta.co.in
liberation of the valuable minerals. If the
grinding circuits are not performing well the
product may become coarser or finer than the
required MOG. This will result in the loss in
recovery of the valuable minerals due to poor
liberation in case of the coarser product. While
in case of the finer product, again the loss in the
recovery may be due to excess fineness of the
product which may be unrecoverable within
the limitations of the succeeding mineral
beneficiation process (i.e., fixed residence time).
Also, these two cases will also cause problems
in the subsequent downstream unit processing
sections (i.e., smelting, leaching, roasting). An
extra 19% of the power is required to grind the
ore one screen finer than that of the regular

75
 MPT-2013

MOG. So, the grinding is the most surveillance

required area, as it is a very energy consuming
operation. (Napier Munn, T.J (1996)).
The importanc e of the hawk eying the
performance of the classification circuit is next
to the grinding operation. If the performance of
classification circuit is not up to the mark, the
material which must report to the stream for
the subsequent mineral beneficiation process
may get recycled back to the grinding section
or the material whic h is supposed to be
Figure 1: The flow diagram of grinding and
reported to the recycling stream may report to
classification circuit of the stream I
the subsequent mineral benefic iation
operation. Either the cases will cause the loss in
the recovery of the valuable minerals which
will also make the grinding operation inefficient.
This will cost same as that of the inefficient
grinding circuit.
So the importance of the regular auditing and
optimizing the size reduction and classification
circuits is pinion of the mineral beneficiation
plant to excel. This discussion is over the case
study on one of our mineral beneficiation Figure 2: The flow diagram of grinding and
circuits of HZL. classification circuit of the stream II, III & IV
The mineral beneficiation plant of Rampura The sampling points in the circuit during the
Agucha Mines, HZL has a capacity of 6 million sampling campaign were as the following:
tons per annum with four streams each having 1. Rod & Sag mill Feed & discharge
different capacities. Stream I has a capacity of 2 2. Single deck screen at sag mill discharge
million tons per annum, Stream II has a capacity over size (only in stream 2, 3 & 4).
of 1.5 million tons per annum, Stream III has a 3. Ball mill discharge
capacity of the 1 million ton per annum & 4. Primary cyclone Feed, O/F & U/F
Stream IV with a capacity of again 1.5 million 5. Secondary Cyclone Feed, O/F & O/F
tons per annum. The stream I is only having a The samples were collected over a sampling
rod - ball mill grinding combination while all period of 3 hours with a cut at every 30 minutes.
the other are sag- ball mill combinations. All The operating conditions of the grinding circuit
the circuits are having two stage classifications were maintained constant over the sampling
(hydro cyclone) which will operate in closed period.
circuit conditions with the ball mill. The operating parameters’ data was noted at
the end of the sampling period from the DCS.
2. Sampling Campaign on the Circuits
The flow diagrams of all the streams are as The samples thus collected were then used for
follows. the pulp density calculations by drying them.
The dried samples were then taken for the size
analysis (wet sieving). The above contains the
experimental sizing data of all the four circuits

76

Table 1: Experimental Sizing data of samples
collected from stream I
Table 2: Experimental Sizing data of samples
collected from stream II
Table 3: Experimental Sizing data of samples
collected from stream III
77
MPT-2013
Table 4: Experimental Sizing data of samples
collected from stream IV
3. Mass Balance Studies
The data collected from the DCS, sizing data &
pulp density data were used in conducting the
mass balance studies with the software JK
SimMet. The software performs the mass
balance calculations with the reconciled data
(which is done by the software itself).
The mass balance results were obtained as
follows.
Table 5: The mass balance results for stream I
 MPT-2013

Table 6: The mass balance results for stream II

100
90
80

Cu m % p a sin g
70
60
50
40
30
20
10
0
0.001 0.010 0.100 1.000 10.000 100.000
Size (mm)
1:Autogenous Mill 3 Combiner, Bal 2:Autogenous Mill 3 Prod, Bal
3:Ball Mill 4 Combiner, Bal 4:Ball Mill 4 Prod, Bal
5:Single Deck Screen 5 O/S, Bal 6:Single Deck Screen 5 U/S, Bal
7:Hy drocy clone 6 U/F, Bal 8:Hy drocy clone 6 O/F, Bal
9:Hy drocy clone 7 U/F, Bal 10:Hy drocy clone 7 O/F, Bal
11:Feed 1 Combiner, Bal

Fig.4: The balanced sizing data for stream II

S izin g
100
Table 7: The mass balance results for stream III 90
80

Cum% p assing
70
60
50
40
30
20
10
0
0.001 0.010 0.100 1.000 10.000 100.000
Size (mm)
1:Feeder Combiner, Bal 2:SAG Mill Prod, Bal
3:Single Deck Screen O/S, Bal 4:Single Deck Screen U/S, Bal
5:Ball Mill Combiner, Bal 6:Ball Mill Prod, Bal
7:2nd stage cy clone U/F, Bal 8:2nd stage cy clone O/F, Bal
9:Ist stage cy clone O/F, Bal 10:Ist stage cy clone U/F, Bal

Fig.5: The balanced sizing data for stream III

S izin g
Table 8: The mass balance results for stream IV 100
90
80
Cum % passing

70
60
50
40
30
20
10
0
0. 01 0.10 1. 00 10.00 100.00 1000.00
S ize (mm)
1: Feed Combiner, Bal 2:SAG Mill Prod, Bal
3: Single Deck Screen O/ S, Bal 4:Single Deck Screen U/S, Bal
5: Ball Mill Combiner, Bal 6:Ball Mill Prod, Bal
7: 2nd st age cy clone U/F, Bal 8:2nd stage cy clone O/F, Bal
9: Ist stage cy clone U/F, Bal 10: Ist stage cy clone O/F, Bal

Fig. 6: The balanced sizing data for stream IV

S izin g 4. The Observations
100
90
80
The key observations that were found from the
Cum % passing

70
60
50
mass balance studies are as follows stream wise.
40
30
4.1 Stream I
20
10
0
 Reduction ratio for Rod mill is observed as
0.001 0.010 0.100 1.000
S ize (mm)
10.000 100.000
6 and for Ball Mill as 5
1:Rod Mill C ombiner, Bal 2: Rod Mill Prod, Bal
3:Ball Mill Prod, Bal
5:2nd stage cy clone O/F , Bal
7:Ist stage cy clone O/ F, Bal
4: 2nd stage cy clone U/F, Bal
6: Ist stage cy clone U/F, Bal  307% Recirculation load is observed at BM,
which is equivalent to 295 T/Hr for 96Ton of
Figure 3: The balanced sizing data for stream I fresh feed. Almost 29% of Feed to BM (86
Tons) is having size less than 75 micron &
18.5% having size less than 37microns.
Mineralogical study could indicate if these
fines contain important metallic minerals

78

in locked form or liberated forms which are
further ground in BM.
 Percentage of Feed water reporting to
primary cyclone cycle under flow is 18%
with particles having size 20% less than 75
microns.
 Similarly percentage of Feed water reporting
to secondary cyclone under flow is 31%, which
is reasonable. This contains particles having
a size of 38% less than 75 micron).
 Scope exists to alter prim. Cyclone cut-size
little coarser. Approximately 20 m3 of water
was getting added in Ball & Rod mill
discharge as unaccounted water.
4.2 Stream II
 Reduction ratio for Sag mill is observed as
103.15 and for Ball Mill as 2.2. 238%
Recirculation load is observed at BM, which
is equivalent to 489 T/Hr for 205Ton of fresh
feed. Almost 23.1% of Feed to BM (116.5
Tons) is having size less than 63 micron &
15.2% (74.3 Tons) having size less than
37microns. Mineralogic al study c ould
indicate if these fines contain important
metallic minerals in locked form or liberated
form which is further ground in BM.
 Out of this <63 micron size tonnage, 65.2tons
are contributed by primary cyclone U/F and
47.83 tons are contributed by sec cyclone U/F.
 Percentage of Feed water reporting to
primary cyclone cycle under flow is 21.7%
with particles having size 21.65% less than
63 microns.
 Similarly perc entage of Feed water
reporting to secondary cyclone under flow
is 10.23%, which is reasonable. These contain
particles having a size of 25.54% less than
63 micron.
 About 10% of the <8mm size particles are
reporting to the under flow of the sag mill
screen.
79
MPT-2013
4.2 Stream III
 Reduction ratio for Sag mill is observed as
214 and for Ball Mill as 1.39.
 415% Recirculation load is observed at BM,
which is equivalent to 623 T/Hr for 150Ton
of fresh feed. Almost 32% of Feed to BM (199
Tons) is having size less than 63 micron
 Out of this <63 micron size tonnage, 87 tons
are contributed by primary cyclone U/F and
111 tons are contributed by sec cyclone U/F.
 Percentage of Feed water reporting to
primary cyclone cycle under flow is 26%
with particles having size 29% less than 63
microns.
 Similarly perc entage of Feed water
reporting to secondary cyclone under flow
is 34%, which is reasonable. This contains
particles having a size of 34% less than 63
micron. Fine size distribution for primary
cyclone feed was observed in case of Sag
mill/Ball mill combination in compare to
Rod mill/Ball mill.
4.3 Stream IV
 Reduction ratio for Sag mill is observed as
277 and for Ball Mill as 1.81.
 277% Recirculation load is observed at BM,
which is equivalent to 601 T/Hr for 220 Ton
of fresh feed.
 Almost 27% of Feed to BM (162 Tons) is
having size less than 63 micron
 Out of this <63 micron size tonnage, 120 tons
are contributed by primary cyclone U/F and
41 tons are contributed by sec cyclone U/F.
 Percentage of Feed water reporting to
primary cyclone cycle under flow is 33%
with particles having size 26% less than 63
microns.
 Similarly perc entage of Feed water
reporting to secondary cyclone under flow
is 12%, which is reasonable. These contain
particles having a size of 29% less than 63
micron.

5. Conclusions
The conclusions made from the observations
observed and the mass balance data is as
follows:
5.1 Stream I
 Feed to flotation contains a particle size p80=
65 micron.
 P80 size for RM discharge is 2.26mm,
whereas that for BM discharge is 0.173 mm.
 About 29% -75 micron fines is recycling back
to BM for grinding; (mineralogy study is
necessary to know how galena and softer
gangue are distributed in the fraction).
 Data around primary & secondary cyclone
are to be used to establishing cyclone
efficiency curve
Similar sampling and mass-balance on a few
more occasions is necessary for verification.
Simulations with a representative model for
the circuit based on accurate data will provide
useful clues for a better optimized circuit.
5.2 Stream II
 Feed to flotation contains a particle size p80=
77 micron which is relatively coarser when
compared to that of the stream I all circuits
subjected to change in the ore.
 P80 size for SAG discharge is 1.013mm,
whereas that for BM discharge is 0.155 mm.
 About 23.1% -63 micron fines is recycling
back to BM for grinding; (mineralogy study
is necessary to know how galena and softer
gangue are distributed in the fraction).
5.3 Stream III
 Feed to flotation contains a particle size p80=
78 micron which is relatively coarser when
compared to that of the stream I all circuits
subjected to change in the ore.
 P80 size for SAG discharge is 0.414mm,
whereas that for BM discharge is 0.132 mm.
 Efficiency of both cyclones was observed to
be reasonable in terms of water reporting
*******
80
MPT-2013
to U/F (Fines reporting to U/F), where poor
effic ienc y was observed in terms of
sharpness of separation.
 High rec irc ulation load (415%) was
observed, in spite of low P80 of cyclone feed
stream, indic ating the sc ope for
improvement in the cyclones.
5.4 Stream IV
 Feed to flotation contains a particle size p80=
76 micron which is relatively coarser when
compared to that of the stream I all circuits
subjected to change in the ore.
 P80 size for SAG discharge is 0.494mm,
whereas that for BM discharge is 0.159 mm.
 Efficiency of both cyclones was observed to
be reasonable in terms of water reporting
to U/F (Fines reporting to U/F), where poor
effic ienc y was observed in terms of
sharpness of separation.
* From conclusions of all the streams mass
balanc e studies mentioned till now, the
comparison is made between all the circuits.
The comparison of the all circuits performances
is as follows:
1. Stream-I is comparatively finer between all
the streams.
2. SAG/Ball mill combination producing finer
size distribution compare to Rod/Ball mill
combination.
3. Hydro cyclone performance of stream-I is
better when compared to other three
streams.
Acknowledgment
The authors are grateful to the management of
the HZL - Rampura Agucha Mine’s beneficiation
plant for supporting the sampling campaign
by providing all the facilities required for the
sampling.
References
Napier-munn, T.J., Morrell, S., Morrison, R.D.
and Kojovic, T. 1996. Mineral comminution
circuits: their operation and optimization.
JKMRC, pp. 413.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Improving Reliability of Screens in Closed Circuit Crushing of

Coal

ParthaDas, Naveen Kumar and PallavGarg*

TATA STEEL, Jamadoba Coal Preparation Plant, Dhanbad, 828112, Jharkhand, India
Abstract
Industrial screening is extensively used in coal preparation plants to obtain the desired size of
coal which ultimately affects the quality of the end product. Performance and availability of
screens become very important factors on industrial scale for efficient running of the plant. This
work was carried out in the coal handling section of the Jamadoba Coal Preparation Plant of Tata
Steel. This section has two screens in closed circuit with an impact crusher. The section is extremely
critical for plant operation because of it being online with the main process plant. The screens
have woven wire surfaces of aperture 16x20 mm. The screens posed frequent problems of clogging
and wire breakage due to which it required frequent maintenance and feed size to the main
process plant was significantly affected. Dismantling and fitting of the screen surface required
ample amount of time and manpower. An attempt was made to improve the circuit by replacing
one of the screen surfaces with polyurethane panel. The performance of the two different types of
screens at different operating conditions was studied. Various operational parameters like feed
rate, raw coal size distribution and feed moisture were considered and the performance of the
screens was analysed. Wear life, Ease of maintenance, Safety and clogging tendencies were also
considered for comparison of both the screen surfaces. It was found that polyurethane panels
excelled in most of the parameters especially clogging frequency and ease of maintenance though
feed rate and open area were a matter of concern.
Keywords: Screening; coal; woven wire; polyurethane

1. Introduction equipment are available for coal sizing out of

Sizing of coal particles is one of the most
significant operations in coal beneficiation
processes. Preparation of coal within specified
size ranges is very important as it affects the
efficiency of subsequent beneficiation processes.
Sizing is the process of separating mixed
particles of different sizes into groups in which
all particles range between certain maximum
and minimum limits. In coal preparation
plants, sizing is generally achieved by passing
coal over screens. Various types of screening
which vibrating screens are the most versatile
machines used on an industrial scale. Vibrating
Screens are applicable in various phases of coal
proc essing from scalping of raw c oal to
dewatering of extremely fine sizes. The
vibrating frequency and amplitude of the
vibrating screens are important parameters for
screen operation which significantly affect the
performance. Results have shown that High
frequency and large swing angle are suitable
for small particles, while small values are
suitable for particles closer to the aperture size

81

(Xiao and Tong 2013). The primary function of
screening is to pass the undersize particles and
reject the oversize particles. If the particles are
brought at the openings at such a velocity and
in such a direction that the passage of undersize
is not hindered, effective screening can be
achieved. If every particle of undersize could
be brought to the opening at substantially zero
velocity and in a perpendicular direction
probability of passage of particle will increase
to a large extent. But tonnage requirements and
mechanical considerations forbid this type of
particle presentation and therefore the design
of screening equipment and the type of screen
surface affect the process of industrial screening
significantly.The screening can be wet or dry
depending upon the requirements of operation.
However, results have shown that during wet
screening, the fine fraction is increased
indicating fragmentation during screening
(Govender and Van Dyk 1947). In this work,
comparison of performance of two different
sc reening surfac es with respec t to both
operation and maintenance has been done for
Jamadoba Coal Preparation Plant.
2. Area Description and Methods
2.1 Plant layout and material flowstream:
Jamadoba Coal Preparation Plant of Tata Steel
is the oldest coal washing plant of Asia.primary
source of raw coal for the plant is from the
underground collieries of Jharia Division of Tata
Steel. The raw coal received by the plant is first
fed to the rotary breaker with size of perforation
being 75 mm. Largepieces of shale and stone
are discharged from the end of the breaker and
the material that passes through the
perforations is stored in bunkers. The coal from
these bunkers is fed to a belt conveyor system
that feeds the material to two vibrating screens
through a pyjama discharge chute. The oversize
material from the screens is fed to an impact
crusher and the undersize is fed to the main
washing circuit. The crushed material is again
82
MPT-2013
fed to the screens thus completing the loop of
closed circuit crushing. The desired size of coal
fed to the main washing plant is -15mm.The
main washing plant is comprised of dense
media cyclone and froth flotation circuits for
beneficiation of coal. Figure 1 shows the
material flow diagram of coal handling section
in the plant.The circuit is very critical for plant
operation as it is online with the main washing
plant. The performance of both the screens thus
significantly affects the plant operation. The
screen surfaces of both the screens were of
woven wire type. One of the major concerns of
this section was screen downtime due to
frequent clogging of material in the woven wire
and wire breakage. Dismantling of damaged
woven wire panel and replacing it required a
lot of time and manpower. In this work, one of
the sc reen surfac es was replac ed with
polyurethane panel and c omparison of
performance of both the screens was done with
respect to different parameters.
Rotary Breaker
Shale/Stone
Raw Coal
Coal Size: -75mm
Silos
Vibrating Screen 1 Vibrating Screen 2
Oversize
Undersize
Undersize
Impact Crusher
Main Washing
Plant
Fig.1: Layout of Coal Handling Section at
Jamadoba Coal Preparation Plant
2.2. Plant sampling and methods of analysis
Individual samples of feed, oversize and
undersize were taken from both the vibrating
 MPT-2013

screens. While collecting samples from one Overall Screen Efficiency = o(f-u)(1-u)(o-f) / f(o-
screen, electrical shutdown was taken in the u)2(1-f)……. Equation (1)
other screen so that the samples were a true
3.1.2. Screening efficiency for woven wire
representative of individual sc reen
surface
performance. A number of samples were taken
on daily basis in different shifts and A number of data sets were chosen and screen
corresponding performance of screens was efficiency was calculated based on the recovery
analysed. Efficiency of screening surfaces were of material at the cut size of 15mm. Figure 2
calculated using mass balance equations. The shows an example of size distribution curves
feed rates at the time of sampling were also noted for woven wire surface. The efficiency of screen
and important derivations were made. Open using the mass balance formulae has been
Area of both the screens was calculated and calculated.
the results obtained were compared with the
clogging tendency of screen surfaces. Time
100.00
required for maintenance of screens was also g
n
sis 90.00
Feed
taken into accord. a
p 80.00
t
n 70.00
ce
r
3. Results and Discussion e 60.00
p Screen
t 50.00
h Overflow
ig
3.1. Screening efficiency e 40.00
w
e
ivt 30.00
3.1.1. Mathematical expression for efficiency al 20.00
u
Screen
Underflow
m 10.00
calculation u
C
0.00

Let F be the tonnage of feed over screen, O be 0.5mm 1 mm 3mm 6 mm 10 mm 13 mm 15 mm20 mm

the tonnage of screen overflow and U be
tonnage of screen underflow. If fraction of
material above cut point size in feed is f, fraction
of material above cut point size in overflow is o
and fraction of material above cut point size in
underflow is u, the overall screen efficiency can
be calculated using the concept of mass balance
(Wills, 2006).
F=O+U
Mass Balance for oversize material:
Ff=Oo + Uu
Mass balance for undersize material:
F(1-f)=O(1-o) + U(1-u)
Hence: O/F= f-u/o-u
U/F= o-f/o-u
Rec overy of oversize partic les in screen
overflow=Oo/Ff= o(f-u)/f(o-u)
Recovery of undersize material in screen
underflow = U(1-u)/F(1-f)=(1-u)(o-f)/(1-f)(o-u)
Overall effic ienc y c an be c alc ulated by
multiplying the above equations.
Size
Fig. 2: Size distribution curve of feed, overflow
and underflow of screen with woven wire
surface
Screen Efficiency for woven wire surface :-
Fraction of material above 15mm in feed (f) =
38.54
Fraction of material above 15 mm in overflow
(o) = 76.47
Fraction of material above 15 mm in underflow
(u) = 1.38
Using Equation 1 for calculation of Screening
Efficiency
Overall Screen Efficiency = 0.795
3.1.3. Screen efficiency for polyurethane
surface
Figure 3 shows an example of size distribution
curves of feed, overflow and underflow from
polyurethane screen surface

83
 MPT-2013

13 0
12 5
12 0
100.00
11 5
90.00
Polyure th an e
te11 0
g80.00 a
R10 5 Su rfac e
n
sis d
e
a70.00 e
F10 0
W ove n w ire
p Su rfac e
t 60.00
n 95
e
cr Fe e d
e50.00 90
p Scre e n O ver flow
t 40.00 85
h
ig Scre e n Unde rflow
e30.00 80
w
ve 20.00 1 2 3 4 5 6 7 8 9 10 11 1 2 1 3 1 4 1 5
it
la10.00
u
m 0.00
u
C Average feed rate achieved from woven wire
Size surface was found to be greater than that of
polyurethane surface. Both screens add up to
Fig. 3: Size distribution curve for feed, oversize give a feed rate of over 200 tons per hour to the
and undersize of screen with polyurethane main washing plant.
surface
3.2.1. Open area calculation
Screen Efficiency for woven polyurethane
surface: Open area is expressed as the ratio of hole area
Fraction of material above 15mm in feed (f) = or area that is free for passage of material to the
39.8 total screen area. Per cent open area is a measure
Fraction of material above 15 mm in overflow to predict how readily a material will pass
(o) = 81.55 through a screen.
Fraction of material above 15 mm in underflow Open Area for Woven Wire Surface
(u) = 0.83 Size of hole =20mm x 16mm =320 mm2
Using Equation 1 for calculation of screening No. of holes in one woven wire cloth =95x75=
efficiency 7125
Overall Screen Efficiency = 0.842 Open Area= 320 x 7125 = 2280000 mm 2
A number of similar trials were done and Dimension of one woven wire cloth = 8 ft x 5 ft=
screening efficiency of polyurethane surface 40ft2= 3716121.6 mm2
excelled that of woven wire surface by 4 per Per cent open area= 2280000 x 100 /3716121.6
cent. =61.3 %
Open Area for polyurethane surface:
3.2. Comparision of feed rates
Size of hole = 18mm x 18mm = 324 mm2
Feed rate obtained from individual screens was No. of holes in one panel = 240
observed and recorded for a number of times. Open Area =240 x 324 = 77760 mm2
Care was taken that feed characteristics to both Dimension of one panel = 2ft x 1ft =2 ft2 = 185806
the screens during test runs remain same. This mm2
was done by feeding the screens from the same Per cent open area = 77760/185806= 41.8 %
storage bunkers in which coal from a particular
3.3. Comparison of clogging tendency of
sourc e was stored. Figure 4 shows the
screen surfaces
c omparison of feed rates obtained from
individual screens during various test runs. Clogging of coal particles on screen surfaces
Average feed rate for woven wire surface:110.2 during operation was one of the major concerns
Average feed rate with polyurethane for the plant. Clogging of screen surface leads
surface:96.4 to blinding of apertures due to which undersize

84
 MPT-2013

material reports to overflow. This leads to of operation. The time required for maintenance
increase in recirculating load of the closed circuit of both the screen surfaces was compared and
and drastic reduction in efficiency of screening. analysis was done. It was found that the
The quantity of fines generated in impact average life of woven wire surface was about
c rusher depends upon the size and one month whereas life of polyurethane
c harac teristic s of c oal been proc essed screening surface was near to six months.
(Eswaraiah et al. 2008).Cleaning of screen Figure 5 and 6 show the average time for
surfaces in each shift of plant operation was maintenance for woven wire surface and
scheduled and the time required for cleaning of polyurethane surface respectively.
the screen surfaces was noted for both the types
160
of screen surface. s 140
e
Table 1: Time required for cleaning of t
u 120
n
i 100
m
polyurethane screen surface f 80
o
r
e 60
b
m 40
Shift A Shift B Shift C u
N 20
Day 1 15 20 15 0
Day 2 10 15 15 Week 1 Week 2 Week 3 Week 4

Day 3 20 10 15
Day 4 10 15 10
Day 5 Scheduled Maintenance 20 25
Figure 5: Time required for maintenance of
Day 6 20 15 20 one woven wire cloth
Day 7 Scheduled Maintenance In the initial days the time required for
Table 2: Time required for cleaning of woven maintenance of woven wire surfaces was
wire screening surface mainly due to wire breakage. Wire binding took
a time of about 45 minutes. The time increased
Shift A Shift B Shift C
Day 1 35 25 30
gradually in the next few days with
Day 2 30 30 25 requirements of side and centre bolt tightening.
Day 3 35 30 25
Gradual deterioration of surface with inability
Day 4 30 25 35
Day 5 Scheduled Maintenance 35 40 to resist the vibrations and high size feed,
Day 6 35 25 30 complete replacement of the surface had to be
Day 7 Scheduled Maintenance
done which took a time of about two and a half
The clogging tendency for woven wire surface hours.
was found to be much more than polyurethane
surface. Open Area in polyurethane surface is 10 0
90
less than woven wire surface but the reduction s
te
u
80
70
n
i
in clogging tendency of material leads to more M
f
o
60
50
r
effec tive screening. Reduced equipment e
b
m
40
30
u
N 20
downtime and increased efficiency of screening 10
0
are the direct benefits of reduced clogging
tendency.
3.4. Comparison of time required for
maintenance of both the screens Figure 6: Time required for maintenance of
one polyurethane panel
The life of sc reen surfac es is of utmost Polyurethane panels required less time for
importance in industrial applications as it maintenance throughout its wear life. The
directly impacts the screen downtime and cost initial maintenance tome required was for

85

placing the panel in the desired. The time
gradually increased with panel dislocation
during operation and damage to panel surfaces.
The process continued up to six months till the
panel and rail had to be replaced completely
and it required a time of about one and half
hours. Figure 6 shows the average maintenance
time required for one polyurethane panel
throughout its wear life of about six months.
The time for maintenance directly affects the
plant availability and the coal handling section
being online with the main plant, directly affects
the throughput of the day. Many works have
been done to highlight the significance of
c ondition based maintenanc e and plant
availability in coal preparation plants (Lester
et al. 1998). Polyurethane panels being lighter
in weight and easy to fit also pose significant
advantages of safer condition to do work and
requirement of lesser manpower.
4. Conclusion
The screening efficiency of polyurethane panel
screen surface wasfound to be greater than that
of woven wire panel surface. The open area of
polyurethane surface is less but the reduced
*******
86
MPT-2013
clogging tendency in the panel leads to more
effec tive sc reening. Minimal time for
maintenance and maximum availability of
screens can be attained using polyurethane
surfaces.Reduced blinding of screen apertures
and reduced recirculating loads are definitely
the clear advantages of using a polyurethane
surface panel.
References:
Eswaraiah, C., Gupta, Anshul, Nagarajan, R.,
Rajavel, M., Nanadakumar, K., 2008,
Minimization of fines generation in size
reduction of coals by impact crusher.
Govender, A., Van Dyk, J.C., 1947. Effect of wet
screening on particle size distribution and
coal properties. South Africa.
Lester M et al., EUR, 1998, Coal Preparation
plant condition based maintenance.
Wills, Barry A, Tim Napier Munn, EUR, 2006
Mineral Proc essing Tec hnology, An
Introduction to the practical aspects of ore
treatment.
Xiao, Jianzhang, Tong, Xin, China, 2013.
Characteristics and efficiency of new
vibrating screen with a swing trace.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Optimization of Grinding Circuit in Uranium Milling Operations

S.Siddique1*, K. Srinivas and N.R. Mandre

1
Uranium Corporation of India Limited,Tummalapalle, YSR Kadapa District, Andhra
Pradesh.
2
Department of Fuel & Mineral Engineering, Indian School of Mines University, Dhanbad,
Jharkhand.

Abstract
Grinding is most cost & energy intensive in entire milling operations and optimization of grinding
circuit is important. Along with energy optimization and smooth operations, product quality
control is a critical requirement for downstream leaching operations. One of the most important
product quality parameters is particle size. In general particle size is analyzed in the laboratory
by collecting periodic samples and results are used for any corrective action. Irregularity in
sampling and delays in analysis coupled with inherent human errors in collecting representative
samples make quality control a challenging task. With the development of new online analyzers
and control instruments has made easy in operation and control of grinding circuit. This paper
deals with the control philosophy and instrumentation used for optimization of grinding circuit.

1. Introduction In any concentrator, grinding is one of the most

The over increasing demand for improved
productivity, and a constant high product
quality have accelerated the growth of control
systems in mineral processing plants. The
development of necessary instruments,
increased availability of fast computing systems
and better understanding of the process through
studies on the modeling of unit operations have
all contributed towards the advances made in
the last dec ade, in automatic c ontrol of
concentrators. Crushing, Grinding, Dewatering,
Leaching, and Filtration circuits were the main
targets for control in mineral processing plants.
Economic gains ac hieved as a result are
significant resulting in increases in productions
and minimizing the operating crew.
* Correspending Author:siddique_4@yahoo.com
important unit, operations both from
processing and economic point of view. This is
bec ause, it is during this operation that
adequate liberation is to be achieved for
subsequent processing such as floatation and
leaching. Also, the energy requirements and
operating costs of grinding circuits are the
highest averaging as much as 30-40% of the total
plant expenditure. It thus becomes obvious why
grinding circuit control has attracted so much
attention. For effective control of grinding
circuits, the objectives of which differ from
concentrator to concentrator, the primary
considerations are.
 Identification of the variables which disturb
the proc ess and those whic h may be
controlled to maintain the process at the
desired state.

87

 Means for measurement of the controllable
variables and the process response.
 The direction of change to be implemented
on the controllable variables and the
methodology to translate the control action
to the system that is development of control
strategy and implementation of control.
2. Control Objectives
The objectives of all control strategies are
directed towards economic optimisation of the
whole system and not for the individual circuit
only. Typical objectives for grinding circuit
control are:
(i) Maintaining a constant grind at constant
feed rate.
(ii) Maintaining a constant grind at maximum
possible tonnage.
(iii) Maintaining a constant grind and density
of the product at maximum tonnage.
For any specific concentrator, the objectives of
the grinding circuit control are to be considered
in the context of the local conditions and
physical limitations of the circuit. These
objec tives might c hange with c hanged
production requirements of the mill or due to
constraints from mine/smelter production
schedules and capacities.
For example at UCIL Tummalapalle mill, the
grinding size required is
-65+100# 3.2%; -100+200 # 11.30%; -200+325 #
14.7%; -325 # 70.80%.
Also it must be pointed out here when there
are more than one constraint in the objectives,
and the circuits is operating at the peak
capacity; in the event of a major disturbance to
the circuit, one constraint must be relaxed to
achieve the other. For example, when the
grinding circuit is operating at its full capacity
and the ore bec omes harder, the same
maximum through put cannot be maintained
without sacrificing the requirement in the
grind.
88
MPT-2013
3. Controlled and Manipulated Variables in the
Grinding Circuit
Control of a grinding circuit is relatively
simplified because of the fact that there are only
two important variables, namely.
a) The feed rate of the ore to the circuit and
b) The rate of addition of water to the circuit.
Which are controlled to achieve the desired
objectives. The circuit is however subject to
common disturbances such as:
a) Changes in the Ore characteristics, such
as hardness, specific gravity and size
distribution
b) Uncontrolled water additions to the
c irc uit, suc h as floor waste water
intermittently pumped into the circuit,
c) Change in quality/ quantity of the grinding
media
d) Changes in the characteristics of the feed
pulp to cyclones caused by aeration,
surging of pump etc.
e) changes in the performances of the mill
classifier circuit due to wear and tear of
mill liners and cyclone spigot; improper
distribution of pulp to parallel processing
unit ( for example, cyclones) and other
mechanical reasons such as blockage of
launders, pipelines etc.
The objectives of the control system are thus to
be realized by manipulation of controllable
variables by applying suitable control action
as and when disturbances occur and persist
for long times. One of the primary objectives of
any grinding circuit control system being to
stabilize the produc t size at a point
corresponding to optimum mineral libration,
the produc t size bec omes an important
controlled variable. As a high circulating load
at a fixed produc t size lowers energy
consumption, control of circulating load also
becomes important. Further for smooth flow of
pulp from the mill it is necessary to control the
mill density below a critical level. Another basic
 MPT-2013

variable which is a target for control is the mill

discharge sump level. This variable is subjected
to control to avoid an overflowing or a dry
sump. Also, the rate of response of the circuit is
influenced by the sump level. For example, a
higher sump level can cause a slower circuit
response. Make: Power Build Ltd.
To summaries the variable which have to be Model: WFPR-141
considered in the context of grinding circuit Water flow rate
control are: 1) Product size, 2) Circulating load, The measurement of the variable is very simple
3) Mill density, and 4) sump level. and general types of sensors are avilable, orifice
In a typical grinding circuit at Tummalapalle plate meter, venturi meter are some of the
mill the above is being c ontrolled by c ommanly used devic e . How ever at
manipulation of: 1) Mill water addition, 2) Ore Tummalapalle mill magnetic flow meter has
feed rate to mill, 3) Sump water addition and 4) been used.
Throughput to cyclone.
In general for control of multistage grinding
circuits the manipulated variables are the ore
feed rate to the circuit, water addition at all
points and classifier throughputs.

4. Instrumentation for Grinding Circuit Control

For development of automatic control systems,

instruments to measure directly, or models to
infer the state of the variables by indirect
measurement are necessary perquisites. These
measurements must be consistent to give
accurate performance continuously over long
periods of time. The various sensing techniques
used in the grinding circuit control systems at
Tummalapalle Plant are described as follows
4.1. Measurement of Mass Flow Rate
Make: Endress+Hauser
Model: Promag 50
Slurry Flow Rate
Magnetic flow meters are the most commonly
used sensors for the measurement of slurry
flow rate in mineral industry. Liquid flowing
through a non magnetic tube in a magnetic field
induces a voltage in fluid proportional to flow
rate and field intensity.

Dry ore flow rate

Continuous weighing of material moved over
the c onveyor system c an be done by
mechanical, electrical or nuclear instruments.
Continuous weighing Belt conveyor for bulk
material – one or more rollers supported on load
cells scale. Belt speed (M/hr) and weight (MT/
M) are integrated to totalize Make: Endress+Hauser
Model: Promag P

89
 MPT-2013

4.2 Measurement of Density of Slurry This can be inferred from a model of the cyclone
(or the classifier in the circuit) or can be obtained
The only satisfactory method for measuring
by direct measurement. Both techniques have
slurry density is the Gama ray instrument. This
been successfully used in grinding circuit
instrument is based on the princ iple of
control. At our Turamdih Plant Particle size
transmission of Gama ray through the slurry.
indicator is in use. The basic principle is, as the
As the slurry becomes densor it transmits less
slurry flows through the Partic le Size
and this shielding is used to measure the slurry
Transmitter (ISTS), individual particles are
density. Typical application include density
physically measured by a reciprocating caliper
measurement of thickener under flow, density
sensor, that converts each measurement into
of cyclone feed in closed loop grinding. The Gama
an electronic signal. These signals are processed
source is cesium 137 in the thickeners under
by a modern set of industrial electronics (PCCS)
flow line at Tummalapalle. mill
designed to operate in a harsh plant
environment.

Make: Endress+Hauser
Model: FMG 60
4.3 Measurement of Sump Level
Particle Size Indicator
A Pulsed Sound Weave, Generated By A Make: outokumpu
Transmitting Crystal, Is Reflected From The intec(outotec)
Interface Between The Fluids And Returned To Model: PSI-200
The Receiving Crystal. The Level Is Measured
In Terms Of The Time Required For The Sound 5. Codes and Standards
Pulse To Travel From The Transmitter To The
Interface And Return STANDARDS:
Instrumentation and control equipment will be
in accordance with the latest
Applicable standards of the following:
 Institute of Electrical & Electronics
ENGINEER (IEEE)
 Instrument Society of America (ISA)
Make: Endress+Hauser  National Electrical Manufacturers’
Model: Micropilot Association (NEMA)
 American National Standards Institute
4.4 Measurement of Particle Size of the Product (ANSI)
 Indian Standards (IS)
One of the most important measurements  Scientific Apparatus Manufacturers’
required for effective control of grinding circuits Association (SAMA)
is the particle size (distribution) of the product.

90

 Americ an Soc iety of Mec hanic al
Engineers (ASMA)
 International Elec tro-tec hnic al
Commission (IEC)
 American Society for Testing Materials
(ASTM)
 Underwriters’ Laboratories (UL)
 Institute of Printed Circuits (IPC)
 Deutsche Institute Normale (DIN)
 British Standards Institute (BSI)
All other national standards meeting or
exceeding the requirements of the above
listing shall also be considered.
6. Metering Bases and Chart units
The following system of units shall be followed
throughout the specification
unless otherwise mentioned.
a) Pressure: Kg/Sq.cm; b) Differential Pressure:
mm of Water Column/Kg/Sq.cm
c ) Draught: mm of Water Column; d)
Temperature: Degree Celsius (deg.C)
e) Flow (solid / Slurry): Tonnes/ hr; f) Flow
(Water): NM3/hr; g) Density: gms/CC
h) Level: Meter; i) Particle Size: mm with % pass
7. General Remarks
In the Indian context, some important factors
to be considered while opting for automatic
control systems are.
a) Availability and after sales service facilities
for special purpose sensing instruments, the
controller hardware and process control
computers,
b) In plant maintenanc e fac ilities for
minimizing mechanical breakdowns and also
for the additional instrumentation required for
automation
91
MPT-2013
c) Finally, training of the plant metallurgists in
the necessary skills to develop, operate and
maintain digital c omputer based control
system.
8. Conclusion
For automating industrial wet grinding
c irc uits, the nec essary instruments,
transducers, actuators and other pieces of
hardware equipment are readily available in
our country. Substantial economic benefits can
be realized by automating mineral processing
operations.
It must be emphasised here that, to derive the
maximum benefits out of automatic control,
mechanical breakdowns in the mill should be
eliminated or minimized through adequate
maintenance.
Acknowledgment
The authors are thankful to the Management of
Uranium Corporation of India Limited for
presentation of this paper and to the colleagues
at Uranium Corporation of India Limited,
Tummalapalle for their help and suggestion.
References
Course II, Optimisation and Control of Mineral
Beneficiation Plants. Khetrinagar: 2nd-7th Feb,
1987.
Tender doc ument for UCTL-1,
Crushing,Grinding etc. prepared by M/s DCPL,
Kolkata.
 MPT-2013

*******

92
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Energy Optimization of Ball Mill Grinding Operation

Shivani Sharma1 and V. K. Gupta2

1
MBE Coal & Mineral Technology India Pvt. Ltd., North 24 Pgs., Kolkata 700156, India
2
B-402 Bansal Plaza, Station Road, Ranchi 834 001, India
Abstract
Size reduction in ball mills is an energy intensive operation. As the energy cost associated with
the grinding operation generally accounts for approximately 40-60% of the total cost of mineral
beneficiation, optimization of the grinding operation from the energy consumption point of view
is a task of considerable importance. With this objective in view, variation in the energy
consumption with various operating variables has been analyzed in terms of the energy specific
absolute rate of production of material finer than a specified size, F*. The operating variables
considered are: mill speed, particle load, ball load and ball size. It has been found that the variation
in F* with the operating variables is quite significant (20-40%) and the nature of variation is quite
complex. In particular, the effect of any one variable on F* was found to vary with the combination
of the values of other variables, and the effect was found to be different for different materials. It
has been emphasized that as the purpose of grinding is to produce fine particles, the mill design
and scale-up work should be based mainly on the F* parameters.

Keywords: Ball mills; design and scale-up; power specific parameters; fines production rate.

at such a methodology, studies related to the

1. Introduction
Every year hundreds of millions of tons of
metallic ores, minerals, cement and coal are
processed all over the world. The specific
energy consumption value for grinding of these
materials typically ranges from 5 to 50 kWh/
ton. Thus, there is a considerable scope for
improving energy efficiency by establishing the
optimum values of various mill operating
parameters, such as the mill speed, ball load,
ball diameter and particle load.
The other important task is to establish a sound
methodology for scale-up of ball mills based on
laboratory or pilot scale test work. For arriving
* Correspending Author:Shivani Sharma, MBE Coal &
Mineral Technology India Pvt. Ltd., North 24 Pgs., Kolkata
700156, India, E-mail: gupta.vinaig@gmail.com
effect of mill diameter on the rate of production
of particles of a desired size distribution are
required.
As the purpose of grinding is to produce fine
particles, it is prudent to use the energy specific
absolute rate of production of fines as the
parameter for characterization of the mill
performance (Gupta and Sharma, 2013). For this
purpose, a grinding kinetics mathematical
model derived from population balanc e
considerations is most appropriate (Reid, 1965;
Gupta and Kapur, 1976). This model is based on
two sets of parameters for various size fractions
of particles: specific breakage rate and breakage
distribution parameters. The equation used for
describing batch grinding kinetics is

93

(1)
where M i (t) is the mass frac tion of the
particulate solids in the sieve size interval i
(bounded by size of the aperture of upper sieve
xi-1 and size of the aperture of lower sieve xi), t is
grinding time, Si is specific breakage rate for
particles of size class i (fractional rate at which
material breaks out of size interval i), and bi,j is
the weight fraction of the material breaking out
of sieve size interval j that reports to sieve size
interval i. Let the weight fraction of material
finer than size xi at time t be denoted by Fi (t).
For the rate of production of material finer than
size xi we can write ( Herbst and Fuerstenau,
1973; Gupta and Kapur; 1976)
(2)
where Bi,,j denotes fraction of broken product
that is finer than the lower size limit of the size
interval i when particles of size interval j
undergo breakage. It is well known that in the
batch grinding operation, when a single size
feed such as a 10/14 mesh size fraction is ground,
the initial rate of production of material finer
than a given size remains constant for a short
but significant duration of time, depending on
the fineness of the c hosen size. This
phenomenon is known as ‘zero order
production of fines’ (Herbst and Fuerstenau,
1973). The ‘power specific absolute rate of
production of fines’, Fi*, can be defined as
(3)
where P is net mill power input and H is the
weight of particulate contents of the mill.
2. Approach to Analysis of Experimental Data
With a view to providing a ready estimate of
the percentage change in the F* value, we
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MPT-2013
defined the normalized value of F* as F**.
Normalization was done using the F* value
corresponding to a chosen reference value of
the operating condition. For example, while
studying the effect of mill speed, normalization
was done relative to 50% critical speed. Also, a
suitable choice of upper size limit was required
to be made for the F* parameter. Taking into
account various factors, we chose 100 mesh (150
µm) as the upper size limit for the ground
product.
3. Results and Discussion
3.1. Effect of mill speed
3.1.1. Effect of mill speed in dry grinding
Kim (1974) has studied the effect of mill speed
on the grinding kinetics for a 10/14 mesh size
fraction of limestone. A 25.4 cm diameter ball
mill was used. The other mill operating
conditions were as follows: mill speed, N: 0.5-
0.8 (50-80 % critical); ball size, d: 25.4 cm; ball
load, J: 0.5 (corresponding to 50% filling of mill
volume by the static ball charge); particle load,
U: 1.0 (corresponding to 100% filling of
interstitial volume of static ball charge). Using
this data, F** values for a -100 product were
calculated. The variation of F** with mill speed
is shown in Fig. 1. It can be seen that as the mill
speed increases from 50 to 70 % critical, the F**
value increases by about 40%. A further
increase in the mill speed leads to a sharp drop
in the F** value.
3.1.2. Effect of mill speed in wet grinding
It is well known that the wet grinding kinetics
are strongly particle size distribution
dependent. Fig. 2 shows results obtained from
Kim’s data for variation in the F** value for a
medium fine size distribution range (-14 mesh:
63-86%; -200 mesh: 11-21%) for grinding of a
10/14 mesh size fraction of limestone. The other

mill operating conditions were: % solids: 60; N:
0.6; U: 1.0, J: 0.5. It can be seen in Fig. 2 that as
the mill speed increases from 50 to 70% critical,
the F** value does not show any significant
increase. Further increase in the mill speed leads
to a sharp decline in the F** value.
Fig. 1: Variation in F** with mill speed for dry
grinding of a 10/14 mesh size fraction of lime-
stone
Fig. 2: Variation in F** with mill speed for wet
grinding of a medium fine size distribution of
limestone (wt.% solids: 60%)
3.2. Effect of particle load in dry grinding
Berlioz (1966) studied the effect of particle load
on the grinding rate of a 7/9 mesh size fraction
of natural, uncrushed dolomite in a 25.4 cm
diameter laboratory ball mill (N: 0.6, J: 0.5, U:
0.2 to 1.6). The F* values were normalized using
the F* value corresponding to U=1. Fig. 3 shows
variation of F** with the particle load. It is
observed that as we go from right to left, the F**
95
MPT-2013
value does not change and remains constant
up to U=0.8. After this point, the F** values
c ontinuously decrease up to the U= 0.2.
Moreover, there is an overall decrease of 38% in
the F** value.
Fig. 3: Variation in F** with particle load for
dry grinding of 7/9 mesh dolomite with mono-
size balls
We carried out a detailed study on the effect of
particle load and ball load on grinding kinetics
by carrying out experiments at two different
mill speeds (55 and 70 % critical) and four levels
of ball load ( J: 0.2,0.3,0.4 and 0.5). A 29 cm
diameter mill with a built in wavy liner was
used. The ball charge consisted of equal number
of 1.27, 1.90 and 2.54 cm balls. The particle load
U was varied in the range 0.25 to 2.0. In this
study, the test material used was quartz. Fig. 4
shows variation of F** (-100 mesh) with the
particle load at 70% critical speed and 40%
filling of the mill volume by the ball charge.
Normalization was done relative to the
respective values at U=0.75. A comparison of
the c urve shown in Fig. 4 with the
corresponding curve in Fig. 3 shows two main
differences: (i) the maximum value is reached
at a lower U value (0.75 as compared to 1.0);
and (ii) the value of the parameter F** does not
remain constant as we move to the right from
the maxima – in fact a sharp decline is observed.
In our opinion these differences are mainly due
to the size consist of the ball charge: a single
size ball charge versus a ball charge made up of
balls of three different sizes. The void space in
the ball charge, the relative movement of
different layers of balls and the type of breakage

events generated are expected to vary with the
ball size distribution.
Fig. 4: Variation in F** with particle load for
dry grinding of 20/28 mesh quartz with a ball
mix consisting of balls of three different sizes.
3.3. Effect of ball load in dry grinding
Smaila (1982) dry ground 20/28 mesh quartz
ground in a 60 cm diameter ball mill ( N: 0.7, U
: 0.75, J: 0.2-0.5). Fig. 5 shows the variation of
F** with ball load at 70 % critical speed. The
curve shows a maxima at J=0.3 and a minima
at a J =0.45. Moreover, there is a marked
variation in the F** value (33%).
Fig. 6 shows variation in the F** value with ball
load at 55% critical speed for two values of U:
0.75 and 1.5. It is observed that in all three cases
the F** value increases consistently with J,
without showing a maxima. The rate of increase
in the values of F* parameter is higher for a U
value of 0.75. As the J value increases from 0.3
to 0.5, there is an overall increase of 25% in the
value of F**.
Fig. 5: Variation in F** with ball load for dry
grinding of 20/30 mesh quartz at 70 % critical
speed
96
MPT-2013
Fig. 6: Variation in F** with ball load for dry
grinding of 20/28 mesh quartz at 55 % critical
speed
3.4. Effect of ball diameter
With a view to comparing the effect of ball
diameter on grinding behaviour of two
materials of significantly different hardness,
we selected the batch grinding size distribution
data of Malghan [7] on 28/35 mesh limestone
and that of Smaila [17] on the same size quartz.
Fig. 7 shows the variation of F** (-100 mesh)
values for quartz and limestone with ball
diameter. It can be seen that in both the cases
the F** values decrease with increase in the ball
diameter. However, the decrease in F** is more
pronounced in case of limestone. Thus, we see
that the effect of ball diameter is not same for
two materials of different hardness.
Fig. 7: Variation in F** with ball diameter for
dry grinding of quartz and limestone.

3.5. Effect of mill diameter
Siddique (1977) has presented data on dry
grinding of 10/14 mesh limestone in 25.4, 38.1
and 76.2 cm diameter ball mills. The mill speed,
ball load and particle load values corresponded
to: (N: 0.6; J: 0.5; U: 1.0). Balls of four different
diameters, 12.7, 19.05, 25.4 and 38.1 mm, were
used for preparing the ball charge. Fig. 8 shows
the variation of F** with mill diameter for this
set of operating conditions. It can be seen that
the F** value increases linearly with mill
diameter, showing an overall increase of 16%.
Fig. 8: Variation in F** with mill diameter for
dry grinding of 10/14 mesh limestone.
3.6. General Discussion
In this paper, we have presented some results
on the effect of mill operating variables on the
power specific absolute rate of production of
fines. Recently, Gupta and Sharma (2013) have
presented a more detailed analysis of the effect
of mill operating variables on the specific energy
consumption in the grinding operation. In their
analysis, in addition to the rate of production
of fines, the rate of breakage of the coarsest size
fraction has also been considered. It has been
shown that the well known proposition of
Herbst and Fuerstenau (1980) that the power
specific absolute rate of breakage of particles
does not vary significantly with the mill
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operating conditions, is not correct. They have
shown that even the breakage distribution
function varies significantly with the mill
operating conditions. The overall result of the
variation in all the S and B parameters is
reflected in the rate of production of fines. It is
for this reason that the F* parameter is more
appropriate for carrying out the scale-up and
design work. Even the Bond (1960,1961) scale-
up model is based on the rate of production of
fines, whic h is c harac terized by the
grindability parameter, G, of the Bond work
index equation.
It should be pointed out that in the mineral
processing plants most of the grinding is carried
out in the wet mode. However, no significant
data is available in the literature on the wet
mode of operation. The grindability test of Bond
is a dry batch grinding test. And, the scale-up
model of Herbst and Fuerstenau (1980) is also
based on dry grinding data.
4. Conclusions
Analysis of a large amount of batch ball mill
grinding data available in the literature has
shown that the value of the power specific
absolute rate of production of -100 mesh fines,
F*, shows a significant variation (20 to 40%)
with various mill operating variables.
The breakage characteristics (hardness of
material) and the mode of grinding operation
(dry/ wet) have significant effect on the nature
and magnitude of variation in the value of the
F* parameter. Moreover, the effect of any
partic ular operating variable on the F*
parameter is observed to be different under
different operating conditions. Therefore, the
effect of any particular operating variable, such
as the mill speed, on F* cannot be described in
terms of mill speed alone. The relationship is
not unique and it should incorporate the effects
of other variables (such as the ball load, ball
size distribution and particle load) also.

In view of the complex nature of variation in
the value of the F* parameter, it is proposed that
depending on the likely range of operating
conditions for the production mill, the optimum
values of various operating variables should
be established by carrying out some well
designed grinding experiments in a laboratory
ball mill of a moderate size.
Nomenclature
bi,j weight fraction of the material breaking
out of sieve size interval j that reports to
sieve size interval i.
Bi,,j fraction of broken product that is finer
than lower size limit of the size interval i
when particles of size interval j undergo
breakage
F* absolute rate of production of fine material
per unit power input
F** power specific absolute rate of production
of fine material relative to the
corresponding value for some chosen
value of the operating condition under
consideration
Fi mass fraction of particulate solids finer
than sieve i
H total mass of the particulate charge in the
mill
J fraction of mill volume filled by static ball
charge
Mi mass fraction of the particulate solids in
the sieve size interval i
N fraction of critical speed of mill
P net power drawn by mill
Si specific breakage rate for particles of size
class i
t grinding time
U fraction of void volume of the static ball
charge occupied by the particulate solids
References
Austin, L.G., Klimpel, R.R., Luckie, P.T., 1984.
Process Engineering of Size Reduction: Ball
Milling, Society of Mining Engineers, New
York, pp. 341-384.
*******
98
MPT-2013
Berlioz, L.M., 1966. Kinetics of dry grinding. M.S.
Thesis, University of California, Berkeley,
Calif., USA.
Bond, F.C., 1960. Confirmation of the third
theory. Trans. AIME 217, 139-153.
Bond, F.C., 1961. Crushing and grinding
calculations. Brit. Chem. Eng. 6, 378-391.
Gupta, V.K., Kapur, P.C., 1976. A c ritical
appraisal of the discrete size models of
grinding kinetics. in: Rumf, H., Schonert,
K. (Eds.), Proceedings, Fourth European
Symposium Zerkleinern, Dec hema
Monographien 79, Nr. 1576-1599, Verlag
Chemie, Weinheim, pp. 447-465.
Gupta, V.K, 2013. Validation of an energy-size
relationship obtained from a similarity
solution to the batch grinding equation. Powder
Technol. 249, 396-402.
Gupta, V.K., Sharma, S., 2013. Analysis of ball
mill grinding operation using mill power
specific kinetic parameters. Adv. Powder
Technol. (in press).
Herbst, J.A., Fuerstenau, D.W., 1973. The zero
order produc tion of fine sizes in
comminution and its implications in
simulation, Trans. AIME 241, 538-546.
Herbst, J.A., Fuerstenau, D.W., 1980. Scale-up
procedure for continuous grinding mill
design using population balance models.
Int. J. Miner. Process. 7, 1 - 31.
Kim, J.H. 1974. Normalized model for wet batch
ball milling, Ph.D. Dissertation, University
of Utah, Utah, USA.
Malghan, S.G., 1975. The scale-up of ball mills
using population balance models. D. Eng.
Dissertation. University of California,
Berkeley, California.
Reid, K.J., 1965. A solution to the batch grinding
equation. Chem. Eng. Sci.. 20, 953-963.
Siddique, M., 1977. A kinetic approach to ball
mill scale-up for dry and wet systems.
M.S.Thesis, University of Utah, USA.
Smaila, F.M., 1982. An investigation of the
kinetics of dry batch ball milling. M.S.
Thesis, The Pennsylvania State University,
Pennsylvania, USA.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Understanding Bond Work Index and Its Limitations

V. K. Gupta*
B-402 Bansal Plaza, Station Road, Ranchi 834 001, India

Abstract
Bond Work Index, Wi, is widely used for estimation of the mill motor power and the size of ball
and rod mills for grinding of minerals, ores, cement and various other materials. The definition of
Work Index has no sound theoretical basis. It is purely an empirical correlation developed from a
large amount of plant operating data. In case of complex, non-homogeneous materials which
exhibit significant variation in the breakage characteristics with particle size, and in case of very
soft and very hard materials, Wi value fails to provide a reasonable estimate of the power required
to grind the material to the required degree of fineness. Therefore, it is found that in most of the
plants the grinding mills are overdesigned to reduce the risk. This paper discusses some of the
important drawbacks and limitations of the Bond Work Index with a view to developing a better
understanding from the point of view of its correct interpretation and practical application.

Keywords: Size reduction, Rod and ball mills, Scale-up, Specific power consumption, Bond work
index

1. Introduction following relationship given by Bond (1952,

In view of the fact that every year billions of
tons of metallic ores, minerals, cement and
various other solids are ground in the rod and
ball mills, it is important to have a sound
methodology for the design and scale-up of
these mills from the energy efficiency and
productivity points of view. In this context, an
important task is the estimation of the mill size
(diameter and length) and the motor power for
the required production rate of the ground
material of desired fineness from a feed charge
of known breakage characteristics (hardness)
and size distribution. At present, for a closed
circuit, wet ball mill grinding operation, the mill
motor power is generally estimated using the
* Correspending Author: V. K. Guita, B-402 Bansal Plaza,
Station Roa d, Ranchi 834 00 1, Ind ia, Email:
gupta.vinaig@gmail.com
1960, 1961).
 1 0W i 1 0W i 
P T    (1)
 x80 ( p ) x 
8o ( f ) 

where P is the power required at the pinion
shaft of the mill (kW), T is the feed rate of the
material (t/h), Wi is the work index (kWh/
ton),x80(p) is the size in microns at which 80
percent of the grinding circuit product (i.e., the
classifier overflow) passes, x80(f) is the size in
micron at which 80 percent of the fresh feed to
the grinding circuit (generally the rod mill
discharge) passes, and p and f denote the
grinding circuit product and feed, respectively.
Based on the results of the standard Bond
grindability test, value of the Work Index, Wi,
is obtained from the following relationship

99

4 8 .9 5
Wi 
S 0 .2 3
G 0 .8 2
 10

10
 
 X 8 0 ( 8 0 ) 
 X 80 ( p )
where S is the opening in microns of the test
sieve, G is grindability, defined as grams of test
sieve undersize product produced in one mill
revolution in the last cycle of the test, X80(p) is
the size in microns at which 80 percent of the
last cycle test sieve undersize product passes,
and X80(f) is the size in micron at which 80
percent of the new feed to ball mill passes. It is
interesting to note that the relationship given
by Eq. (1) is applicable to a closed-circuit,
continuous, wet grinding operation, but it is
based on the Work Index value derived from a
dry batch grinding test data. Actually, both the
equations are purely empirical equations,
developed from a large amount of test data
obtained for a continuous 2.44 m (8-ft.) diameter
ball mill.
Various limitations of the Bond approach to the
scale-up of ball mills have been discussed in
detail by Herbst and Fuerstenau (1980), Austin
et al. (1984) and Gupta (2013). Some of the
important ones are listed below:
 As the size reduction of particles takes place
in the grinding mill, in respect of the energy
requirement what really matters is the size
distribution of the actual feed to the mill
and the size distribution of the mill
discharge. However, Eqs. (1) and (2) of the
Bond model are based on the 80% passing
sizes of the fresh feed and the final circuit
product, which are quite different from the
corresponding values for the actual mill
feed and mill discharge.
 Bond model assumes that all materials
break similarly. Therefore, the exponent of
80% passing sizes in Eq. (2) has a fixed value
of 0.5. This is not correct as shown by Kapur
(1972) and Gupta (2013). The value of this
exponent varies over a wide range, possibly
from 0 to 2.
MPT-2013
 Bond test proc edure uses ideal

(2) classification, while the classifiers used in
the industry deviate substantially from
perfect separation behaviour. Therefore,
Bond test does not correctly simulate the
ac tual plant operation (Herbst and
Fuerstenau, 1980; Austin et al., 1984).
 Batch grinding test simulates plug flow
behaviour as all particles remain in the mill
for the same length of time. In practice, in
the continuous mode of operation particles
exhibit a distribution in their time of
residenc e in the mill (Herbst and
Fuerstenau, 1980; Austin et al., 1984).
 The influence of slurry density and slurry
rheology on particle breakage rate and
breakage distribution function is not taken
into account in calculation of the energy
requirements (Austin et al., 1984).
 Variation in the spec ific energy
consumption with important operating
and design variables such as the mill speed,
ball load, ball size distribution and lifter
design is not c onsidered (Gupta and
Sharma, 2013).
We disc uss below the above mentioned
deficiencies and their influence on prediction of
energy consumption in the grinding operation.
2. Discussion
2.1. Choice of the feed and product streams
In the c ontext of his ‘Third Theory of
Comminution’, Bond (1961) has stated: “Work
index expresses the resistance of material to
crushing and grinding. Numerically the work
index is the kWh per ton required to reduce the
material from theoretically infinite size to 80%
passing 100 µm.” The basic Third Theory
equation is
 10Wi 
10Wi
E 
 y ( p)
  (3)
 80 y80 ( f ) 
where E is the specific energy input (kWh), y80(p)
is the size at which 80 percent of the product
passes, and y80(f) is the size at which 80 percent
100
 MPT-2013

of the feed passes. We have used here letter y for one for which á value is 0.5. It follows that the
particle size because we are now considering greater is the deviation in á value from a value
the actual feed to the grinding mill and the of 0.5, the greater will be the error in the
actual mill product. As Bond proposed his Third predicted Work Index value.
Theory after rejecting the theories of Rittinger
(1867) and Kick (1885), originally his Third 2.3. Influence of the X values on the accuracy
Theory referred to the material being actually of the work index
broken in the mill. Later, while proposing Eqs. (1) The standard procedure for preparation of the
and (2) he used the 80% passing sizes of the fresh fresh feed for carrying out the Bond grindability
feed to the grinding circuit and the final circuit test requires stage crushing of the as received
product, i.e., the classifier overflow( test sieve sample of the test material to 100% passing 6
undersize in case of Eq.(2)). No justification was mesh sieve. It has been observed that in a large
given by Bond for doing so. It should be noted number of cases the 80% passing size for the
that in general the three sets of x, X and y values fresh feed prepared in this manner,X80(f), lies in
are quite different in magnitude. In view of these a narrow range of 1900 – 2100 µm, and the 80%
passing size for the last c yc le test sieve
observations, it can be concluded that Eqs. (1)
undersize product,X80(p), lies in a narrow range
and (2) are purely empirical equations and have
of 110-125 µm (see Table 1). In such cases, it can
nothing to do with Bond’s original Third Theory. be easily seen that irrespective of the value of
2.2. Choice of the exponent of particle size the exponent  , for a chosen value of S, the
work index value will be mainly determined
In Eqs. (1), (2) and (3) Bond, based on his by the parameter G. However, if the values of
argument that the energy input is proportional the parameters X80(f) and X80(p) are found to be
to the new crack tip length produced, has used far removed from the respective range of values
mentioned above, as is the case with some
a value of 0.5 for the exponent of particle size.
samples of iron ore and chromite ore, depending
However, it has been shown that it is true only
on the  value the Bond Work Index value
for an ‘ideal Bond material” (Austin and Luckie, obtained from Eq. (2) can have significant error
1972; Herbst and Fuerstenau, 1980). A more (note that the error will be zero if  = 0.5).
general energy-size relationship derived by
Kapur (1972) and verified by Gupta (2013) is Table 1: Bond grindability test data for
different materials and the work index value.
C C S. No. Material G, g/rev X 80 (f), µm X 80 (p), µm Wi, kWh/t
E 
  (4)
x ( p ) x80 ( f )
80
1 Anthracite 0.156 1866 121 105.2
2 Nut coke 0.415 1720 125 48.7
3 Pyroxinite 1.123 1949 123 20.8
where C is a mill-material constant, and á is 4 Olivine 1.553 1359 116 16.4
the exponent of particle size v in the following 5 Iron ore 1.602 1925 110 14.5
6 Limestone-1 1.662 2220 110 13.8
expression for the grinding rate parameter k
7 Dolomite 1.860 1964 110 12.8
k(  )  A  (5) 8 Limestone-2 1.971 1971 113 12.4
9 Iron ore-1 2.260 1185 114 12.1
10 Iron ore-2 3.003 1180 108 9.4
where A is a mill-material constant. The value
11 Iron ore-3 4.830 1510 95 4.3
of á has been found to vary in the range of 0 to 2 12 Chromite-1 3.780 1569 80 6.0
(Gupta, 2013). 13 Chromite-2 4.730 792 92 6.3
14 Chromite-3 5.742 1690 125 5.7
In Eq. (4) if C is replaced by (10 Wi) and á is
assigned a value of 0.5, we obtain Eq. (3) of Bond. It should be pointed out that Eq. (2) was
Thus, we see that an ‘ideal Bond material’ is the developed by Bond using the experimental data

101

obtained on a 2.44 m diameter wet overflow
ball mill operated in closed circuit at a 250%
circulating load and the data obtained for same
materials by c arrying out standard
grindability tests in the 300 mm x 300 mm size
standard Bond mill. Though it is not known, it
is likely that the range of X80 and x80 values for
the two sets of tests conducted in the two mills
were nearly same and similar to those
mentioned above. If this was really true, then
the values of X80, x80 and á did not have any
significant effect on the final result, as can be
seen by substituting for Wi in Eq.(1) from Eq.
(2). In fact, for a special case where we have:
x80(p) = X80(p) and x80(f) = X80(f), substituting for
Wi in Eq. (1) from Eq. (2) we obtain
48.95T
P (6)
S 0.23 G0.82
Thus, we see that for a given S value the power
required for the size reduction job is mainly
determined by the parameter G if the two sets
of x80 and X80 values are same or nearly same.
But if in any particular case the two sets of x80
and X80 values differ significantly or they lie
outside the range covered by Bond in his test
work, the power estimates obtained using Bond
equation can be in error.
2.4. Understanding the significance of the
exponent of ‘Grindability’
Grindability, G, is expressed in grams of the fine
product produced per unit mill revolution. As
energy input to the mill is proportional to
grinding time, it follows that the energy
required in kWh/ton should be inversely
proportional to G. However, in Eq. (2) we notice
that the exponent of G is 0.82 instead of 1. It can
be shown that this empirical exponent appears
in Bond’s correlation to account for two main
differences in the grinding operation carried out
in the standard Bond grindability test ball mill
and an industrial production mill: (i) the
102
MPT-2013
residence time distribution of the Bond mill
used for determination of the grindability
corresponds to plug flow (characterized by a
zero variance) as it is operated in the batch
mode; the residence time distribution of a
production mill is a well distributed function
for which the variance value is significantly
greater than zero, and (ii) the test sieve used in
the grindability test acts as a perfect classifier;
the efficiency of the classifier used in the
industrial grinding circuit is significantly lower
than 100%. For production mills, the value of
the normalized variance of the residence time
distribution is typically in the range of 0.3 to
0.5 (Marchand et al., 1980). In the context of the
‘m perfect mixers in series’ model of the
residence time distribution, a normalized
variance value of 0.5 corresponds to m = 2 and a
value of 0.333 corresponds to m = 3 (Austin et
al., 1984). Following the example given by
Herbst and Fuerstenau (1980), in Table 2 are
given the values of c orrec tion fac tors
corresponding to two values of the normalized
variance of the RTD and two values of the
c lassifier effic ienc y. If the value of the
normalized variance of the RTD for the 2.44 m
diameter mill used by Bond and the efficiency
of the classifier used by Bond were known, we
could find out the corresponding correction
factor from Table 1. It should be noted that this
correction factor is already included in the
c onstant 48.95 of Eq. (2). However, an
appropriate correction factor should be worked
out for each individual grinding circuit.
Table 2: Correction factor for the work index
value obtained from Eq. (2) as a function of the
variance of the residence time distribution and
the classifier efficiency.
S. No. Normalize Number of Correction factor
d variance perfect Classifier efficiency, %
of RTD mixers 100 70 50
1 0.000 ∞ 1.0 1.167 1.546
2 0.333 3 1.041 1.235 1.665
3 0.500 2 1.068 1.279 1.757

In Eq. (2) the exponent of the grindability has a
value 0.82. It will be seen that for G values
greater than 1 g/rev. the calculated work index
value will be greater than the one obtained with
a value of 1 for the exponent. For example, for
the case G = 2 g/rev. an increase of 13.3% is
obtained in the calculated work index value as
compared to the value obtained with a value of
1.0 for the exponent. However, if the G value is
lower than 1 g/rev., it results in a decrease in
the work index value (a decrease of 11.7% for a
G value of 0.5 g/rev.). Thus, we see that a G value
dependent correction factor is not appropriate
in the Bond model.
2.5. Effect of the operating and design variables
on energy requirement
A major criticism of the Bond model is its
inability to account for the effect of operating
variables such as the ball size distribution, mill
speed, ball load and slurry density on the
specific energy consumption. It has been
recently shown (Gupta and Sharma, 2013) that
there can be up to 40% variation in the specific
energy consumption on account of these
variables. An analysis of the effect of the
operating variables in terms of the work index
of the Bond model is beyond the scope of this
paper.
3. Conclusions
Based on the discussion of the Bond model
presented above, in conclusion it can be said
that though the Bond model gives reasonably
good estimates of the power requirements in a
number of cases, there is a considerable scope
for improving the accuracy of the energy
estimates by using the size-mass balance
mathematical modelling approach (Herbst and
Fuerstenau, 1980; Austin et al.; 1984; Gupta,
2013; Gupta and Sharma, 2013). In our opinion,
this is partic ularly true for materials
characterized by a grindability value less than
1.0 and more than 3.0 g/rev., and for those
grinding operations where the slurry density
is significantly lower or higher than the value
*******
103
MPT-2013
corresponding to the normal range for the
weight percent solids (60-70%).
References
Austin, L.G., Klimpel, R.R., Luckie, P.T., 1984.
Process Engineering of Size Reduction: Ball
Milling, Society of Mining Engineers, New
York. 341-384.
Austin, L.G., Luckie, P.T., 1972. Grinding
equations and the Bond work index. Trans.
SME-AIME. 252, 259-266.
Bond, F.C., 1952. The third theory of
comminution. Trans. AIME. 193, 484-494.
Bond, F.C., 1960. Confirmation of the third
theory. Trans. AIME 217. 139-153.
Bond, F.C., 1960. Crushing and grinding
calculations. Brit. Chem. Eng. 6, 378-391.
Gupta, V.K, 2013. Validation of an energy-size
relationship obtained from a similarity
solution to the batch grinding equation.
Powder Technol. 249, 396-402.
Gupta, V.K., Sharma, S., 2013. Analysis of ball
mill grinding operation using mill power
specific kinetic parameters. Adv. Powder
Technol. (in press).
Herbst, J.A., Fuerstenau, D.W., 1980. Scale-up
procedure for continuous grinding mill
design using population balance models.
Int. J. Miner. Process. 1, 1-31.
Kapur, P.C., 1972. Self-preserving size spectra
of comminuted particles. Chem. Eng. Sci.
27, 425-431.
Kick, F., 1885. Das Gesetz der proporionalen
Widerstande und siene Anwendung,
Arthur Felix, Leipzig, 118.
Marchand, J.C., Hodouin, D., Everell, M.D., 1980.
Residence time distribution and mass
Transport c harac teristic s of large
industrial grinding mills. O’Shea, J., Polis,
M. (Eds.), Proceedings Automation in
Mining, Mineral and Metal Processing, 3rd
IFAC Symposium, Montreal, Canada,
Pergamon Press. 295-302.
Von Rittinger, P.R., 1867. Lehrbuc k der
Aufbereitungskunde, Ernst und. Korn,
Berlin, 595.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Effect of Breakage on Coal Characteristics-A Case Study

Arun K Hardaha, Anubhav Kumar, Utkarsh Singh, Shalini Gautam and V K

Saxena*
Department of Fuel & Mineral Engineering, Indian School of Mines, Dhanbad, India

Abstract
As the Coal is mined from the seam, the breakage of coal starts and continues till the end utilization
of coal. During the breakage process all reduced or broken coal does not have the same size and
same percentage of each fraction. The characteristics of coal also may not be the same for all size
fractions. They may vary with the each size fraction; thereby it is important to understand how
these characteristics are varying with different size fraction. In the present context breakage
study adopting the simple drop test was conducted to investigate the changes in various properties
like ash content, volatile matter, ultimate analysis, HGI, CSN and caking index. The study has
been made using the two low volatile medium ash medium caking coal. From the study it was
observed that in a particular size fraction there is considerable improvement in almost all the
properties viz. ash from 24.30% to 18.07 % and 27.76% to 21.91 %, volatile matter from 19.08 to
21.25 % and 19.05 to 21.35 %, HGI from 56.13% to 61.71 and 64.98 to 81.51, CSN from 1.5 to 4.5 in
both cases and caking index from 16 to 18 & 19 respectively. Calorific values also show improvement
in both cases.

Keywords: Coal Breakage, Drop Shatter Test

1. Introduction The handling cause to more breakage but

The breakage of coal occurs in the process of
mining, loading and unloading and during
beneficiation due to the fracture in coal. The
cause of these fracture are natural entities of
coal and forces which applied during these
operation. Coal is fragmented in no uniform size
these sizes have different strength to cause
further fragmentation and fines generation. The
fragmented portion of coal should possess coal
entities that characterize the fraction giving
pertinent properties for beneficiation and
utilization.
* Correspending Author: V.K. Saxena, Professor, Department
of Fuel & Mineral Engineering, Indian School of Mines,
Dhanbad, India
mannerly, by the some specific property on
specified size fraction. Thus specific coal is
concentrated on specified size fraction. These
concentrations affect the physical and chemical
properties of coal. Breakage study of coal during
loading and unloading can easily be studied by
Drop Shatter Test, which simulate the dropping
of coal on loading and dropping into the bunker,
it measures the resistance to shattering or the
impac t hardness, whic h is measured in
abrasion test. Representative sample of coal
over a certain specified sized is dropped under
standard condition, the resistance to breakage
being measured by the percentage of the coal
which retain on different sieves after the test.

104

2. Material and Methods
2.1. Sample collection and preparation
The study has been made using the two low
volatile medium ash medium caking coal from
Jharia coalfield named as ‘Coal Sample A’ and
‘Coal Sample B’. These samples were resized
not less than 51 mm nor more than 60 mm. A
part of the sample is used for the basic
characterization of coal viz. Proximate and
Ultimate Analysis, Caking Index Swelling
Index, Caking Index, HGI. Rest of the prepared
samples is used for the Shatter Index Test to
simulate the breakage during dropping.
2.2. Method of the drop shatter test (ASTM
D440-86)
The test is designed to simulate the effect of
dropping of coal on loading, dropping into
bunker; it measures therefore the resistance to
shattering or the impact hardness, which is
measured in abrasion test. Representative
sample of coal over a certain specified sized is
dropped under standard c ondition, the
resistance to breakage being measured by the
percentage of the coal which remain on different
sieves after the test, or some mathematical
expression of these values.
2.2.1. Apparatus
The main part of the apparatus are the boxes to
hold coal before shattering and after shattering
with a poll which used to rising the coal holder
box to a height of 6 feet The main support are
fastened to the outside of the side plates of the
base plate and also to a top plate to support the
pulleys from which the box is suspended. The
vertical supports are kept outside the base plate
to facilitated shoveling the coal after each drop.
The top plate is 15 to 20 cm wide and 6 mm
thick, it supports two pulleys from which the
box is suspended by two wire ropes which
guides on the end plates near the box. A counter
weight is suspended through the other end of
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MPT-2013
two wires ropes so that a double pulley is
necessarily at the right hand end. The counter
weight consists of a fixed weight equal to that
of the box and two 12 g removal weight, which
are slotted into rods which pass through the
centers of the fixed weights.
2.2.2. Sieve
The sieves used for the analysis are of the Indian
Standard, which is made of from woven wire
in the frame of timber-slabs. The size of screened
used for the analysis are of 51 mm, 38 mm and
12.5 mm.
2.2.3. Procedure
25 kg of over 51 mm coal sample was weighed
and placed in to the box of Shatter Apparatus,
care was taken to ensure that fracture of coal
has not taken place while putting the coal in
box. The bottom plate of box was closed by latch.
The height of box was raised to 6 feet, and the
latch of the shatter test box was opened to allow
the coal to fall on to the base plate. The process
was repeated for three times.
A sieve of 51, 38 and 12.5 mm aperture was
arranged, keeping the large aperture sieve at
top. Shattered coal collected from base of the
apparatus was placed on to the top of +51 mm.
The four sizes, +51 mm, -51 + 38 mm, -38 + 12.5
mm and -12.5 mm sizes was obtained, all
fractions of shattered coal was measured and
shatter indices for 51, 38, 12.5 & - 12.5 mm was
reported as percentage basis.
The coal properties viz., Proximate analysis (IS
1350 Part 1 – 1984 (Reaffirmed 1996)), HGI (IS
4433- 1979 Reaffirmed 1994), Free Swelling
Index or Crucible Swelling Number (CSN) ,
Caking Index (CI) (IS 1353: 1993), and Specific
Gravity of these fractions were analyzed by
following standard test procedure, whereas
ultimate analysis and gross calorific value was
determined using Elementar Vario EL III CHNS
analyser and Leco AC 350 bomb calorimeter
respectively.
 MPT-2013

3. Results and Discussion 3.3. Variation of coal properties of shattered

3.1. Characteristics of coal samples fraction
To know the effect of breakage on coal properties
The Characteristics of Feed Coal Sample A and each fraction of Drop Shatter Test is subjected
B are presented in Table 1 and Table 2. to various analysis and the result of these
Table 1: Proximate and Ultimate Analysis of analysis are presented in Table 3 to Table 6.
Coal Sample A & Coal Sample B Table 3: Proximate & Ultimate Analysis of
Shattered Fraction of Coal Sample A
Sample Proximate Analysis Ultimate Analysis
M VM ASH FC C H N S O Sample Proximate Analysis, % Ultimate Analysis, %
A 19.0
1.24 24.30 55.38 63.73 3.91 1.69 0.86 4.34 “A” M VM Ash FC C H N S O
8
B 19.0 + 51 1.39 18.76 25.03 54..82 64.08 3.98 1.67 0.81 3.31
0.19 27.76 53.00 62.68 3.88 1.77 0.73 2.99
5 - 51+38 1.22 18.89 24.30 55.59 64.71 3.94 1.71 0.65 3.465
- 38+12.5 1.03 19.52 22.87 56.58 65.97 3.96 1.54 0.83 3.527
-12.5 0.96 21.25 18.07 59.72 70.96 4.37 1.81 0.74 3.088
Table 2: Results of HGI, CSN, CI, Calorific
Feed 1.24 19.08 24.30 55.38 63.73 3.91 1.69 0.86 4.337
Value and Specific Gravity of Coal Sample A
& Coal Sample B
Table 4: Proximate and Ultimate Analysis of
Shattered Fraction of Coal Sample B
Sample Coal Properties
HGI CSN CI GCV( Cal/g) Sp. Gr.
Coal Sample A 56.13 1.5 16 6122.9 1.50 Sample Proximate Analysis, % Ultimate Analysis, %
Coal Sample B 64.98 1.5 16 5911.1 1.54 “B” M VM Ash FC C H N S O

+ 51 0.23 18.97 28.34 52.46 62.05 3.85 1.72 0.77 3.04

3.2. Results of drop shatter test - 51+38 0.28 18.35 28.74 52.64 61.72 3.79 1.66 0.65 3.16
-
0.56 19.32 24.54 55.58 65.4 4.01 1.61 0.61 3.27
To simulate the Breakage of coal Drop Shatter 38+12.5
-12.5 0.45 21.35 21.91 56.29 67.74 4.25 1.83 0.77 3.04
test is carried out. Percentages of coal retained Feed 0.19 19.05 27.76 53.00 62.68 3.88 1.77 0.73 2.99
on different sieve of 51, 38, and 12.5 mm and
Pan are reported below in graphical form: It Table 5: Specific gravity, HGI, CSN, Caking
can be observed from Fig. 1 that more than 55% Index (CI) and GCV of all Shattered Fraction
of the coal has retain their original size of above
51mm whereas below 12.5 fraction has 6% in SAMPLE Coal Sample“A” “B”
coal sample A and about 8% in coal sample B. Property Specific HGI CSN CI GCV, Specific HGI CSN CI GCV,
Fraction Gravity kcal/kg Gravity kcal/kg
+51 1.59 54.81 2.5 17 6233.1 1.60 68.41 2.5 14 6233.1
-51+ 38 1.56 54.25 1 17 6270.4 1.64 64.60 1 13 6270.4
-38+12.5 1.52 56.93 2 16 6307.9 1.57 65.14 2 17 6307.9
- 12.5 1.43 61.71 4.5 18 6833.8 1.52 81.51 4.5 19 6833.8
FEED 1.50 56.13 1.5 16 6122.9 1.54 64.98 1.5 16 6122.9

3.4. Effect of breakage on various coal

Fig. 1: Shatter Index (Stability) of Coal Samples
properties
Effect of various size fractions and variation in
the various properties viz., proximate analysis,
ultimate analysis, Free swelling index (CSN),
caking index (CI), hardgroove grindability
index (HGI), specific gravity and calorific value
are presented in Fig. 2-7.

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 MPT-2013

matter increase from 19.08% to 21.75% and

Fig. 2: Proximate & Ultimate Analysis of
Shattered Fraction after Breakage of Sample
“A”
19.05% to 21.35% respectively for coal sample
A and coal sample B. There is improvement in
both free swelling index (CSN) as well as caking
index in -12.5 mm size fraction, swelling index
has increased from 1.5 to 4.5 in both cases,
whereas caking index has increased to 18 & 19
from feed value of 16 of both coal sample. There
is also marked improvement in calorific value
of -12.5 mm size fraction.
This may be due to the reduction in ash
content, improvement in volatile matter and
possibly because of enrichment of vitrinite and
liptinite macerals in small coal size fraction.

Fig. 3: Proximate & Ultimate Analysis of

Shattered Fraction after Breakage of Coal
Sample B
It is visible from Fig. 2 & 3 and Table 3 & 4 that
there is good reduction in ash content in both
coal samples A & B from the feed coal. In coal
sample A, ash % has reduced from 24.30 to 18.07 Fig. 4: HGI & Ash % of Shattered Fraction &
and in coal sample B, from 27.76 to 21.71. In – Feed of Samples
38+12.5 fractions ash content has content has
reduced slightly, whereas in other two fraction
the ash content has increased from feed coal.
This may be due to fact that during fracturing
of coal more carbonaceous part of the coal may
has retained in smaller size fractions resulting
in low ash content.
Fig. 4 depicts that -12.5 mm fraction shows Fig. 5: CSN & VM% of Fractions and Feed
higher HGI suggesting that this fraction is soft Samples
compare to other fraction, this may be due to
the enric hed with higher c arbonac eous
substance.
Variation of free swelling index with volatile
matter and ash with caking index for each size
fraction of both coal samples is shown in Fig. 5
& 6. It can be noticed that there is increase in
volatile matter from feed coal sample in -12.5 Fig. 6: Caking Index & Ash% of Fractions &
mm size fraction for both coal samples. Volatile Feed Samples

107

Fig. 7: Gross Calorific Value of Different
Fractions of Coal Samples & Feed
4. Conclusions
Study revealed that there is marked
improvement in basic characteristics of coal,
when larger size of coal subjected to drop test,
in particular, ash content, volatile matter
content, free swelling index, calorific value and
hardgrove grindabilty index of both coal
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108
MPT-2013
samples in below 12.5 mm size. This may
suggest that coal characteristics may changed
during transportation, loading, handling when
larger sizes of coal fragments in to smaller sizes,
which may have better characteristics than
larger sizes of coals.
References
ASTM D440-86, Standard Test Methods of Drop
Shatter Test for Coal.
IS 1350 Part 1 – 1984 (Reaffirmed 1996) Methods
of Test for Coal and Coke Part 1 Proximate
Analysis
IS 1353: 1993, Methods of Test for Coal
Carbonization -Caking Index, Swelling
Number and (LT) Gray-King Assay
IS 4433: 1979 (Reaffirmed 1994), Methods for
determination of Hardgrove
Grinadability Index of coal
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

High Energy Milling of Boehmite: Changes in Particulate

Characteristics

T.C.Alex1*, Rakesh Kumar1, S.K. Roy2 and S.P. Mehrotra3

1
Metal Extraction & Forming Division, CSIR-National Metallurgical Laboratory,
Jamshedpur-831007, India
2
Metallurgical and Materials Engineering Department, Indian Institute of Technology
Kharagpur-721302, India
3
Materials Science and Engineering, Indian Institute of Technology Gandhinagar-382424,
India

Abstract

Changes in particulate characteristics of boehmite during high energy milling/ mechanical

activation (MA) carried out in a planetary mill is the theme of this paper. Boehmite used in the
study, prepared by thermal dehydroxylation of gibbsite, has been characterized by a monomodal
size distribution with a median size (d50) of 110 mm, and large BET specific surface area (264 m2/g).
Keeping other parameters constant, the extent of activation has been varied by changing the
milling time (0 to 240 min). High impact forces prevailing in the mill has resulted in changes in the
particulate characteristics such as size reduction, changes in specific surface area etc, and structural
disordering. With the progress of milling, size reduction ceases and particle aggregation sets in.
BET specific surface area has anomalously decreased during milling. Analysis of such changes
during MA is described in this paper.
Keywords: boehmite, mechanical activation, particulate characteristics, specific surface area,
pore size distribution
leaving other associated minerals in the residue.
1. Introduction
Less reactive monohydrates need higher
Bayer process of alumina production continues temperature and alkali concentration for their
to remain unchallenged since its inception, over dissolution; equation (1) represents the
more than a century ago. In this process, dissolution of boehmite:
aluminium minerals (gibbsite [ã-Al(OH) 3],   AlOOH ( s )  NaOH ( aq )  Na  Al( OH )41( aq ) (1)
boehmite [ã-AlOOH] and diaspore [á-AlOOH])
High energy milling of monohydrate minerals
in bauxite ore are selectively digested in hot
of Al are being tried to enhance their reactivity,
concentrated caustic solution in the first step,
and thereby increasing its leachability in
caustic solution (Pawlek et al., 1992, Taskin et
* Correspending Author:T.C. ALEX
Metal Extraction and Forming Division, CSIR-National
al., 2009). Changes in particulate characteristics,
Metallurgical Laboratory, Jamshedpur-831007, India which influence the reactivity of materials
Contact No.: +91 6572345042; Email: tc_alex@yahoo.com during high energy milling, are generally not

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highlighted. This paper specifically focuses on deduced from the PSD is ~0.1 m2/g. BET specific
the changes in particulate characteristics of a surface area, on the other hand, has been found
high surface area boehmite during high energy to be exceptionally large, ~264 m2/g compared
ball milling. to that reported in many studies (~1 m2/g). Such
a large difference is attributed to the difference
2. Materials and Methods in the preparation process. Most of the low
2.1. Boehmite surface area boehmites described in earlier
studies have been prepared by hydrothermal
Details of the preparation and characterization
methods whereas boehmite used in this study
of boehmite used in this study have been
has been prepared by thermal decomposition
reported earlier [Alex et al., 2013]. Detailed
of gibbsite. Constitutional water released
characterisation using X-ray diffraction (XRD),
during thermal decomposition of gibbsite
Fourier Transform Infrared (FTIR) and thermal
creates large number of slit shaped pores, as
analysis studies has shown that the test sample
shown in Fig. 1, for their exit and thereby
is phase-pure boehmite.
resulting in a highly porous boehmite. XRD
2.2. Mechanical Activation (JCPDS No. 83-2384) and FTIR studies have
A batch type planetary mill (Pulverisette P6, shown that the synthesized material is phase
Fritsch GmbH, Germany) has been used for pure boehmite.
mechanical activation (MA). Milling conditions
are: ball to powder ratio =30:1, rotational speed
=400 rpm, milling time 0-240 min.
2.3.Characterization
Particle size distributions (PSD) of milled and
unmilled boehmite samples have been
determined using a particle size analyzer based
on laser diffraction (Model: Mastersizer,
Malvern, UK). Micromeritics ASAP2020 surface
area analyser has been used to measure the BET
specific surface area and pore size distributions.
Fig. 1: SEM micrographs of boehmite showing
Geometric specific surface area has been
slit like pores on the surface
deduc ed from the PSD distribution.
Morphological features are studied using a 2.3. Particle size distribution of milled
scanning electron microscope (SEM) (Model: boehmite
840A, Hitachi, Japan). Particle size data of milled boehmite obtained
from the sizer are presented in Fig. 2 in terms of
3. Results and Discussions
reduction ratio of median size; i.e. the ratio of
3.3. Boehmite used median size at any milling time, d (50, t) and
Boehmite used in this study has been found to median size of unmilled sample, d(50, 0) is plotted
as a function of milling time. High milling
have a monomodal distribution with a median
efficiency of planetary milling is evident in Fig.
size, d 50 of 110 mm. Other charac teristic
2; particle size (median size) shows ~60 times
diameters, d10 and d90 are 77 mm and 153 mm, reduction in just 15 min of milling. Beyond 15
respectively. Geometric specific surface area min of milling, however, the reduction ratio is

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seen to increase, indicating coarsening of To understand the anomalous decrease in

particles; such coarsening is ensuing from specific surface area, various milled samples
particle aggregation on account of the intense have been c harac terised in terms of N 2
particle-particle interactions. During high adsorption at liquid N2 temperature. Nature of
energy milling, especially in dry operations, adsorption isotherms (not shown here) has been
suc h aggregation/agglomeration is quite found to be different for the milled sample; such
possible (Juhasz and Opoczky, 1990). c hanges reflec t changes in the pore
1
characteristics. Detailed analysis of these
reduction ratio (median size)
adsorption isotherms has been carried out using
BJH method (Barret et al., 1951). Pore size
d(50,t)/d(50, 0)

distributions of milled samples and unmilled

0.1
0.01
0 50 100 150
Milling time, min
Fig. 2: Variation of size reduction ratio of with
milling time
3.5. Specific surface area and pore size
Geometric specific surface area of boehmite
milled for different durations of time along with
that of unmilled sample is presented in Table-
1.There is an initial increase followed by a
decrease, a trend just reverse that of particle
size reduction as it an inverse function of PSD.
BET specific surface area of milled boehmite is
also included in Table-1 to have a comparison
samples estimated by BJH method are presented
as cumulative distribution in Fig. 3. It can be
seen that majority of the surface area of
200 250 unmilled boehmite is from micropores having
size < 5 nm. The average pore diameter is found
to be around 3 nm. As the milling progressed, a
decrease in the pores having size < 5 nm and a
consequent decrease in specific surface area is
observed. Contribution of bigger pores towards
surface area has, however, been notic ed.
Consequently, the average pore diameter has
increased to ~13 nm after 240 min of milling.
This indicates that the decrease in specific
surface area during milling results mainly from
the annihilation of pores having size < 5 nm.
300

with the geometric specific surface area. BET 2 nm 4 nm 22.5 nm

250
Cum. pore area, m /g

specific surface area, as shown in Table -1, has

2

Milling time, min

200 0
continuously decreased with milling time 15
instead of a typical increase with decrease in 150 120
240
particle size; such a significant reduction in 100
specific surface area cannot be accounted by 50
particle aggregation alone, inferred from
particle size analysis data (Fig. 2). 1 10 100
Table 1: Variation of specific surface area of Pore size, nm
boehmite with milling time Fig. 3: Cumulative pore area of boehmite
Milling Specific surface milled for different time
time, min area, m 2 /g
Geometri BET
c 3.3. Morphological Features
0 0.1 264.1
15 2.7 201.2
30 2.6 188.9 To understand the extent of particle aggregation
60 2.4 143.1
120 2.2 115.1
inferred from PSD and pore size analysis,
240 2.1 67.6 changes in the morphological features under

111

the influence of planetary milling have been
studied using a SEM; SEM micrographs of
particles milled for 3 min and 60 min and are
presented in Fig. 4 (a) and Fig. 4(b), respectively.
Disjointing of the platelets (of initial unmilled
boehmite) oc c urs during early stages of
milling. Images at higher magnification show
smaller particles sticking to the larger particles
even for 3 min milled samples as seen in Fig.
4(a). As the milling time is increased to 60 min,
the smaller particle sticking to the bigger ones
diminishes almost completely, and aggregation
of smaller elongated particles is observed in the
sample [Fig. 4(b)]. Such severe aggregation is
responsible for the annihilation of micropores
and decrease in specific surface area, in turn.
(a) (b)
Fig. 4: SEM images of milled boehmite: (a) 3
min (b) 60 min
2.3. Reactivity
Reactivity, in general, is synonymous with
specific surface area; it increases as the specific
surface area increases while a decrease occurs
when specific surface area decreases. In spite of
the anomalous decrease in BET specific surface
area, it is observed that that the reactivity of
boehmite in terms of alkali dissolution and
thermal transformation (details are not covered
here) increases with the milling time. It is the
struc tural c hanges suc h as inc rease in
microstrain, dec rease in microc rystallite
dimension etc. (not detailed here) that are
responsible for the enhanced the reactivity;
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structural changes offset (and surpass) the effect
of 75% reduction in specific surface area.
3. Conclusions
Conc lusions drawn from the study is
summarised below:
 Sharp size reduction in early stages of
planetary milling shows high milling
efficiency
 Aggregation of particles as a result of
particle-particle interactions
 Anomalous decrease in BET specific surface
area of boehmite with milling time
 Changes in pore characteristics leads to the
decrease in specific surface area
 Despite the anomalous decrease in specific
surface area, reactivity increases with
milling
References
Alex, T. C., Kumar, R., Roy and S. K., Mehrotra,
S.P., 2013. Leaching behaviour of high
surface area synthetic boehmite in
NaOH solution. Hydrometallurgy. 137,
23–32.
Barret, E. P., Joyner, L. G. and Halenda P. P., 1951.
The determination of pore volume and
area distributions in porous substances.
I. Computations from nitrogen isotherms.
J. Am. Chem. Soc. 73, 373-380.
Juhasz, Z. and Opoczky, L., 1990. Mechanical
Ac tivation of Minerals by Grinding:
Pulverizing and Morphology of Particles.
Akademiai kiado, Budapest.
Pawlek, F., Kheiri, M. J. and Kammel, R., 1992.
The leaching behaviour of bauxite during
mec hano-c hemic al treatment, in:
Cutshall, E. R. (Ed.), Light Metals. The
Minerals, Metals & Materials Society,
Warrendale, US. 91-95.
Taskin, E., Yidiz, K. and Alp, A., 2009. Direct
alkaline leac hing of mec hanic ally
activated diasporic bauxite. Miner. Metall.
Process. 26(4), 222-225.
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GRAVITY SEPARATION

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Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

A Simple Laboratory Alternative to Large Scale Jigging Tests

Philip Thompson*
Senior Mineral Processing Advisor,
Dawson Metallurgical Laboratories—FLSmidth, Inc.
7158 S. FLSmidth Drive
Midvale, Utah 84047-5559 USA
philip.thompson@flsmidth.com

Abstract
Jig testing is a widely accepted method for determining the amenability of an ore to gravity
separation at relatively coarse sizes of up to 25 mm. However, this type of test often requires a
relatively large sample size of up to 500 kilograms or more. This sample requirement can be
problematic for new projects in the exploration and early development stage when only limited
amounts of expensive drill core are available. A relatively simple laboratory test using
approximately 200 individual pieces of suitably crushed sample will be described. The procedure
usually requires less than 5 kilograms of representative sample and measures the specific gravity
of each numbered piece using a simple “Jolley” balance. The “Jolley” balance data is then corrected
against the actual specific gravity using the LeChatlier flask method. The corrected data is used to
construct a yield curve graph of weight vs. specific gravity. Several examples of this method are
provided for Barite ores and a comparison of the yield curve with an actual operating plant are
provided.
1. Introduction
Gravity testing coarse samples of Barite, iron requires equipment with a minimum bed
ore, or coal with particle sizes greater than 12.5 surface area of 650 mm2 and a continuous test
millimeters is usually limited to either heavy can often require up to 500 kilograms or more
liquid — heavy media techniques or continuous of sample. These relatively large test units are
jigging techniques. Heavy media or jig testing required to ensure that the three principles of
is preferred due to the toxic nature of several jigging, namely differential acceleration,
organic heavy liquids and the limited specific hindered settling, and consolidated tricking, are
gravity ranges of the new inorganic heavy met on the large particles to be tested.
liquids. Heavy media testing usually requires a An alternative to the large scale expensive
large scale continuous test unit to keep the media jigging tests was developed by Dawson
in suspension and this in turn requires large Metallurgical Laboratories to evaluate the
amounts of sample. Jig testing of coarse material response of samples from several Barite
exploration projects. Limited amounts of
* Correspending Author: Philip Thompson*
expensive drill core were available for this work
Senior Mineral Processing Advisor,
Dawson Metallurgical Laboratories—FLSmidth, Inc. and full scale jigging tests were not an option.
7158 S. FLSmidth Drive The alternative technique developed consisted
Midvale, Utah 84047-5559 USA of specific gravity determinations of many
philip.thompson@flsmidth.com

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individual particles and the construction of a
product yield curve from these individual
particle measurements.
2. Test procedures and materials
Only two pieces of laboratory equipment are
required for the alternative technique—a
“Jolley” Balanc e for measurement of the
apparent specific gravities of individual sample
pieces, and a Le Chatlier specific gravity
volumetric flask for accurate determination of
the true specific gravity of the pieces. A
schematic of the “Jolley” Balance is presented
in Figure 1.
The test procedure consists of crushing a
representative sample, usually 10 to 20
kilograms, to an appropriate jig feed size,
usually minus 25 mm. It should be emphasized
that the appropriate weight of sample to be
crushed will be determined by appropriate
sampling protocols The 1.7 mm (10 Tyler mesh)
material is screened off and, depending upon
the weight on minus 10 mesh, this fraction can
be tested separately by spirals, or discarded
depending upon its specific gravity. Two
hundred (200) individual pieces of +1.7 mm
sample are then selected at random and
numbered from 1 to 200 with a magic marker
or other suitable waterproof ink. The total
weight of these selected pieces is approximately
2 kilograms and each individual piece usually
weighs between 3 and 15 grams. The apparent
specific gravity of each piece is then determined
using the “Jolley” Balance. The 200 pieces are
gravity due to the fact that the piece may not
be c ompletely wetted throughout. This
correction factor varies from approximately
1.00 to 1.09 as indicated in Figure 2.
Weight in Air Weight in Water
Balance Balance
Fishing line Fishing line
sample sample
Beaker with water
Beaker with water
Figure 1. Schematic of “Jolley” Balance
3. Calculations and data manipulation
The data obtained by the procedure described
in the previous section is used to generate a
graph of product yield vs. product specific
gravity using the apparent specific gravities
calculated from the “Jolley” Balance. The
apparent specific gravity is the weight of
sample piece in air divided by water volume
displaced (sample weight in air minus sample
weight in water). These apparent specific
gravities are then correc ted against the
LeChatlier true specific gravities by the factor
illustrated on the next page.
Specific Gravity Correction Factor
Le Chatlier/Jolley Balance
1.10
Correction factor, Le Chatlier/Jolley Balance

then oven dried and separated in groups of 1.08

similar specific gravity (usually 20 per group),

1.06
the group is pulverized and the true specific
gravity determined using a Le Chatlier flask 1.04

with a kerosene displac ement fluid. A R² = 0.7436

1.02
correction factor of Le Chatlier vs. “Jolley”
Balance specific gravity is then applied to the 1.00
2.0 2.2 2.4 2.6 2.8 3.0 3.2 3.4 3.6 3.8 4.0 4.2 4.4
20 pieces in the corresponding group. It should Specific Gravity by Jolley Balance, gm/cc

be noted that the apparent specific gravity by Figure 2. LeChatlier vs.“Jolley” Balanc e
“Jolley” Balance is lower than the true specific Correction

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A summary of the calc ulations and data
manipulations are presented in the following
bullets.
 Calculate the specific gravity of each
individual piece based upon the weights
in air and water.
 Arrange the data in descending order of
specific gravity (highest to lowest).
 Calculate individual and cumulative
weights, cumulative weight percentage of
all samples, individual sample volumes,
and cumulative volume of all samples.
 Apply the LeChatlier/”Jolley” Balance
correction factor to every specific gravity
value using the appropriate factor for each
group. Adjust the weight in water and
the corresponding volume for each piece
in accordance with the corrected specific
gravity.
 Re-arrange the adjusted data in
descending order of corrected specific
gravity.
 Calculate the cumulative product specific
gravity by dividing the c umulative
product weight by the cumulative product
volume for the entire data set of 200
samples.
 Graph the cumulative product yield vs. the
cumulative corrected (true) specific gravity.
Table 1: Variation of Product Yield with
Sample Population
Database Product Yield, wt%
# of pieces at 4.2 g/cc
100 66.3
200 63.2
300 63.1
Product yield curves for three different Barite
ores are illustrated in figure 3 on the following
page. Inspection of these results indicate that
samples A and C are not suitable for coarse (25
mm) jigging due to low product yields at Barite
market specifications of 4.2 gm/cc specific
gravity. These two samples were exploration
drill core from a potential Barite deposit in Asia.
Sample B was crushed ore feed to an operating
Barite jigging plant in North America. This
sample has a relatively high 4.2 gm/cc product
yield of 63% of plant feed. The laboratory-
generated yield curve for sample B was
compared with actual jig plant performance
over a period of several days. Results, presented
in figure 4, indicate excellent agreement
between plant performance and laboratory
results.
Yeild Curves for 3 Barite Ores

100
4. Results 90

Several preliminary tests were performed to 80

63.0% at
Product Yield, % of Test Feed

70 4.2 gm/cc
determine the minimum number of individual
60
sample pieces that would be required. Sample 50 Sample A

populations of 100, 200, and 300 were tested 40

Sample B
Sample C
against the procedure described in the previous 30 Barite Product Specification
32.5% at
sections. Results indicated that a significant 20
13.1% at
4.2 gm/cc
4.2 gm/cc

10
difference in the product yield at 4.2 gm/cc 0
specific gravity was obtained between 100 and 3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.0 4.1
Product Specific Gravity, gm/cc
4.2 4.3 4.4 4.5

200 pieces, but almost no difference was noted

between 200 and 300 pieces, therefore a sample
Figure 3: Yield Curves for Three Barite Ores
population of 200 pieces was chosen for all
further testing. These results are presented in
table 1 below.

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5. Discussion Comp arison of Laboratory Generated Yeild Curve with Actual Plant
Production
The relatively simple laboratory procedure 100

described in this paper has indicated excellent 90

potential as a substitute for large scale jigging 80

Product Yield, % of Test Feed

70
tests of coarse heavy minerals up to 25 mm in 60

size. The technique requires approximately 2 50

kilograms of sample for the actual test and is 40

30
therefore ideally suited to projects where only 20 Lab Generated Yeild Curve

limited sample is available. The relatively low 10

Barite Prod uct Specification
Actual Plant Production Data

sample weight requirements allow this 0

3.3 3.4 3.5 3.6 3.7 3.8 3.9 4.0 4.1 4.2 4.3 4.4 4.5
Product Specific Gravity, gm/cc
technique to be used for ore variability testing.
It is the author’s opinion that this procedure Figure 4: Comparison of Laboratory Yield Curve
could be used to evaluate the gravity separation with Plant Production
potential for other high specific gravity material Acknowledgements
such as iron ore if the specific gravity can be The author wishes to thank FLSmidth Inc. for
correlated with the iron content. their permission to publish this paper.

*******

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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar
Misplacement of Particles in Liquid Solid Fluidization

Alok Tripathy1, S.K. Biswal1 and B.C. Meikap2

1
CSIR-Institute of Minerals and Materials Technology, Bhubaneswar 751013, Odisha, India
2
Indian Institute of Technology, Kharagpur 721302, West Bengal, India

Abstract
Liquid solid fluidization principle is used for particle separation in mineral processing based on
size, shape and density. Different particles have different terminal velocities which affects the
expansion of these particles under the action of liquid velocity in liquid solid fluidization. Generally
heavier particles report to bottom of the bed and lighter particles report to top of the bed. However,
due to wide size distribution of feed layer inversion happens which allows lighter particles to
report to bottom of column and heavier particles to report to top of column. This phenomenon
misplaces the particles. In addition to this presence of near gravity materials and flaky particles
also contribute to the misplacement of particles. The present work aims at understanding the
misplacement of particles in liquid solid fluidization. In present work synthetic mixture of high
grade iron ore and quartz was used to study the misplacement of particles in separation. For the
quantification of particle misplacement an index was introduced called misplacement index.

Keywords: Fluidization; layer inversion; bed expansion; misplacement index.

Mineral beneficiations can be performed by

1. Introduction
India is blessed with different mineral resources
like iron ore, chromite, manganese etc. These
minerals contribute substantially to the
countries economy and growth. In the last
decade or so there is rapid growth of mineral
beneficiation especially in the field of iron ore
beneficiation. The demand of high grade ore is
increasing day by day bec ause of rapid
industrial growth. However, supply of high
grade ore is not sufficient as per the demand and
this necessities the use of low grade ore after
beneficiation.
* Correspending Author: Alok Tripathy, Mineral Processing
Department, CSIR-Institute of Minerals and Materia ls
Technology, Bhubaneswr 751013
Email: atripathy@immt.res.in , altriatl@gmail.com
gravity separation, magnetic separation,
flotation, selective flocculation etc. However,
among all the processes available gravity
separation is the most preferred method because
of it’s low cost of operation and easy in handling.
Gravity separators use the difference in specific
gravity of different minerals for the particle
separation. Gravity separation c an be
performed using jig, spiral, tables, flotex density
separator, allflux mineral separators, dense
medium separators etc. (Das, et al., 2009; Das et
al., 2007; Mishra and Tripathy 2010; Panda, et
al. 2012; allmineral.com) Selection of the
separators largely depends on liberation
characteristics of the minerals in an ore.
Generally Indian iron minerals are liberated at
finer size fraction. Spiral, flotex density
separator, and allflux mineral separators are few
such types of

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equipment which can be used for beneficiation Synthetic mixture of high grade iron ore
of finer size particles. Among these separators particles and high grade quartz particles were
flotex density separator and allflux mineral used for the present study. The particle size of
separators uses the principle of fluidization for iron ore sample used was -150+75 micron and
separation of particles. that of quartz particles was -100+75. The true
density of the iron ore sample used was 4.6 and
Use of fluidization princ iple in mineral
that of the quartz was 2.63. For eac h
processing is gaining importance day by day.
experimental run pressure drop and expanded
Wet beneficiation method uses liquid-solid
bed height was noted down. Initially
fluidization principle for particle separation.
fluidization of only iron ore particles were
These liquid-solid fluidized bed separator uses
carried out; then fluidization of only quartz
physical characteristics of particles i.e., size,
particles was carried out. After the two initial
shape, and density for beneficiation of ores.
experimental runs all experiments were
Extensive research had been carried out to
performed using synthetic mixtures of iron ore
understand liquid-solid fluidization (Asif, 1997,
and quartz in weight ratio of 7:3 (iron ore :
2002; Barghi, et al. 2003; Funamizu and
quartz). For understanding the partic le
Takakuwa 1996; Moritomi et al., 1986,
misplac ement in every experiment with
Mukherjee and Mishra 2007; Qian, et al., 1993;
synthetic mixture samples were collected at five
Tripathy et al., 2013). However, the
different points along the axis of the column at a
understanding of particle misplacement in these
given superficial velocity. The collected sample
fluidized bed density separators is still limited,
was then analyzed for iron ore and quartz content.
because the ore feed to these fluidized bed
separators have wide size distribution, wide
density distribution and are highly irregular
shape particles. A liquid-solid fluidized bed
density separator is considered to be efficient if
it separates particles based on their difference
in specific gravity.
The aim of the present study would be to
understand the misplacement of particles in a
fluidized bed separator at a fundamental level
and quantify this misplacement. In addition to
this effect of different parameters on the
misplacement of particles would also be studied. Fig. 1: Schematic diagram of experimental setup
2. Materials and Methods (Tripathy et al. 2013)
The schematic diagram of the experimental set- The hydrodynamics of mixing and segregation
up is shown in Fig. 6. The experimental set-up were normally quantified with mixing index and
consists of a fluidization column of 100 mm segregation index. However these indexes are not
diameter having a plenum chamber. The plenum effective in quantifying the particle misplacement
chamber is filled with glass balls for uniform in fluidized bed density separator. When liquid
distribution of the water into the column. The solid fluidized bed is used as density separator
pressure difference in the fluidized column was in mineral processing, it is desired that lighter
measured using mercury manometer and particle should be completely segregated from
flowrate of the water was measured using heavier partic les. Two extreme state of
rotameter. A centrifugal pump was used for segregation may occur in such density separators
pumping the water (Tripathy et al. 2013). depending on the particle sizes of the lighter and
heavier particles as given below:
120

a) extreme stages. The indexes mentioned above
gives different index values for When all the
heavier particles are at the bottom and all
the lighter particles are at the top part of the
fluidized bed column.
b) When all the lighter particles are at the
bottom and all the heavier particles are at
the top part of the fluidized bed column
(complete stage of layer inversion).
The second type (i.e. b) of extreme segregation
occurs when size of the lighter particles are
sufficiently larger than the heavier particles. The
stage of completely mixed fluidized bed is an
intermediate stage between these both the
extremes of segregation mentioned above. This
sometimes does not give clear picture of the
particle misplacement. Because of which in
present work for quantification of particle
misplacement an index called “misplacement
index” was proposed. The misplacement index
can be calculated as given below:
x  x LP
I Misplaceme nt  UP (1)
x CM
Where IMisplacement is misplacement index, xUP is the
fraction of component for which misplacement
is calculated in upper part of fluidized bed, xLP
is the fraction of c omponent for whic h
misplacement is calculated in lower part of
fluidized bed and x CM is the frac tion of
c omponent for whic h misplac ement is
calculated at completely mixed condition.
Once the misplacement index is measured using
above equation its value varies between –(1/ xCM)
to (1/ x CM ); and during completely mixed
condition misplacement index will be zero.
Separation of particles are better if the index
value is away from zero i.e. misplacement index
value may be positive value or negative value
but it should be away from the zero.
3. Results and Discussion
3.1. Particle hydrodynamics study
Initially general hydrodynamics study of the
fluidized bed was carried out. This study
includes the fluidized bed expansion and
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MPT-2013
pressure drop across fludized bed. Fig. 2 shows
the pressure drop across the fluidized bed at
different superficial velocity. From Fig. 2 it was
observed that all the plots follow the standard
graph of fluidization. It was also observed from
Fig. 2 that pressure drop for iron ore bed
particles was more compared to the quartz and
synthetic mixture bed of particles. The result is
natural as iron particles are heavier compared
to others. Yet another observation from Fig. 2
was that the pressure drop across synthetic
mixture (iron ore + quartz) was in between the
pressure drop across iron ore and quartz. The
order of pressure drop across the fluidized bed
for different materials is given below.
Iron ore > Synthetic mixture (iron ore + quartz)
> Quartz
12000
10000
Pressure drop, N/m2
8000
6000
4000
Iron Ore
2000 Quartz
Iron Ore + Quartz (70:30)
0
0 0.0001 0.0002 0.0003 0.0004 0.0005 0.0006 0.0007 0.0008
Superficial velocity, m/s
Fig. 2: Pressure drop across fluidized bed at
different superficial velocity of water
Bed expansion is one of the important
parameter required to be studied to understand
the particle motion inside the fluidized bed
column. Fig. 3 shows the variation in expanded
bed height at different superficial velocities.
From Fig. 3 it was observed that quartz particles
expand more compared to synthetic mixture
and iron ore particles. The order of fluidized bed
expansion for different materials is given below.
Iron ore < Synthetic mixture (iron ore +
quartz) < Quartz

150
125
Expanded bed height, cm
100
75
50
25
0 0.03
Fig. 3: Fluidized bed expansion at different
superficial velocity of water
Samples were collected from five different points
along the axis of the fluidized bed column and
solid concentrations were measured. The axial
solid concentration profile of fluidized bed for
synthetic mixture is shown in Fig. 4 for different
flowrates of water. From Fig. 4 it was observed
that there is very wide variation of solid
concentration along the axis of the column The
top of the c olumn was having a solid
concentration of around 2.9 % by wt. and bottom
of the column was having a solid concentration
of around 49.8 % by wt. at flow rate of 190 lph.
This wide change in solid concentration indicates
there exist different zones of separation inside
the fluidized bed column. Broadly these zones
can be classified as free zone at top of the column
and hindered zone at bottom of the column. In the
free zone motion of the particles are hardly
affected by the other particles around; however,
in the hinder zone motion of particles are strongly
affected by the presence of other particles around.
80
70
Solid Concentration, wt. %
60
50
40
30
20
10
0
0 20
Fig. 4: Solid concentration profile of the
fluidized bed column
MPT-2013
3.2. Particle misplacement study
The values of fraction of iron ore or quartz
present in upper and lower part of fluidizing
column is required for understanding the
misplacement of the particles. Because of which
the sample collected at different points along
the height of the column were analysed for the
Iron Ore
Quartz
amount of iron ore and quartz present. Fig. 5
Iron Ore + Quartz (70:30)
shows the variation of iron ore and quartz
content along the height of the fluidized bed
0.06 0.09 0.12 0.15
column. From Fig. 5 it was observed that for
Superficial velocity, cm/s
every case (Fig. a, b, c, d) as the bed height
increases amount of iron ore decreases and
amount of quartz increases. It was also observed
that there exists a point where concentration of
both iron and quartz is 0.5 (50%). It is also
interesting to note that plots showing
concentration of iron ore and quartz crosses
each other at this point every time. From Fig. 5
it was also observed that at any given point of
height both iron ore and quartz are present. This
indic ates misplac ement of partic les is
happening. Fig. 5 shows that there exists appoint
aling the height of the column where bed of
particles are in completely mixed state.
These plots shown in Fig. 5 give an indication
that either misplament is happening or not;
however, they do not provide any quantification
of misplacement. For quantification of the
misplacement of particles misplacement index
was calculated taking iron ore as the desired
component from the binary mixture of iron ore
and quartz. Fig. 6 shows the variation of
misplacement index with the overflow height.
The overflow height is the column height above
which all particles were considered as overflow
190 lph 150 lph
materials and below that point all particles were
110 lph 70 lph
considered underflow material. It was observed
that all the values of index are negative. It was
also observed that with the increase of overflow
height the misplacement index value increases
or in other wards the index values are more near
to zero (as all the misplacement index values
40 60 80 100 120 are negative). This means as the overflow height
Bed height, cm
is less (from bottom of the column) particle
separation is better and misplacement is less
with respect to iron ore.
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120 120

100 100

80 80
Percentage

Percentage
60
a Iron ore %
60 b Iron ore %
Quaetz % Quaetz %
40 40

20
20

0
0
0 20 40 60 80 100 120
0 20 40 60 80 100
Bed height, cm
Bed height, cm

120 120

100 100

80 80
Percentage

Percentage

60 c Iron ore %
60 d Iron ore %
Quaetz % Quaetz %
40 40

20 20

0 0
0 10 20 30 40 50 60 70 0 5 10 15 20 25 30 35 40
Bed height, cm Bed height, cm

Fig. 5: Variation of iron ore and quartz concentration with the bed height for different superficial
velocities a) 0.0672 cm/s, b) 0.0531 cm/s, c) 0.0389 cm/s, and d) 0.0248 cm/s

-0.7 increases the misplacement index values are

-0.75
0 20 40 60 80 100 120
more near to zero. This indicates at lower
-0.8
superficial velocity particle separation is better
or misplacement is less compared to at higher
Misplacement Index

-0.85

-0.9
superficial velocity.
-0.95
-0.7
-1
0 0.01 0.02 0.03 0.04 0.05 0.06 0.07 0.08
-1.05 -0.8

-1.1
-0.9
Misplacement Index

-1.15
Overflow height, cm -1

-1.1
Fig. 6: Variation of misplacement index with
respect to overflow height -1.2

-1.3
Similar to Fig. 6 the variation of misplacement
index with the change of superficial velocity was -1.4

shown in Fig. 7. The overflow height was Superficial Velocity, cm/s

maintained constant at 37 cm from the bottom

of the fluidized bed column. From Fig. 7 it was
Fig. 7: Variation of misplacement index with
observed that as the superficial velocity
respect to superficial velocity at constant
increases misplacement index increases. In this
overflow height of 37 cm from bottom of
case also all the misplacement index values are
column
negative. This means as the superficial velocity

123

3. Conclusion
A misplacement index was proposed in the
present study. It was found that the index was
suitable for quantifying the misplacement of
particles or separation of the particles. It was
also found that if the overflow collecting height
is less separation is better and misplacement is
less with respect to iron ore. It was also found
that at lower superficial velocity separation is
better and misplacement is less with respect to
iron ore.
Acknowledgement
The authors would like to gracefully
acknowledge the financial support given by
CSIR, New Delhi under the 12th five year plan
project scheme (Project. No. ESC – 0205) to carry
out this work. The authors would also like to
acknowledge Direc tor, CSIR-IMMT,
Bhubaneswar for giving permission to publish
this paper.
References
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fluidized bed, Chem. Eng. Technol. 20, 485–
490.
Asif, M., 2002. Predicting binary-solid fluidized
bed behavior using averaging approaches,
Powder Technol. 127, 226–238.
Barghi, S., Briens, C.L., Bergougnou, M.A., 2003.
Mixing and segregation of binary mixtures
of particles in liquid–solid fluidized beds,
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Das, A., Sarkar, B., Mehrotra, S.P., 2009.
Prediction of separation performance of
Floatex Density Separator for processing of
fine coal particles, Int. J. Miner. Process. 91,
41–49.
Das, S.K., Godiwalla, K.M., Panda, L.,
Bhattacharya, K.K., Singh, R., Mehrotra, S.P.,
*******
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2007. Mathematical modeling of separation
characteristics of a coal-washing spiral.
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84, 118–132.
Funamizu, N., Takakuwa, T., 1996. A minimal
potential energy model for predicting
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solid–liquid fluidized beds, Chem. Eng. Sci.
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Mishra, B.K., Tripathy, Alok, 2010. A preliminary
study of particle separation in spiral
concentrators using DEM, International
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Moritomi, H., Yamagishi, T., Chiba, T., 1986.
Prediction of complete mixing of liquid-
fluidized binary solid particles, Chem. Eng.
Sci. 41, 297– 305.
Mukherjee, A.K., Mishra, B.K., 2007.
Experimental and simulation studies on the
role of fluid velocity during partic le
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82, 211-221.
Panda, Lopamudra, Sahoo, A.K., Tripathy, A.,
Biswal, S.K., Sahu, A.K., 2012. Application of
artiûc ial neural network to study the
performance of jig for beneûciation of non-
coking coal. Fuel, 97, 151–156.
Qian, D., Wang, Z., Chen, G., 1993. On the
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Accepted in Press.
w w w. a l l m i n e r a l . c o m _ d e _ d o w n l o a d _
newsletter_Newsletter_dt_1204.pdf
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Segregation of Minerals in Floatex Density Separator – A Study

by Using Synthetic Mixture

Sharath Kumar Bhoja1*, Srijith Mohanan1, CRaghu Kumar1, S Mohan

Rao1,Ashok Kumar1,Shobhna Dey2 and Avimanyu Das2
1
Tata Steel Jamshedpur, 831001, Jharkhand, India
2
CSIR-National Metallurgical Laboratory, Jamshedpur, 831007, Jharkhand, India.

Abstract
Floatex density separator is a new generation classifier making use of different particle settling rates
to segregate particles based on size shape and density. To understand the process dynamics, various
studies have been carried out in floatex density separator while treating different minerals like coal,
silica, chromite and iron ore. Most of these studies have focussed on the application of this unit at
different scale of operation. For better control a deeper insight to understandthe separation phenomena,
one has to study the effect of process parameters like teeter water flowrate, bed pressure, pulp density
and feed rates on the segregation of minerals. Present study deals with thestudy on effects of these
process parameters on the partition of minerals. Synthetic mixture of magnetite and silica was used
for the experimentation in the floatex density separator and the results are analysed statistically to
understand the influence of these process parameters on partition of minerals. Further, main effects
has been analysed in terms of analysis of variance and regression analysis followed by study of
interactional effects byusing response surface plots. It is observed that in case of magnetite partition/
recovery, teeter water flow rate and bed pressure has played a vital role.

Keywords: Floatex density separator; advanced gravity separator, hindered settling, Fine particle
processing.
literature [Sarkar et al. (2008), Kumar et al.
1. Introduction
(2011), Tripathy et al. (2008)]. There
Floatex Density Separator (FDS) is an advanced areseveralpublished literature explaining
hindered settling classifier, also called as process dynamics incurred with respect to
counter-current and autogenous teetered bed classification as well as the concentration
separator, which makes use of particle settling operation and on its performance evaluation.
rates to segregate particles according to size, In the present study, an attempt has been made
shape and density. The basic working principle to understand the effect of process variables on
of FDS has been explained in detail in the segregation of minerals.
* Correspending Author: SHARATH KUMAR BHOJA, 2. Materials and methods
Manager, Mineral and Ferro Alloys Technology, Raw Material
and Iron Ma king Tech nology Group ,Ta ta Steel Ltd .,
2.1 Magnetite:
Ja msh edp ur- 83 1 0 07, INDIA. Co nta ct No.: + 91 About 600 kg of magnetite was processed
7763807445, E-mail:sharath.bhoja@tatasteel.com locally and the sample was beneficiated with

125
 MPT-2013

the scheme mentioned in Figure 1 to obtain the
maximum possible purity. The obtained
magnetic product from LIMS is the pure
magnetite sample (99.6 % purity when
measured using Davis Tube magnetic
separator) for subsequent use in the FDS. The
partial chemical analysisis tabulated in Table
1 While conducting experiments, the feed slurry
2.2. Silica
About 2 tons of heavy mineral sand tailings
was received from Sathankulam, Tamil Nadu,
India for the experimental work. The
representative sample analysed 99.5% Silica
when tested using heavy liquid; Bromofrom; of
density 2.86 kg/m3. This sample was then size
reduced to <1mm (100% passing); in the
laboratory roll crusher; which was used in the
entire experimental work. The partial chemical
analysis is tabulated in Table 2.
The size analysis of the magnetite and silica
sample is shown in Figure 2. The D80% passing
size of the magnetite is 300 µm and Silica is 297
µm. During material preparation the material
was made to pass through 1.0mm sieve to make
sure that the feed does not contain any particle
larger than 1 mm.
variables on classification performance. The
variables and their levels are given in Table 3.
Experiments were carried out using a lab model
Floatex Density Separator of 230 mm X 230 mm
X 530 mm size (Outokumpu make). The
schematic diagram of the experimental setup
used for the present study is shown in Figure 3.
was first pumped to the FDS at a desired flow
rate with the help of the pump while the
equipment was in operation. Samples from the
overflow and underflow streams were collected
after attainment of the steady stat only. The
samples from the overflow and underflow
streams were collected at steady state, dried,
weighed and analyzed for granulometry. The
results were then used calculate the Magnetite
recovery (%), Silica recovery (%). Regression
equations were developed for predicting the
response at different levels of variables by using
Design Experts®software. These equations were
then used to analyze the effect of process
variables, viz. teeter water flow rate, set point,
feed rate and pulp density.
Table 2: Chemical analysis of the silica sand
Constituent Weight (%)
SiO2 97.48
Na 2O 0.05
K2O 0.13
MgO 0.12
CaO 0.01
FeO 0.74
Specific gravity 2.6

F eed inlet
line

Floatex
Overflow
density
discharge
separator

Figure 2: Particle size distribution of Magnetite L

P
Feed slurry
tank
Injection
and Silica for the experiments
M

water
tank Underflo w
discharge

3. Experimental setup Injection

water line
Pump

Statistically designed experiments (2 4) were

Figure.3: Experimental set up of Floatex
carried out to investigate the effect of process
Density Separator

126
 MPT-2013

Table 3: Design of Experiments 4.2. Regression analysis

Sl No Variables
Level Regression analysis was carried out and the
Min Max
model equations to predict the performance in
1 Teeter water (lpm) 10 16
2 Bed Pressure (bars) 6.7 7.9
terms of recovery to underflow fraction (%)
3 Feed rate (kg/h) 100 120 were generated. Further,to understand the
4 Feed Pup Density(% sol) 30 50 interactional effect of the parameters, response
4. Results and Discussion surface graphs were plotted and analysed for
the interactional effect of significant parameter
The test results were analysedusing the on the responses.
statistical techniques to understand the effect Regression equation:
of each variable, their interactional effects and
the significant variables were ascertained. The
results of the statistical analysis are presented
in Figure 4 and the main findings are described
in the following sections.
4.1. ANOVA
4.3. Magnetite recovery
It can be observed from the Figure 4 that in case
of primary effects, the Teeter water and Bed Figure from 5 to 7shows the effect of teeter water
pressure has major influence on magnetite and bed pressure atdifferent level of pulp
recovery to underflow fraction whereas, for density and feed rate. From Figure 5, it may be
silica recovery the pulp density also has major observed that the maximum recovery was
influence. In the binary effect, Feed rate x Bed obtained by operating the floatex at lower
pressure is significant in case of Silica recovery teeter water and bed pressure. At this
to underflow. The order of significance for the condition, the hindrance to the settling particles
responses are shown below is muc h low and the voidage will be
high[Kumar et al (2011)]. Hence the higher yield
to under flow fraction is expected [Raghu et al
(2010b) Kumar et al (20011)].Gradually by
increasing the teeter water and bed pressure
the magnetite recovery to underflow fraction
decreases.
Design-Expert® Software
Factor Coding: Actual
Magnetite Recovery
76

60

X1 = A: BP 80
X2 = B: TW
Magnetite recovery(%)

Actual Factors 75
C: PD = 30.27
D: FR = 100.54 70

Figure.4.ANOVA results showing the 65

60

significance of variables 55

Main effects: 16

15

14 7.9

Magnetite rec overy: Teeter water > Bed Teeter water flowrate(lpm) 12
13

7.3
7.6

pressure
11 7.0

10 6.7 Bed pressure (bars)

Silica Recovery: Bed pressure > Teeter water >

Pulp density
Figure 5: Effect of teeter water flowrate and
Binary effects: bed pressure on Magnetite recovery at lower
Silica recovery: Bed pressure x Feed rate level of Pulp density and Feed rate.

127
 MPT-2013

Similarly Figure 6shows the interactional effect rate and pulp density levels (Raghu et al (2010a).
at intermediate level of teeter water and bed Basically the silica particle reporting here may
pressure. It may be noticed here that with be of coarser size whic h has reported to
increasing the feed rate and pulp density to underflowdue to higher settling velocity.More
c entre level the magnetite rec overy to over the bed formed in this condition is having
underflow fraction decreases. more coarser silica particles which results in
the lower bed density.
Design-Expert® Software
Factor Coding: Actual
Magnetite Recovery
76 Design-Expert® Software
Factor Coding: Actual
60 Silica Recovery
37.8049
X1 = A: BP 80
X2 = B: TW 4.47531
Magnetite recovery(%)

Actual Factors 75 50
X1 = A: BP
C: PD = 40.27 X2 = B: TW
D: FR = 120.00 70 40
Actual Factors

Silica recovery(%)
65 C: PD = 30.27
30
D: FR = 100.00
60
20
55
10

0
16

15

7.9 16
14
15
13 7.6
14
7.3
Teeter water flowrate(lpm) 12 13
7.90
11 7.0 7.60
Teeter water(lpm) 12
7.30
10 6.7 Bed pressure (bars) 11 7.00
10 6.70
Bed pressure(bars)

Figure 3.6: Effect of teeter water flowrate and

bed pressure on Magnetite recovery at Figure 8: Effect of teeter water flowrate and
intermediate level of Pulp density and Feed bed pressure on Silica recovery at lower level
rate. of Pulp density and Feed rate.

Design-Expert® Soft ware

Factor Coding: Act ual
Design-Expert® Software Silica Recovery
Factor Coding: Ac tual 37. 8049
Magnetite Recovery
76 4.47531
50
60 X1 = A: BP
X2 = B: TW
40
X1 = A: BP 80 Actual Factors
Silica recovery(%)

X2 = B: TW C: PD = 40.00
30
Magnetite recovery(%)

75 D: FR = 120.00
Actual Factors
C: PD = 50.00 20
D: FR = 138.92 70
10
65
0
60

55
16
15
16 14
7.90
15 13
7.60
14 7.9
Teeter water(lpm) 12
7.30
11 7.00
13 7.6
10 6.70
7.3 Bed pressure(bars)
Teeter water flowrate(lpm) 12
11 7.0

10 6.7 Bed pressure (bars)

Figure 9: Effect of teeter water flowrate and

Figure 3.7:Effect of teeter water flowrate and bed pressure on Silica recovery at middle level
bed pressure on Magnetite recovery at higher of Pulp density and Feed rate.
level of Pulp density and Feed rate Further from Figure 9 and 10 that by gradually
4.4. Silica recovery increasing the feed rate and pulp density
Figure 8to Figure 10shows the interactional towards higher level the plane representing the
effect of Teeter water and bed pressure on the interac tional effec t shifts downwards
silica recovery at different levels of feed rate indicating the lower recovery of the silica
and pulp density. It can be observed from Figure particles to underflow fraction. With higher
8that thehigher silica recovery to underflow feed rate the concentration of the particles in
fractionmay be obtained by maintaining low the floatex density separator increases with
bed pressure and low teeter water at lower feed magnetite concentration in the bed resulting

128
 MPT-2013

the bed density increase and building of silica

particles entering the underflow fraction. References
Das, A, Sarkar B, Biswas P, Roy S, 2009.
Design-Expert® Software
Factor Coding: Actual
Silica Recovery
Performance prediction of floatex density
37.8049

4.47531
50
separator in processing iron ore fines — a
X1 = A: BP
X2 = B: TW

Actual Factors
40
relative veloc ity approac h. Mineral
Silica recovery(%)

C: PD = 50.00
30
D: FR = 139.98

20 Processing and Extractive Metallurgy 118

10

0
(2), 78–84.
16
Kumar C R, M. Srijith a, Tripathy, S K,
15
14
7.90
Ramamurthy Y, Venugopalan T, Suresh N,
13

Teeter water(lpm) 12
11 7.00
7.30
7.60
Prediction of process input interactions of
10 6.70
Bed pressure(bars) Floatex Density Separator performance for
separating medium density particles.,
Figure 10:Effect of teeter water flowrate and International Journal of Mineral
bed pressure on Silica recovery at higher level Processing 100 (2011) 136–141.
of Pulp density and Feed rate. Raghu Kumar, C., Rama Murthy, Y., Tripathy,
5. Conclusions Sunil, 2010. Application of floatex density
For deeper understanding of process variables separator for Prec onc entration of
effect/impac t on segregation of mineral Chromite from COB tailings, TATA Search
particles in (terms of recovery) using FDS an 2010b.
experimental campaign was carried out using Raghu Kumar, C., Tripathy, Sunil Kr., Mohanan,
synthetic mixture of magnetite and silica sand. Srijith, Venugopalan, T., and Nikkam
The following are the important conclusion. Suresh, 2010. Evaluation offloatex density
1. Teeter water flowrate and bed pressure separator performanc e using silic a
are the main parameter from which the sand,Proceedings of the XI International
Magnetite recovery to underflow can Seminar on Mineral Proc essing
be c ontrolled whereas for silic a Technology (MPT-2010a),pp. 701–706.
recovery the pulp density also plays a Sarkar B, Das A, Roy S, Rai SK. In depth analysis
significant role. of alumina removal from iron ore fines
2. The silica recovery to underflow can be using teetered bed gravity separator.
brought down by operating the floatex Miner Process Ext Met (Trans Inst Min
density separator at higher teeter Metall C) 2008; 1:117.
water flowrate, bed pressure and feed Tripathy S.K., Mallick M.K., Singh V., Rama
rate. Murthy, Y., 2013. Preliminary studies on
Acknowledgements teeter bed separator for separation of
The authors are thankful to Tata Steel Ltd., manganese fines. - Powder Technology,
management for all the support, encouragement
and permission to publish the paper

*******

129
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Performance Evaluation of Ultra Fine Gravity Concentration

Circuit

Y.Rama Murthy*, Sunil K. Tripathy, Veerendera Singh, A. Ranjan and A.

Srinivsulu
Research and Development Division, Tata Steel Ltd., Jamshedpur - 831001, India
Chrome Ore Beneficiation Plant Sukinda -755018 Odisha, India

Abstract
The availability of high grade chrome ore resources in India is limited to Sukinda region of Odisha
state. Several beneficiation plants are operating in this region to beneficiate the low to medium
grade chrome ore. These beneficiation plants incorporate gravity concentration techniques for
the recovery of chromites values to make it suitable for different end user applications. The
performance of these gravity circuits need to be evaluated on timely basis so that they can perform
with peak efficiencies. Mineral engineers are required to modify the critical operating process
parameters on continuous basis which is very difficult and tiresome. Better control of grade and
recovery with minimum loss of value is the focus of such plants. In the present investigation the
results obtained on the performance evaluation studies carried out on a gravity concentration
plant, Sukinda has been discussed. Based on the systematic approach followed by analysis of the
data the performance of the circuit has been evaluated specifically in terms of SiO2. The results of
plant trials based on the above methodology has shown that the SiO2 in the ultrafine concentrate
has reduced to <4% from 6%.

Keywords: Chromite; chromitebeneficiation; gravity concentration techniques; characterization;

plant operating data bank.

1. Introduction
Chrome ore demand is driven by ferrochrome
market as ~95% of the chrome ore is used for
the metallurgical purpose. Two percent of the
demand comes from chemical industry and rest
from refractory and foundry industry. Stainless
steel is the largest consumer of ferrochrome and
as such a change in the dynamics of the
stainless steel industry has impact on the
ferrochrome industry. In the long run, in line
* Correspending Author: yrama.murthy@tatasteel.com
with expectation of increase in stainless steel
demand, demand for ferrochrome is expected
to increase. The consumption is expected to
reach ~11Mt by 2013 (Figure 1, 2) at a CAGR of
7% per annum. South Africa plays a significant
role in the world’s output of ferrochrome
contributing around 38% of the total in 2011.
India, the number three producer of chrome ore,
with only 1% of the global resources, has only
~17 years of production life left at the current
level of production (1).

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 MPT-2013

possesses the largest chromite deposit of the

country. The chromites of both SUB and BNIC
and elsewhere in India can be categorized as
hard massive, banded, disseminated, friable,
granular and lateritoid type depending on the
amount of gangue mineral and their textural
arrangements , Sahoo etal. 2009. The Indian
deposits are typic ally c harac terized as
Figure 1: Chrome ore and Ferrochrome price ferruginous and siliceous type ores. The ores of
forecasts Sukinda valley are mostly high grade, soft and
(Source: Merafe Resources October 2011 friable in nature besides few quantities of hard
presentation) lumpy ore, formed in separate bands. These are
mainly assoc iated with laterite, altered
ultramafic roc k, nickeliferrous limonite,
goethite and talc serpentine schist.

Figure 2: Stainless steel end-use consumption,

2007–15F
(Source: Outokumpu presentation dated 10
January 2012, KPMG analysis)
Figure3. Chromite distribution in India
2. Chromite Deposits - India
3. Beneficiationpractice
India ranks 3rd in chromite production and 5th
In both Sukinda and Boula-Nausahi sectors
in terms of chrome ore reserves in the world.
chrome ore is mined by open cast mechanized
Chromite deposits occur in several Indian states
mining method. Early mining of chromite was
(Figure3) like Tamilnadu, Goa, Karnataka,
on a small-scale and was relatively straight
Maharashtra and Odisha in the form of
forward from outcrops or to shallow depths
discontinuous bands, lenses and pockets in
followed by hand sorting.With the increased
different host rock associations. Though
demand, conventional open-pit mining and
insignificant in the context of world resources,
mechanical underground mining became
India is endowed with appreciable quantities
necessary. Open-pit mining is generally applied
of good grade chrome ores. Around 90% of the
to the podiform ores at first but this progresses
chromite resources of India are concentrated in
to underground mining as deeper levels of the
Sukinda valley of Jajpur district and Boula-
deposit are reached. An overview of the
Nuasahi belt of Odisha state. Sukinda
beneficiation scenario is presented in the
ultramafic belt (SUB) and Boula-Nausahi
Figure4 below.
Igneous Complex (BNIC) of Odisha, India

131

Figure 4: Changing chromite beneficiation
scenario in India
3.1.1. Beneficiation at sukinda mines – India
The Sukinda Chromite Mine (SCM) is one of the
largest open cast mechanized chromite mine in
India, under the Tata Steel Ferro Alloy and
Mineral Division. There are three chromite
bands within the leasehold area. The ROM ore
from the various mines is sent to beneficiation
plant via stack yard where ore is blended before
being fed to beneficiation circuit. The sequence
of operation is presented in Figure5.
The beneficiation plant has two major sections:
(a) Communition (for preparing the material to
the subsequent unit operations)
(b) Conc entration - (Classific ation and
beneficiation)
The feed preparation unit inc orporates
screening of the ROM ore to 25 mm from -220
mm followed by two stage crushing (primary
and secondary crusher) and screening to
produce less than 3 mm size fraction. This
132
MPT-2013
fraction is further ground to less than 1 mm in
a ball mill and then sent to beneficiation circuit
to produc e the c ustomized c onc entrate
products.
3.1.2. Challenges in beneficiation plants
All mineral processing / beneficiation plants are
designed to operate at a rated capacity to meet
the specific targets of production, grade, yield
with minimum losses based on the feed (ROM)
c onstituents. The design and operating
parameters of the unit operations of such plants
are set accordingly. But in real practice the
process operators as well as the plant has to
undergo numerous uncertainties viz a viz
input to the plant such as feed properties,
mineral composition, size distribution of the
feed etc. This variability affects the overall
performance of the beneficiation circuit in
terms of grade, recovery, throughput including
loses of valuable minerals into tailing.
Continuous observation, monitoring and
timely recording of these variations in an
operating plant has to be done to make the
process efficient. An operator should always
have in hand information of the changes in the
quality of feed so as to make the necessary
changes in the circuit and to predict the product
grade.
Although literatures on the performance of
individual concentrators are available but
detailed information on the performance with
respect to size and liberation of particle etc., is
scarce.The main trends in gravity concentration
are towards developing processes for the
treatment of fine ores, improving the efficiency
of existing mac hines and c onc entrating
minerals. In the last two decades, many
processes have been reported in the form of
technical reports, papers and reviews (Rama
Murthy, et al. 2011a, 2012b, Tripathy, et al. 2013,
Li et al., 2011, Gu et al., 1988, Guney, et al.,
1990a,1994b,2001c , Cic ek,et al., 2002, ,
Atalayand Ozbayoglu, 1992, Ozdag et al.,

1994,Sönmez and Turgut, 1998).A comparison
of the peak efficiencies cannot be made based
on the effect of operating conditions alone. The
research works of Pascoe, et al., 2007, Ozdag, et
al., 1994, shows that it is possible to make a
sensible selection of gravity separation from
information on particle size and the mineralogy
of the ore. The present work is carried in an
operating chromite ore beneficiation plant,
Sukinda, with an objec tive to develop a
monitoring system / data base to improve the
quality of the product.
4. Methodology
Accurate data collection and proper data
interpretation followed by making necessary
change which is implementable in an operating
plant play very critical role in performance of
the circuit.There are many causes of the data
variability, including both error (sampling and
assay), and real variation in performance due
to changes in ore mineralogy, operating
conditions and other factors. The methodology
adopted is outlined in the Figure 5.
.Figure 5: Methodology adopted
4.1. Circuit sampling and analysis
For better analysing the circuit, it is necessary
to understand the performance of individual
unit operations in the c irc uit. But, in a
continuous operating process plant, it is very
difficult to get all the required operating
parameters , as there is continuous change in
the feed conditions and other parameters.
Within the limitations of available data in the
133
MPT-2013
present study initially the samples were
collected from the classifying units such as
hydrocyclone and spirals and were analysed
for size and chemical analysis. The variation of
Cr 2O3 and SiO2 were also measured at the
existing operating parameters.
5. Results and Discussion
5.1. Mineralogical studies of circuit
Sink and float analysis using heavy liquids and
liberation and mineralogic al studies by
QEM*SEM (Quantitative Evaluation of
Materials by Scanning Electron Microscopy)
was carried out for characterizing samples
collected from individual unit operations of the
circuit. The product grade was contaminated
by the siliceous gangue minerals. Hence in the
c harac terization studies analysis was
primarily done for siliceous gangue phases and
was discussed.
5.1.1. Feed circuit analysis
The liberation analysis of the feed to ultrafine
circuit is presented in Figure.6. It is observed
from the characterization studies that silica
deportment is either from quartz or from Fe
Silicate (Mg & Al). Free quartz is majorly
contributed by flaotex density separator as is
visible from the float fractions of sink and float
analysis whereas the other form (fine Fe Silicate)
is c ontributed through c lassifiers i.e.
hydrocyclone. The liberation analysis shows
that 50% (mass)of the quartz is fully liberated.
(a) Sink and Float analysis
(b) Mineral Mass Percent
(c) Liberation of quartz (d) Elemental Deportment of Silica
Fig.6: Liberation studies of SiO2 and Cr2O3 in
the feed
 MPT-2013

5.1.2. Spiral circuit analysis constant vortex finder diameter of 50mmand

58mm. In the present article only the results
From the characterization studies of the spiral
obtained at optimised conditions are presented.
circuit samples it was revealed that:
The effect of these parameters on SiO2reduction
 The middling’s and tailings contain more
in the overall circuit was highlighted.
gangue phases i.e., SiO2, Fe silicates and
kaolinite (Figure.7 (d). Observation from the
mineral mass fraction and liberation
analysis carried out by QEMSEM confirms
the presence of locked fractions.
 Cr2O3 in the middling and tailing of rougher,
cleaner and scavenger circuit was found in
between 45% - 50% (by mass).
 Cr2O3 in the cleaner concentrate contain
80% Cr2O3 (by mass) whereas rougher and
scavenger contain ~65% Cr2O. (a) Effect of spigot diameter on cut size

Liberatio
n of
Quartz

(b) Mineral Mass Percent (rougher and cleaner)

(a) Liberation of quartz in Rougher and Cleaner Circuit

Liberati
on of
Quartz
(d) Mineral Mass percent of Scavenger circuit (b) Overall effect on circuit (SiO2)
(c)Liberation of quartz Figure 8: Results of plant trials
Following observations were made from the
Figure 7: Liberation studies of SiO2 and results obtained from plant trials under the
Cr2O3 rougher, cleaner and scavenger optimised conditions:
circuit  The average size of the cyclone under flow
wasreduc ed to 40 µm and 30 µm
5.2. PlantCircuit performance analysis respectively as shown in Figure 8 (a).
In a continuously operating gravity based  A considerable reduction (<12% Cr2O3) in
beneficiation plant it is always very critical and the Cr 2 O 3 losses into the tailings was
cumbersome to carry out real time trials. observed in all the hydrocyclone overflow
Monitoring numerous parameters of beneficiation circuit, which are earlier
simultaneously and analyzing the data without reporting to the tailing stream.
hampering the day to day plant process is a  The overall silica in the ultrafine
challenging job. Keeping this in view for the concentrate under optimized conditions
first campaign hydrocyclone spigot diameters has reduced to 3.27% from the audited
were varied between 33mm to 35mm at a value of 6.94%.

134

6. Conclusions
Following conclusions were drawn from the
performance evaluation studies carried on the
ultra-fine beneficiation circuit of chrome ore
beneficiation plant, Sukinda:
 Literature review revealed that unsteady
operation of beneficiation units in the
proc ess circ uits, espec ially gravity
operated circuits and qualitative changes
in the feed (ROM) to the plant affects the
overall performance of the beneficiation
circuit. Thus the efforts and solutions were
also unique and tailor-made for the
problems at hand.
 The results obtained from the
characterization studies of the circuit
samples revealed that:
 The silica deportment is from two
minerals - free silica i.e., quartz and
locked silicates i.e., Fe (Mg &Al)
silicates.
 In most of the samples major
dominance is of Fe (Mg& Al) silicates
was observed.
 Continuous evaluation of the process
circuit helps in improving the performance
of the any gravity circuit and helps in
achieving required target of the product by
making changes in the operating parameter
of existing units.
 The overall silica in the ultrafine
concentrate under optimized conditions
has reduced to
3.27% from 6.94% followed by reduction
(<12% Cr 2O 3) in the Cr 2O 3 losses into
tailings.
Acknowledgements
The authors are thankful to Tata Steel
management for their encouragement, support
and permission to publish the paper. Thanks
are also due to all team members and
supporting staff of FAMD and R&D and SS for
their support and throughout the work.
135
MPT-2013
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Pascoe, R.D., Power, M.R., Simpson, B., 2007.
QEMSCAN analysis as a tool for improved

understanding of gravity separator
performance. Minerals Engineering 20, P-
487–49520.
Rama Murthy Y, S.K.Tripathy, Raghu Kumar. C
2011. Chrome ore beneficiation challenges
& opportunities - A Review, International
Journal Minerals Engineering. Minerals
Engineering 24, P-375–380.
Rama Murthy Y, Sunil K Tripathy, Veerendra
Singh, Vilas D Tathavadkar and A Ranjan
2012. Studies on reduction in chromite
losses in tailing in an operating plant. Xxvi
International Mineral Proc essing
Congress(IMPC) 2012 proceedings / New
Delhi, India / 24 - 28 September 2012. 4377-
4385.
*******
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Sahoo, R.K., Mohanty, J.K., Das, S.K., and Paul,
A.K., 2009. Chromites of India Their
Textural and Mineralogic al
Characteristics. International seminar on
magmatic ore deposits ( ISMO 2009).
Sönmez, E., Turgut, B., 1998. Enrichment of low-
grade Karaburhan chromite ores by
gravitational methods. In: Atak, S., Onal,
G., Celik, T. (Eds.), Innovation in Mineral
and Coal Processing. Balkema, Rotterdam,
The Netherlands, pp. 723–726.
Sunil Kumar Tripathy, Y.Rama Murthy,
Veerendera Singh 2013. Characterization
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beneficiation plant tailing. International
Journal of Mineral Processing 122, P- 47–
53.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Developments in Fine Mineral Spiral Separation Technologies

Glen Rampola Alex D Costa1* and O K Venugopal2

1
MD Mineral Technologies Pvt Ltd. No: 17,14th Main, 14th Cross, HSR, Sector IV,
Bangalore Karnataka India 560102. T +91 9823897911.
2
MD Mineral Technologies Pvt Ltd 14/81 B, Alliance Junction, Thevarakavu Road,
Tripunithura, PO, Ernakulum – 682 301, Kerala, India T +91 484 2785160, Mineral
Technologies Pty Ltd Head Office -Carrara, Gold Coast, Queensland, Australia, T +61 7
5569 1300 F +61 7 5525 3810 Emailto: info@mineraltechnologies.com

Abstract
The utilization of low grade fine iron ores and tailings can help maintain a sustainable supply of
minerals to meet the need of the steel industry. There have been recent developments in Spiral
technology that has enhanced recovery and grade in many mineral processing plants in India.
This paper highlights the development and use of fine mineral spirals for the beneficiation of low
grade iron ore and rejected plant tailings with case studies discussed and presented.

Keywords: Mineral processing; gravity separation; spirals; spiral separators; iron ore tailing
recovery; fine mineral beneficiation.
1. Introduction
Flow sheet of the existing processing plant in
The use of spiral separators in mineral
India reveal that fine-grained iron minerals are
processing is an old concept which has recently
present in the process stream due to the natural
been used widely to process iron ore. The
fine content of the ore and those produce in the
inc rease in pric e of iron ore fines and
process of crushing screening, grinding,
simultaneous depletion of ore bodies has
stacking and reclamation from the blending
prompted the adoption of new methods and
yard. Traditional mineral dressing techniques
technologies in mineral processing. Mineral
such as selective classification and magnetic
processing plants are affected by many factors
separation may not entirely concentrate the
among which are grain size ranges, liberation
recoverable iron units. The use of a gravity
size of the ore, the percentage of natural fines in
separation technique with the fine mineral
the ore, etc these factors present new challenges
spiral can be complimentary and thus to
and directly affects recovery and concentrate
enhanc e overall iron rec overy. This
grades.
methodology of process design has also been
* Correspending Author: Glen D Costa, proven to be a cost effective. Another challenge
Email :glendcosta@gmail.com Ph :+ 91982 38 97911 that is put forward by the industry is the
processing of low grade ore (BHQ/BMQ) and

137

the need to retreat plant tailings that have been
rejected over the years. These low grade fine
ores and tailings c an help maintain a
sustainable supply of minerals to meet the need
of the industry if processed with the right
equipment and techniques. Another aspect is
the price of iron ore fines has increased
significantly in recent times, pressure for
environmental remediation of mine sites , the
shortage of suitable or available sites on current
leases, has made iron ore dump reclamation
more attractive for both proc essors and
regulators. Resourc e c onservation,
environmental engineering demands and
competitive pricing for high quality fine
concentrate, have seen a range of dumps and
pond reclamation projects initiated in Brazil,
Australia, South Africa and most recently India.
This paper makes an effort to showcase that
iron ore tailings can be processed economically
and efficiently by using low capital cost, low
operational and low maintenance equipment
like gravity spiral concentrators. The majority
of the metallurgical information contained in
this paper come from data recently gathered
from Mineral Technologies pilot testing and
laboratory facility located in India. Test work
has also been independently carried out by
clients using the FM1 spiral at their plant sites.
Spiral separators principles
Gravity c onc entration of minerals has
traditionally been recognised as a low cost and
environmentally friendly process for the
separation of minerals. In recent years a
number of new process technologies have
emerged allowing ever-finer materials to be
successfully processed. Fine mineral spirals
separators are just one of these new emerging
tec hnologies that have the potential to
efficiently separate mineral species down to 20
micrometres in size. Spirals separators are
simple, low energy consuming devices that
138
MPT-2013
separate minerals based on their respective
densities and have proven to be metallurgically
effic ient and c ost effec tive sinc e their
widespread commercial introduction more
than 50 years ago.
The general principle of spiral are that high
density particles rapidly settle in the pulp
stream, contact spiral profile and slow down
and then move towards the centre. Splitters
divert high density partic les into the
concentrate channel while the fine particles
tend to centre and the low density particles are
held up in the pulp flow. Centrifugal forces hold
particles and water in outer trough where as
the coarse or high density particles tend to the
inner trough. Low density fines (silica ,alumina
and clays) reports with the fluid, the primary
flow transports slurry and allows settling and
stratification where as the secondary flow is
brought about by centrifugal forces and causes
shearing of the strata. This is unique to spirals.
Primary
(down trough)
flow
Secondary flow
Primary flow
Secondary
flow
Lights
Middlings band
High density band Inner zone Transition zone Outer (recovery) zone
Fig. 1: Primary and secondary flow patterns
on a spiral separator
Considerable effort has been expended on the
development of new gravity separators in an
effort to achieve separations at finer sizes and
more discreet proc essing c apabilities to
accommodate such difficulties as smaller
particle density differences. The greatest efforts
appear to have been reserved for high gravity
devices with new machines such as the Kelsey
jig, the continuous Falcon separator and the
Mozely MGS. These devices generally provide
 MPT-2013

greatly enhanced “gravity” forces that are Con Fe Tails Fe Con Wt Fe rec’y
generated in a drum type mechanism rotating Source/Stream Fe% Feed % % % %
56.5 45.1 34.4 39.7
at high speed around a central axis. Size Tailing pond 49.0
56.7 46.0 28.2 32.6
separations down to less than 10 micrometres
are ac hievable and good metallurgic al CASE 2: Fine iron ore sample taken from a tail-
performance on minerals with small density ing pond.
differences is achievable in some circumstances.
Con Fe Tails Fe Con Fe rec’y
However, all of these enhanc ed gravity Source/Stream Fe% Feed % % Wt% %
mac hines are mec hanic al in nature and 51.0 32.9 22.7 31.2
generally have higher costs both from a capital Tailings pond 37.0 51.2 32.5 24.1 33.3
and operating perspective. They also require D50=45 micron
48.9 35.3 12.5 16.5
significantly higher level of technical expertise
in operations and maintenance. Case 3: Fine iron ore sample taken from a
A recent development is the FM1 spiral 6.5 turn
tailing pond (D50=45 micron)
separator; designed to operate down to 20
micrometres whilst ac hieving acceptable Fe
Con Fe Tails Fe Con WT rec’y
mineral recoveries and upgrade ratios. This Source/Stream Fe% Feed % % % %

updated model of the spiral separator is aimed Primary U/F 48.0 60.0 35.3 51.4 64.3
48.8 60.9 36.4 50.6 63.2
at both roughing and cleaning applications.
50.7 61.7 38.6 52.4 63.7

2. Case Studies 49.1 61.2 36.1 51.8 64.6

The need to recover fine heavy particles from Case 4: Fine iron ore sample taken from a pri-
process streams is becoming increasingly mary cyclone underflow.
necessary in the mineral processing industry
Fe
as a number of the potential reserves available Tails Fe Con WT rec’y
Source/Stream Fe% Feed Con Fe % % % %
for future mining contain finer minerals than
Ball Mill cyclone 52.6 59.0 43.1 59.7 67.0
those being treated currently. Many of these fine underflow
60.3 42.5 56.7 65.0
grained deposits have been found in the iron
62.1 48.3 41.3 47.5
ore and mineral sands industry of India. As the 54.0
61.2 48.6 42.9 48.6
development of the deposits within this sector
is currently being pursued in India, recent Case 5: Ball mill ground cyclone underflow.
testing of fine products has been carried out on
Con WT Fe rec’y %
the FM1 spiral in out test rig facility in India Source/Stream Fe% Feed Con Fe % Tails Fe % %
Cleaner Stage 63.7 53.5 39.0 43.2
with improvements in Fe grade in only one 57.5
64.7 53.4 36.0 40.6
stage of spiral separation 62.9 54.9 74.7 77.2
60.9
Test work was carried using various ores from 63.5 54.7 70.2 73.2

different part of the country and also using both CASE 6: Fine iron ore sample Cleaner stage.
natural fines and tailings.
During the pilot plants tests the feed conditions
Con Fe Tails Fe Con Wt Fe rec’y
Source/Stream Fe% Feed % % % % of the spiral were maintained at 35-40 % solids
53.4 24.2 65.4 80.7
Tailing pond 43.3 w/w pulp density with a solids loading per
52.6 24.7 66.7 81.0
start feed ranging from 0.8 tph to 1.1 tph.
CASE 1: Fine iron ore sample taken from a tail- The particle size distribution of the test work
ing pond. samples were predominantly in the sub -150

139

micron range. Samples that were taken from
the tailing ponds (Case 1 to 3) had naturally
occurring fines where as the samples taken
from the low grade dumps (Case 4 to 6) were
ground to minus 50-60 micron in order to
liberate the mineral and then passed onto the
spiral.
Close considerations of the case studies show
effective recovery and upgrade of fine iron ore
into a final concentrate in a single spiral pass.
The iron ores used in the study were taken from
various tailing ponds and low grade iron ore
dumps around India. Based on the results it is
clear that an effec tive flow sheet c an be
developed for the recovery of fine iron ore with
a final concentrate that can be used as a feed
product to the steel plant.
The benefits of using the FM1 spiral for the
treatment of fine iron ore has been proven
through this test work data. Other potential
applications for the use of fine spiral technology
include operations that currently grind their
feed material to 50-60  m to ac hieve
satisfactory liberation especially in BHQ and
BHJ ores. While the use of traditional spiral
separation technology to treat this material has
historically been ineffective at this size range,
the use of FM1 type spirals may enable a
reduction in the amount of material treated
through subsequent processing stages by the
rejection of fine liberated gangue material after
grinding. For example in the preparation of
material for flotation, significant recovery can
be made by introducing a gravity stage prior
to the flotation stage, hence reducing the size of
the flotation circuit and therefore reducing
capital and operating expenses.
3. Process Implications
The c lassic al approac h to fine gravity
separation of ores involved classification of the
feed into a number of relatively narrow size
ranges followed by separate parallel treatment
140
MPT-2013
of the classified streams. This approach proved
to be very successful particularly in the tin
industry, and although since these times there
has been movement towards reducing the
number of classified parallel streams, the
concept remains valid. The availability of spiral
separator models that can effectively process
material down to below 20 micrometres in size
provides a means to design flow sheets that
conform to the traditional concepts of gravity
separation of parallel classified streams.
The utilisation of FM spiral separators to treat
material in the size range below 0.15
millimetres and conventional spiral separators
to process material above say 0.15 millimetres,
provides a low cost option for a number of likely
proc essing systems; inc luding those
applications in Mineral Sands, Tin, Chromites,
and Iron ore.
In some applications, such as fine iron ore
upgrading or tailings re-treatment, the
required separation can be satisfied with a
single stage circuit and this is confirmed by
some extensive test work in the Hospet-Bellary
region.
Whether single or multi-stage spiral circuits
are utilised, the availability of the FM model
spiral will enable the benefits of spiral
separators to be extended to encompass a wider
size range of the total ore treated. Subsequent
cost reductions will result from:
• Simplified operational requirements
• Lower capital costs
• Reduced operating costs
• Improved overall recoveries
• Greater versatility to handle variability of
ore type and associated
changes to size consist of ground (or
naturally occurring) ores
• Reduced water demand
• Improved plant control.
Competing equipment is generally
mechanically and operationally more complex,
 MPT-2013

and invariably involves higher capital and using FM1 spirals it is possible to recover a
operating costs compared to spiral separators. significant quantity of fine iron into a saleable
Any metallurgical performance gains must product. Analysis has also demonstrated that
therefore be weighed against these cost and the value generated from the additional
operational benefits. recovery outweighs the cost of the additional
plant and equipment.
4. Conclusions
Acknowledgements
With the need for better grade and recoveries
We take the opportunity to acknowledge the
in mineral process plants, spiral separation
opportunities to discuss and interact with the
technologies have been shown to provide cost
people of various mining companies who have
effective and eco-efficient mineral processing
provided the means to conduct test work by
solutions. Fine mineral (FM1) spiral separators
which our solutions and experience have been
extend the cost effective size range for gravity
developed. We also thank the management of
separation using this technology down to well
Mineral Technologies for permission to publish
below that previously considered technically
this paper.
feasible using spiral separators.
The focus in spiral plant design in recent years References
has been to not only improve separation
Richards, R. G., Machunter, D., Gates ,M. P. J. ,
efficiencies, but significantly increase feed
Palmer ,M. K., Gravity Separation of Ultra-fine
capacities using cost effective and eco friendly
(- 0.1mm) Minerals using spiral separators. MD
equipment.
mineral technologies, P.O. B ox 2569, Nerang
The results obtained from the test work
Mail Delivery Centre, Queensland 4211,
undertaken in these case studies has shown that
Australia.

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141
 MPT-2013

142
 MPT-2013

FLOTATION

143
 MPT-2013

144
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Single Reagent for Graphite Flotation

N.Vasumathi 1 *, T.V.Vijaya Kumar 1 , S.Ratchambigai 1 , S.Subba Rao 1 ,

S.Prabhakar 1, G.Bhaskar Raju1 , B.R.Nayak2 , S.Shiva Kumar 3 and Uma Raman3
1
CSIR-National Metallurgical Laboratory Madras Centre, Chennai, 600113, Tamil
Nadu, India.
2
CSIR-National Metallurgical Laboratory, Jamshedpur, 831007, Jharkhand, India
3
M/s Somu Organo Chem Pvt. Ltd., Bengaluru, 560076, Karnataka, India.

Abstract
Generally, diesel and frother are used as reagents in graphite flotation. With the escalating cost of
petroleum products and their negative impact on environment, attempts are made to formulate
an eco-friendly single reagent to replace the diesel-frother system without affecting the flotation
performance. CSIR-NML Madras Centre in collaboration with M/s Somu Organo Chem Pvt Ltd.,
India, has worked out the formulation and evaluation of single reagent on a low grade graphite
ore sourced from eastern India. The petrography studies indicate that the ore primarily consists
of quartz and graphite with minor quantity of mica and analyzing 87.85% ash content. The ore is
crushed in stages followed by primary coarse wet grinding to 242 µm (d80). Rougher flotation is
carried out in Denver flotation cell with a view to eliminate gangue as much as possible in the
form of primary tailings with minimal loss of carbon. Regrinding of rougher concentrate to 216
µm (d80) is opted to improve the liberation of graphite values. This approach involving a primary
coarse grinding and regrinding of rougher float followed by multi-stage cleaning using this single
reagent is found to yield better recovery and grade when compared with that of the dual reagent
system. A final concentrate of 12.03% weight recovery with 3.22% ash could be achieved. Based
on encouraging laboratory studies using the single reagent, plant trials were carried out. From
the cost benefit analysis, this single reagent proves to be an economically viable in place of diesel-
frother for processing low grade graphite.

Keywords: Low grade graphite; liberation; froth flotation; single reagent; diesel.

1. Introduction metamorphism of organic matter in sediments.

The global graphite market consists of two main Flake graphite is assumed to be derived from
products namely amorphous graphite and flake the fine-grained sediments rich in organic
graphite (Wakamatsu and Numata, 1991). matter. As metamorphic grade increases,
Graphite generally oc c urs as a result of carbonaceous material converts to amorphous
graphite (Dey and Pathak, 2005). Flake graphite
* Correspending Author: N. Vasumathi, Scientist, CSIR-
National Metallurgical Laboratory Madras Centre, Chennai,
600113, Tamil Nadu, India. Contact No.: +91-44-22542077;
Email: vasumatisamy@gmail.com

145

is classified based on the size of the crystal flakes
and graded according to their graphitic carbon
content and particle size. Microcrystalline
graphite is commercially called as amorphous
graphite. The r.o.m ore of low grade, containing
about 10% fixed c arbon (FC), has to be
invariably beneficiated before marketing.
Processes for graphite beneficiation depend
upon the nature and association of gangue
minerals present. Graphite can be enriched
easily by flotation because of its natural
hydrophobicity (Kaya et al, 2007 and Acharya
et al, 1996). Froth flotation process is used
widely as it helps in producing a high-grade
graphite concentrate (Kim et al, 2003) which
finds applications in refractories, batteries and
high temperature lubricants (Mitchell, 1993).
Flotation utilizes the differences in the surface
properties mainly the hydrophobic ity of
graphite (Chau et al, 2009; Kim et al 2002 and
Deryagin et al, 1982) which is one of the main
factors in determining the separation efficiency
by flotation. Beneficiation of low grade graphite
ore using mechanical cell and column flotation
cell were studied (Bhaskar Raju et al, 2000; El-
Raheim, 2004 and Narasimhan et al, 1972) by
using conventional hydroc arbon oils as
collectors.
In froth flotation, graphite ores are often
subjec ted to a suitable hydroc arbon oil
treatment to alter their hydrophobic ity,
enhance recovery, and / or improve selectivity
(Patil et al, 2000). Conventionally, the collectors
used in most of the graphite flotation studies
are diesel, kerosene, petrol in combination with
pine oil as frother (Didolkar et al, 1997). Various
combinations of these conventional reagents
namely kerosene collector in combination with
90:10 ratio of methyl isobutyl carbinol (MIBC)
and ethyl alcohol were studied in graphite
flotation (Ravichandran et al, 2012). Also
commercial grade frothers such as pine oil,
MIBC, eucalyptus oil and ethyl alcohol with
kerosene and diesel oil as collectors were used
in graphite flotation (Ravichandran et al, 2013).
Flotation studies of graphite in aqueous salt
solution using sodium acetate were carried out
146
MPT-2013
(Grabowski and Drzymala 2008). T he
polyethylene oxide type of frothers like
polyoxypropylene glycol butyl ether was also
studied as a replacement for MIBC in graphite
flotation (Pugh, 2000). Major studies on
collectors and frothers other than diesel/
kerosene and MIBC/pine oil respectively were
found much in graphite flotation literatures.
Hence in this present investigation, eco-friendly
single reagent was developed as a replacement
for diesel-frother system. This single reagent
developed was tested for its efficiency at
laboratory scale. After encouraging results are
obtained at laboratory sc ale, trials were
undertaken at industrial scale in a graphite
beneficiation plant with 5.0 t/h flotation circuit.
Also the cost benefit analysis was carried out
to study the economic feasibility of the single
reagent developed with that of diesel-frother
system.
2. Materials and methods
2.1. Materialsa low grade run-of-mine graphite
ore was received from Jharkhand state of India.
The ore is crushed in stages followed by mixing
thoroughly. A representative sample was
drawn for size and chemical analysis (Reddy
et al, 1997) and the results are shown in Table 1.
Table 1: Analysis of graphite ore.
Sample Ash, % Moisture, % Volatile Matter, % Fixed Carbon, %
Graphite ore 87.80 0.12 3.49 8.59
2.2. Size analysis
The particle size distribution of the stage-
crushed graphite ore was carried out using
B.S.S sieves and the weight percentage retained
on each screen along with their ash values are
tabulated in Table 2. The calculated d80 of this
graphite sample was found to be 605 µm.
Table 2: Size & Ash Analysis of stage-crushed
graphite.
 MPT-2013

2.4. X-ray diffraction studies

Ash
Size, µm Wt. retained, % Ash, %
Distribution, % The graphite ore was subjected to x-ray
+850 12.13 91.01 12.23 diffraction studies for mineralogical phase
-850+500 14.91 91.69 15.14
analysis especially the identification of non-
graphite minerals (Delviller et al, 1992) and the
-500+300 17.49 90.02 17.45
diffractogram is shown in Figure 2. The
-300+212 15.31 89.24 15.14
characteristic x-ray of copper-Ká radiation
-212+106 22.86 90.92 23.02
with 1.54 Å wavelength was used in this
-106 17.30 88.83 17.02 diffraction study. The sample was found to
consist predominantly of quartz and with
It is evident from the above table that the ash minor fractions of graphite and traces of mica.
content is above 88.83% in all size fractions. This
This high intensity of quartz presenc e
implies that there are hardly any free and
contributes to the high ash content of the ore.
liberated graphite flakes in any size range and
demands size reduction before attempting to
recover the graphite values.
2.3. Mineralogy
The mineralogical characterization of graphite
ore was carried out to determine the extent of
graphitic carbon content and graphite flake
size. These two properties determine the
economic value of the graphite and also provide Figure 2. X-ray diffractogram of
a basis for beneficiation feasibility studies. graphite ore
Petrographic characters (Figure 1a to 1d) under
optical microscope indicated that the sample 2.5. Flotation methodology
consists primarily of quartz and graphite in the
The flotation experiments were conducted in
form of both fine & thick flakes dispersed in the
Denver laboratory flotation machine, D-12 with
silica matrix, with minor quantity of mica
(biotite). a cell volume of about 3000 ml. The flotation
studies were carried out on graphite feed with
eco-friendly single reagent Sokem 705C. Also,
flotation tests using conventional reagents
namely diesel as collector for graphite and pine
oil as frother and sodium silicate as depressant
for silica / silicate bearing minerals were carried
out for performance comparison and evaluation
of the single reagent with the conventional
reagents. Flotation experiments were
conducted at 15% solids at natural pH and
Figure 1. (a) Petrographic images of graphite impeller speed of 1200 rpm. The graphite slurry
ore with long graphite flakes dispersed within was conditioned with the reagents for 3 minutes
silica matrix; (b) Thick fibrous graphite
each and the froth (float) was collected till froth
surrounded by silica; (c) Fine flakes of graphite
formation ceased. The collected float and tailings
dispersed in silica matrix and (d) Thin fibrous
graphite. were dewatered, dried, weighed and subjected

147
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to ash analysis. The combustible recovery (CR), 3.1. Effect of primary grind time
ash rejection (AR) and efficiency index (EI) were Flotation tests for primary grind optimization
calculated from the weight recovery / yield and studies were carried out using single reagent,
ash values for each test using the following Sokem 705C. Sodium silicate (3.0 kg/t) was used
equations respectively. as depressant for silica bearing minerals during
M C (100  A C ) grinding. The graphite ore was subjected to
%CR  x100 primary wet grinding in a ball mill for different
M f 100  A f  periods of grinding time. Each time the ground
sample was subjected for size analyses to find
M A  out d80 of it. The grinding media used was 3.5 kg
%AR  1   C C  x100
 Mf Af  of steel balls and grinding was carried out at
65% solids by weight. After primary grinding,
EI  CR  AR )  100 0.137 kg/t Sokem 705C was added as collector
where, for graphite flotation and this same dosage was
Ac = ash content in concentrate, % maintained for all the grind variation studies.
Af = ash content in feed, % The concentrate and tailing obtained were
Mc = Mass of concentrate, g dried and subjected to ash analysis and
Mf = Mass of feed, g tabulated as shown in Table 3.
Also plant trials were conducted at a graphite Table 3. Effect of primary grind variation on
flotation plant circuit of 5.0 t/hr capacity using flotation Sodium silicate: 3.0 kg/t; Sokem
Sokem 705C for validating the findings obtained 705C: 0.137 kg/t; Ash of Head sample: 87.85%
from the laboratory flotation studies.
2.6. Plant trails Primary grind
time, minutes
d80 size, µm Products Yield, % Ash, %
CR,
%
AR,
%
EI

Plant trials were conducted at a graphite 605

Concentrate 14.11 49.15 60.77 92.13 52.90

0 Tailing 85.89 94.60

flotation plant with a treatment capacity of 5.0
Concentrate 19.12 44.11 84.62 90.35 74.97
t/hr. For this purpose 0.05tonnes of the reagent 5
349
Tailing 80.88 97.60
Sokem 705C was used for 7 shifts continuously Concentrate 19.20 48.42 86.42 89.50 75.92
292
to validate the findings obtained in the 7 Tailing 80.80 98.07

laboratory studies. 242

Concentrate 17.03 35.93 86.96 93.00 79.96

9 Tailing 82.97 98.03

2.7. Flotation reagents Concentrate 17.57 38.29 88.12 92.33 80.45
206
11 Tailing 82.43 98.23
The new eco-friendly single reagent Sokem
Concentrate 16.63 34.18 89.45 93.52 82.97
705C, a proprietary chemical of ether-alcohol 13
180
Tailing 83.37 98.45
based was used in this graphite flotation Concentrate 16.14 32.93 88.98 93.95 82.93
164
studies. This single reagent was manufactures 15 Tailing 83.86 98.41

by M/s Somu Organo Chem. Pvt. Ltd., Bangalore

and evaluated by CSIR-NML Madras Centre.
Commercial grade diesel and pine oil used for
the flotation experiments were purchased from
the local market.
3. Results and Discussion
From the above results, the primary grind at 9
minutes was found to be optimum as the ash
c ontent of the rougher c onc entrate was
relatively lower at 35.93% with respectable
weight recovery of 17.03%. Also the ash
rejection in tailings was high at 93.00% at the

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coarsest possible primary grind. It is essential Table 5: Effect of Sokem 705C at primary grind
to keep the graphite flake size as big as possible on graphite flotation Primary grind d80: 242 µm;
which is the criteria for its value/price. Hence, Sodium silicate: 3.0 kg/t; Ash of Head sample:
the d80 of 242 µm obtained at 9 minutes primary 87.85%
grind was found to be optimum and all Sokem 705C Products Wt., Ash, Ash CR, AR, EI
dosage, kg/t % % Distribution, % % %
subsequent flotation tests were conducted at 0.110 Concentrate 14.92 25.02 4.29 85.90 95.71 81.61

this particle size. Tailing 85.08 97.85 95.71

0.137 Concentrate 15.12 26.69 4.63 86.67 95.37 82.04

3.2. Effect of Sodium silicate Tailing 84.88 97.99 95.37

0.160 Concentrate 16.36 30.44 5.73 86.45 94.27 80.72

Tailing 83.64 97.88 94.27

The d80 size of primary grind was fixed at 242 0.181 Concentrate 17.65 34.08 6.93 88.26 93.07 81.33

µm. After primary grind variation studies, Tailing 82.35 98.12 93.07

sodium silicate dosage optimization was 0.195 Concentrate 18.56 38.49 8.20 88.58 91.80 80.38

Tailing 81.44 98.19 91.80

carried out. A fixed dosage of 0.137 kg/t for
Sokem 705C was maintained for flotation for From the above flotation results, the optimized
all the tests in this series and the flotation test Sokem 705C dosage was found to be at 0.137
results are given in Table 4. kg/t. At this dosage, the rougher concentrate
Table 4. Effect of sodium silicate variation on assaying 26.69% ash with weight recovery of
flotation 15.12% and ash rejection of 95.37% in tailings
Primary grind d80: 242 µm; Sokem 705C: 0.137 could be achieved. The efficiency index at this
kg/t; Ash of Head sample: 87.85% dosage was found to be the highest at 82.04.
In order to compare the performance of single
Sodium Products Wt, % Ash, % Ash CR, % AR, % EI reagent Sokem 705C with diesel-pine oil
silicate Distribution, system, further graphite flotation studies were
dosage, kg/t %

1.0 Concentrate 19.48 49.22 11.05 74.76 88.95 63.

carried out using diesel and pine oil.
71
Tailing 80.52 95.85 88.95 3.4 Effect of diesel
2.0 Concentrate 16.87 43.16 8.39 72.37 91.61 63.
98 The primary grind (d80: 242 µm) and sodium
Tailing 83.13 95.60 91.61
silicate dosage (3.0 kg/t) were maintained the
3.0 Concentrate 17.48 43.40 8.77 73.18 91.23 64.
41 same. Flotation tests on diesel dosage variation
Tailing 82.52 95.60 91.23
at fixed dosage of pine oil (0.154 kg/t) were
carried out to study its effect and the results
The sodium silicate dosages were varied from
are given in Table 6.
1 to 3 kg/t. From the results obtained, the sodium
Table 6. Effect of diesel at primary grind on
silicate dosage was optimized at 3 kg/t as the
graphite flotation , Primary grind d80: 242 µm;
efficiency index is high at 64.41%. The dosage of
Sodium silicate: 3.0 kg/t; Pine oil: 0.154 kg/t,
sodium silicate was maintained at 3.0 kg/t for
Ash of Head sample: 87.85%
further optimization studies.
Diesel Products Wt., Ash, Ash CR, AR, EI

3.3 Effect of single reagent Sokem 705C dosage, kg/t

0.198 Concentrate
%

13.88
%

34.42
Distribution, %

5.45
%

73.81
%

94.55 68.36

Tailing 86.12 96.25 94.55

The primary grind (d80: 242 µm) and sodium 0.231 Concentrate 14.52 38.45 6.33 75.33 93.67 69.00

silicate dosage (3 kg/t) were optimized. Further Tailing 85.48 96.58 93.67

0.265 Concentrate 15.43 38.74 6.85 74.32 93.15 67.47

flotation tests on single reagent Sokem 705C Tailing 84.57 96.13 93.15

dosage variation were carried out to study its 0.330 Concentrate 15.00 38.00 6.51 75.12 93.49 68.61

Tailing 85.00 96.37 93.49

effect and the results are given in Table 5.

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 MPT-2013

From the results, the diesel dosage is optimized Table 8: Comparison of reagents
at 0.198 kg/t as the ash rejection is maximum in consumption at rougher flotation of graphite
the tailings at 94.55% with relatively good Reagent dosage, Products Wt., Ash, Ash CR, AR, EI
efficiency index of 68.36 at relatively lower kg/t % % Distribution, % % %

diesel consumption. Optimization of pine oil Diesel: 0.198

Pine oil: 0.154
Concentrate 13.88 34.42 5.45 73.81 94.55 68.3
6
Tailing 86.12 96.25 94.55
dosage was carried out at this diesel dosage. Sokem 705C: 0.137 Concentrate 15.12 26.69 4.63 86.67 95.37 82.0
4
3.5. Effect of pine oil Tailings 84.88 97.99 95.37

The primary grind (d80: 242 µm), sodium silicate From the above table, it can be observed that
dosage (3.0 kg/t) and diesel (0.198 kg/t) were the consumption of single reagent Sokem 705C
maintained the same. Flotation experiments on is relatively less as compared to diesel-pine oil
variation of pine oil dosage to study its effect system. The cost benefit analysis is given in the
were carried out and the results are given in following discussion. Also, the performance of
Table 7. Sokem 705C is superior to that of diesel-pine oil
Table 7. Effect of pine oil at primary grind on system as evident from the efficiency index
graphite flotation, Primary grind d80: 242 µm; values.
Sodium silicate: 3.0 kg/t; Diesel: 0.198 kg/t,
3.7 Regrinding of rougher concentrate
Ash of Head sample: 87.85%
followed by 5-stage cleaner flotation
Pine oil
dosage,
Products Wt.,
%
Ash,
%
Ash
Distribution, %
CR,
%
AR,
%
EI In the rougher flotation, it was seen that much
kg/t
of the gangue is rejected at the coarsest possible
0.154 Concentrate 13.88 34.42 5.45 73.81 94.55 68.36
size in the form of primary tailings. In order to
Tailing 86.12 96.25 94.55

0.185 Concentrate 14.40 37.63 6.17 73.87 93.83 67.70

further liberate the graphite values in the
Tailing 85.60 96.29 93.83
rougher concentrate, regrinding was carried
0.246 Concentrate 14.93 37.68 6.44 73.60 93.56 67.16 out. Hence, the rougher concentrate was
Tailing 85.07 96.08 93.56 subjected to regrinding for 40 minutes (d80:144
0.277 Concentrate 15.51 40.43 7.17 73.97 92.83 66.80
µm) in ball mill with 1.5 kg/t sodium silicate
Tailing 84.49 96.15 92.83
followed by 5-stage cleaner flotation. During
cleaner flotation, no reagent was added and the
From the pine oil optimization results, it is
result of cleaner flotation is given in Table 8.
observed that 0.154 kg/t dosage is sufficient for
providing good separation (EI: 68.36). As the Conditions during rougher flotation:
pine oil dosage is increased further, the Primary grind d80: 242 µm; Sodium silicate: 3.0
concentrate grade is found to be diluted. kg/t
Sokem 705C: 0.137 kg/t
3.6. Comparison of single reagent Sokem 705C Ash of Head sample: 87.85%
and diesel-pine oil system Conditions during cleaner flotation:
The flotation tests were also carried on graphite Regrind (rougher concentrate) d 80: 144 µm;
using diesel as collector and pine oil as frother sodium silicate: 1.5 kg/t
at a primary grind of d80: 242 µm and sodium
silicate dosage at 3.0 kg/t. The consumption of
reagent dosages at equivalent metallurgical
grade of the rougher concentrate was compared
as shown in Table 8.

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 MPT-2013

Table 9: Cleaner flotation of reground rougher The results of the plant trails indicates that the
concentrate efficiency of separation using single reagent
Products Yield, % Ash, % Sokem 705C is comparable in terms of yield and
Final. Conc. 12.03 3.22
ash content in the final concentrate. The
consumption of Sokem 705C is 266 cc/t of feed
Cleaner-V Tails 0.23 26.51
which is much less compared to that when
Cleaner-IV Tails 0.20 58.38
diesel and pine oil are being used in the plant.
Cleaner-III Tails 0.34 80.79
This single reagent doesn’t have adverse effect
Cleaner-II Tails 1.00 92.76 on the downstream operations in the plant such
Cleaner-I Tails 3.88 97.28 as thickener water quality. Also, the addition
Primary Tails 82.32 97.48 of this reagent also makes the operation easier.
From the above results, final concentrate of 4.1 Cost benefit analysis
12.03% yield with 3.22% ash content was
obtained after 5-stage cleaning of reground The cost and benefits analysis was carried out
rougher c onc entrate. The c ombustibles to compare the economic viability in using
recovery was found to be 82.03% and the single reagent in place of diesel-frother (pine
separation efficiency index of 81.58. oil) system. The throughput capacity of the
After the encouraging results on using single flotation circuit in the plant where trials were
reagent Sokem 705C in place of the dual reagent c arried out is 5.0 t/h. The reagents c ost
system at laboratory scale studies, it was estimation comparison for treating one tonne
thought prudent to test the same at commercial of graphite is given in Table 11.
plant level. Table 11: Cost benefit analysis for single
4. Plant trials using Sokem 705C reagent, Sokem 705C and diesel-frother system
After ensuring that the efficacy of single reagent
Sokem 705C is not inferior to that of the diesel- Parameters Values Cost (INR)

pine oil system in graphite flotation, trials were Feed rate (tonne/hour) 5.0 --

undertaken in an operating graphite flotation Diesel consumption (cc/t) 225 12.60

Frother (pine oil) consumption

plant in eastern India. The plant of 5.0 t/h (cc/t)
758 113.70

capacity involves multistage grinding-cum- Sokem 705C consumption (cc/t) 266 66.50
flotation. In this plant, diesel and pine oil are
being used as collector and frother respectively.
Plant trials were conducted using Sokem 705C It is evident that the cost of single reagent is
in this plant flotation circuit. The results of cheaper by half of the dual reagent cost per tonne
conventional plant practice with diesel and of feed. The reagent cost per day for Sokem 705C
pine oil system and single reagent Sokem 705C would be 7980 INR while that of diesel-pine oil
are comparable as shown in Table 10. system would be 15156 INR. This is over and
Table 10. Results of plant trials conducted above the reduced capital expenditure and
using single reagent Sokem 705C operational simplicity.

Yield, %
Reagent Dosage, cc/t Feed Ash, %
Final
Ash, %
Conc. Tailings Ash,
%
(graphite 5. Conclusion
recovery)

Sokem 705C
Diesel & pine
266 87.50 3.95 94.40 10.90
11.08
The single reagent Sokem 705C was evaluated
225 & 758 87.50 3.90 94.00
oil for its efficiency on graphite flotation both in

151

laboratory benc h scale studies and in an
operating graphite beneficiation plant. It was
found that single reagent was superior to the
conventional diesel-frother system, in terms of
cost benefit analysis. Flotation results also
indicate that the single reagent Sokem 705C is
superior to diesel-pine oil system. Considering
the plant operation point of view, handling
single reagent system is much easier than
compared to dual reagent system. This single
reagent Sokem 705C proves to be economical
compared to diesel-frother system. Moreover,
it is biodegradable and environmental friendly.
Acknowledgements
The authors wish to thank The Director, CSIR-
NML for his support and permission to publish
this work.
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

An Alternative for the Conventional Graphite Depressant in Lead

Zinc Flotation at H.Z.L’s Rampura Agucha

Jayesh B. Gakare, T. S. Anil Kumar Nistala, Ajit Swain and K. D. Sharma*

Central Research and Development Laboratory, Hindustan Zinc Ltd, Udaipur 313024,
Rajasthan, India

Abstract
In the ore of base metal sulfides (such as CuFeS2, PbS and ZnS), carbonaceous gangue is often
present. Relevantly, Rampura Agucha is a major Lead – Zinc deposit having 1.5-2.5% Lead, 10-
15% Zinc and 4-6% Graphitic Carbon and mineralogically fine liberated. Carbonaceous and
micaceous Gangue minerals tend to float along with the galena, during selective flotation of galena.
Graphitic Carbon has a property of floating independently of physico chemical conditions of the
pulp (Eh, Ph,..), which leads to the contamination of mineral concentrates. Therefore, to avoid this
inadvertent flotation, it is possible to separate graphite or carbonaceous minerals from the ores
by flotation at the conditions at which the valuable ore fractions do not float or to depress them
with a suitable reagent. The earlier case is not suitable for the RAM, as there is a slight loss in the
recovery of valuable metal sulphides into the concentrate. So, Nigrosene is used as the reagent to
depress the free carbonaceous matter. However, after being known the ability of Reagent X as
graphite depressant, we tested it on the Rampura Agucha ore and it worked instantly. This paper
deals with the lab scale test results and reagent’s performance in plant scale.

Keywords: Graphitic carbon; nigrosene; flotation.

1. Introduction with pyrite (FeS2) [2]. Minerals contaminated

by a carbon over layer floats independently of
Rampura Agucha deposit is fifth largest deposit
Eh conditions. Inadvertent flotation may lead
and third largest in terms of production of
to contamination of mineral concentrates. It is
contained lead zinc metals in the world. The
possible to separate graphitic carbon by
average percentage of minerals is Sphalarite:
flotation from ores at reduced Eh, i.e. at the
15-20%, Galena: 1-2%, Pyrite: 15-18%,
conditions where the valuable minerals will not
Pyrrhotite: 12-14%, Graphite: 4-7%, Gangue:
tend to float. But, through this there may be
45-50%. Out of all the gangue minerals, the
metal loss in the graphitic carbon concentrate.
mineral that causes the most disturbances in
An alternative to this is the use of suitable
the lead flotation is graphitic carbon.
c arbonac eous flotation depressants. The
In the flotation of base metal sulfides (such as
depressant chemicals (reagents) may be added
CuFeS2, PbS and ZnS), carbonaceous gangue is
to the flotation circuit or in the milling section
often present [1], and is frequently associated
without any plant modification. So this option
* Correspending Author: Dr. K. D. Sharma, Head-C.R.D.L,
is ec onomic ally acc eptable if significant
Central R&D Laboratory, Hindustan Zinc Ltd, Udaipur
313024, Rajasthan, India. E-mail: kd.sharma@vedanta.co.in improvements are possible.

154

1.1 Mechanisms of the interactions of organic
compounds with the graphitic carbon:
The theory which explains the adsorption of
the aqueous phases on the activated carbon is
Polanyi theory. Ac cording to the theory,
adsorption of an adsorbate by adsorbents
should be described in two aspects: adsorption
capacity and affinity. Adsorption capacity is
limited by the potential space of a sorbent
available for adsorption of a given adsorbate,
while adsorption affinity is dependent on the
strength of the attractive forces between
adsorbate and adsorbent.
The net attractive forces involving the solute,
solvent, and the adsorbent are assumed to be
responsible for the solute adsorption by
sorbents suc h as Graphitic c arbon and
activated carbon. Among these forces, Vander
Waals force is normally the dominant force for
gas or vapor adsorption onto a hydrophobic
adsorbent, which may also be significant for
adsorption from the aqueous phase.
Considering only vander Waals forc es,
however, may not be applicable in cases when
dipole-dipole, induced-dipole, and hydrogen-
bonding donor-acceptor interactions exist,
typically in aqueous phase, where these forces
can be important especially for chemicals with
c ertain func tional groups. Five possible
interactions including hydrophobic effect, ð-ð
bonds, hydrogen bonds, and covalent and
electrostatic interactions have been observed
and are responsible for the adsorption of
organic chemicals on Graphitic Carbon surface
(Yang, and Xing 2010). These interactions, their
strengths, and contribution to the overall
sorption are a function of the properties of both
organic chemicals and Graphitic Carbon.
1.2 Graphitic carbon depressants in the
conventional flotation:
The graphitic carbon depressants those are
been used in the mineral beneficiation flotation
155
MPT-2013
plants were like Nigrosine, Reagent X, Aero 633
(a spec ialist reagent produc ed by Cytec
industries), etc.,
At the benefic iation operations in the
Hindustan zinc limited’s mining site, the
conventional graphite depressant used since
ages is nigrosine. The Reagent X is found as
another graphite depressant from the literature
survey.
The possible c hemical structures of the
Nigrosine and Reagent X are as follows.
Figure 1: Chemical Structure of Nigrosine
2. Experimental Procedure
The experimental testing is done in two
conditions, open cycle batch flotation & closed
cycle batch flotation conditions.
The experimental proc edure for testing
conditions consists of 1. Sample preparation for
the flotation (c rushing & grinding), 2.
Differential flotation (open cycle batch flotation
& closed cycle batch flotation), 3. Generated
sample preparation for the chemical analysis.
Flotation kinetics tests were conducted in the
lead flotation. The rougher concentrates of lead
were collected in time interval of 20 sec for about
one minute.
The tec hnic al c onditions whic h were
maintained in the testing procedure are
1. Specific gravity of the slurry : 1.3-1.32
2. % passing 80 through 240# (mesh) or
63 microns.
3. Ore type (three ore types of RAM ore).

3. Results and Discussion
3.1. Open cycle batch flotation with first and
second ore types
The reagent combination for the lead and zinc
flotation is as follows. The regent combination
is the optimized combination.
Table 1: Reagent combination for the lead and
zinc flotation for the first and Second ore types
Table 2: Results with Nigrosine & Reagent X
for the first ore type
Table 3: Results with Nigrosine & Reagent X
for the Second ore type
The detailed flotation kinetic study was carried
out to have better emphasis on the performance
of the Reagent X and Nigrosine in lead and zinc
flotation.
Figure 2: The grade-recovery curves of the
graphite in lead flotation with Nigrosine and
Reagent X graphite depressants
156
MPT-2013
The above plots depict the grade recovery
curves of the graphite with the Nigrosine and
Reagent X. The grade recovery curves of both
the reagents were found to be of similar nature
in the first ore type, which indicates the
depression mechanism performance of the both
the reagents is at par. i.e, for any particular
grade of graphite in the lead concentrate the
recovery of the graphite is same with both the
reagents.
In the subsequent plot, the grade recovery curve
of the graphite with Nigrosine as depressant is
clearly above the grade recovery curve with
the Reagent X as graphite depressant. This
informs that for any arbitrary grade of the
graphite in the lead concentrate the graphite
recovery is less in case of the Reagent X to that
of Nigrosine
Figure 3: The Lead grade-Graphite recovery
curves in lead flotation with Nigrosine and
Reagent X graphite depressants
Figure 4: The Lead grade- recovery curves in
lead flotation with Nigrosine and Reagent X
graphite depressants
 MPT-2013

creates positive sense; this may be because of

its better depression of the gangue minerals
causing less misplacement of the same.
3.2 Open cycle batch flotation with third ore
type:
The reagent combination for the lead and zinc
Figure 5: The Zinc grade- recovery curves in flotation of the third ore type is as follows. The
lead flotation with Nigrosine and Reagent X regent c ombination is the optimized
graphite depressants combination.
Table 4: Reagent scheme for the open cycle
From the figure 4, the lead grade vs. recovery batch flotation of third ore type
curves indicates that the quality of the lead
concentrate that is produced is better in case of
the Reagent X than with the Nigrosine. i.e, for
any arbitrary lead recovery the grade of lead
rougher concentrate is more in case of Reagent
X. This can be related to the figure 3. The lead *Only in control tests
grade vs. graphite recovery curves with the
first ore type indicates that for any arbitrary
graphite recovery the lead rougher concentrate
grade was more in case of Reagent X during
initial stages. But, later both the reagents landed
at the same graphite recovery for the final lead
rougher concentrate grade.
But, with the second ore type the lead recovery Figure 6: Lead grade - recovery & lead grade –
vs. graphite recovery curve with Nigrosine as graphite recovery plots of the lead flotation in
graphite depressant is above the grade recovery both control and tests with Reagent X.
curve of the Reagent X. This indicates that for The present graphical chart depicts, that for an
any arbitrary lead rougher concentrate grade arbitrary grade of lead in its concentrate the
the graphite recovered is more in case of lead recovery is approximately similar. But,
Nigrosine. The graphite is better depressed in graphite recovery in the concentrate with the
case of the Reagent X in lead flotation than with Nigrosine as the graphite depressant is higher
the Nigrosine which resulted in the lower in comparison with that of the Reagent X.
misplac ement of the graphite in lead
concentrate. So, this may be one of the reasons
for lead grade recovery curve to be on the
higher side than the curve of the Nigrosine in
figure 4. Figure 5 indicates that the zinc
metallurgy is undisturbed in both the cases of
the reagents. That means for any arbitrary zinc Figure 7: Graphitic carbon grade – recovery &
rougher concentrate the recovery of zinc Time – graphite recovery plots during the lead
remained constant in both the cases. But visibly flotation in both control and tests with Reagent
the grade recovery curve with the Reagent X X.

157

The graphitic carbon recovery trend with that
of its grade is very similar in the both cases.
Where as its recovery with respect to the time
is low in case of the Reagent X with comparison
with that of the Nigrosine.
During this test work emphasis was on the
characteristics of the zinc flotation in both the
cases of the Nigrosine and Reagent X. So,
flotation kinetics tests were conducted in the
zinc flotation also. The rougher concentrates of
zinc were collected in time interval of 30 sec for
about two minutes. The following graphs and
plots will describe the effect of both the reagents
in zinc flotation post dosage.
Figure 8: Zinc & graphite grade – recovery
plots during the Zinc flotation in both control
and tests with Reagent X
The grade vs. recovery trend line of zinc in case
of the Reagent X is slightly over the trend line
of the Nigrosine. Which indicates the effect of
both the reagents is one and the same with
neglisable deviation. Also the grade recovery
c urve of the graphite with Nigrosine as
graphite depressant in the zinc flotation is over
the trend line of the Reagent X which informs
that for any graphite grade the graphite
recovery is more in case of the Nigrosine when
compared with that of the Reagent X.
Figure 9: Zinc grade – iron and graphite
recovery plots during the Zinc flotation in both
control and tests with Reagent X
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MPT-2013
For any partic ular zinc grade in zinc
concentrate the recovery of the iron (pyrite/
pyrrotite) is more in case of the Nigrosine. The
reason behind this is to be explored thoroughly.
But in case of the graphite the recovery of the
graphite is low even in zinc flotation in case of
the Reagent X for any particular zinc rougher
grade.
3.3. Closed cycle batch flotation
We have a mini closed cycle batch flotation
system facility at our laboratory which consists
of two flotation cell banks. One bank can be used
for the rougher and scavenging flotation and
the other bank as a cleaner flotation cell bank.
The system also contains a conditioning tank
which holds the slurry through constant
agitation. The slurry is transported to the cells
through peristaltic pumps.
The electricity supplied to the cells is Direct
Current which is transformed by the control
panel associated with the system. The launder
water addition is done manually with the wash
bottles.
The cell selection for the roughing stages and
the scavenging is very simple.
For the present study, for lead flotation the
rougher were 4 and scavengers were 2. And
two stage cleaning was done. 1st stage cleaning
is of two cells and the second stage comprises
of single cell. Similarly cell arrangement is for
the zinc flotation also.
Below is the picture of the mini closed cycle
batch flotation system facility.
Figure 10: Closed cycle batch flotation system
facility photograph.
The reagent scheme maintained for the closed
cycle flotation testing was given below.

Table 5: The reagent scheme for the closed
cycle flotation testing.
The following tables contain the results of the
test work with the Nigrosine and Reagent X as
graphite depressants.
Table 6: Closed Cycle Control Tests Results:
With Nigrosine @ 250 gpt in Lead Flotation
Table 7: Closed Cycle Tests Results: With
Reagent X @ 250 gpt in Lead Flotation
Observations
Lead Flotation:
From the results the graphite grade and
recovery in the lead concentrate is 5 & 2.86% in
Control Tests whereas with Reagent X tests 3.95
& 2.56%. The lead concentrate Grade and
Recovery in control tests are 56.88% & 55.26%,
whereas in tests with Reagent X 53.25% &
56.25%.
Zinc Flotation: From the results the graphite
grade and recovery in the Zinc concentrate is
1.53 & 9.12% in Control Tests whereas with
Reagent X tests 1.5 & 8.73%. The Zinc
concentrate Grade and Recovery in control tests
are 48.13% & 87.93%, whereas in tests with
Reagent X 49% & 89.16%.
3.4. Plant trial with the reagent
Plant trial was done with Reagent X in one of
our c irc uits at RAM. Initially, after the
introduction of the reagent into the circuit, we
left a period of about three hrs to get rid of the
effect of Nigrosine, after then sampling of the
*******
159
MPT-2013
streams was started. The hourly sample cuts
were made in to two shifts composites samples
(1.00 PM to 8.00 PM) and (8.00 PM to 2.00 AM).
Table 8: The mass balance results for the circuit
during the shift (1.00 PM to 8.00 PM)
Table 9: The mass balance results for the circuit
during the shift (8.00 PM to 2:00AM)
The samples thus c ollec ted were shift
composites and they were dried and then sent
for the chemical analysis. The analytical results
were then reconciled in the JK SimMet. The
reconciled data is tabulated in the above
displayed tables.
Observations: During plant trial, Reagent X &
Nigrosine were run for 16 & 8 hrs respectively.
The day average of lead concentrate is 55.6%
Pb (daily assay report), whereas with Reagent
X it is 56%. Similarly, the day average graphite
content in lead concentrate is 10%, where as
with naphthalene it is 8%. So graphite is
effectively depressed with Reagent X with no
significant deterioration in Pb Conc. grade.
4. Conclusion
From the open, closed cycle batch flotation test
work results & one day plant trial results it
was observed that the Reagent X is an efficient
graphitic carbon depressant which can be used
in the plant scale in place of the conventional
graphite depressant Nigrosine. The Reagent X
is cost effective when compared to that of the
Nigrosine.
References
Yang, K., and Xing, B., (2010), Adsorption of
Organic Compounds by Carbon Nanomaterials
in Aqueous Phase: Polanyi Theory and Its
Application ,Chem. Rev.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Hydrodynamics of Flotation Column Using Sphalerite Fines

Kamalendu Bhunia, Gautam Kundu and Dibyendu Mukherjee
Chemical Engineering Department, Indian Institute of Technology, Kharagpur-721302,
India, kamalendu.bhunia@rediffmail.com; gk@che.iitkgp.ernet.in;
dibyendu@che.iitkgp.ernet.in

Abstract

Recent research progress in mineral flotation in mechanical cell shows that flotation rate depends
on bubble surface area flux (Sb), which is defined by the total bubble surface area flows through
column cross sectional area per unit time, and that flux has strong correlation with gas holdup
(åg). Yet no experimental work on Sb has been made to sphalarite flotation in column cell. This
paper studies the hydro-dynamical effects on the flotation behavior of sphalerite in terms of gas
holdup, bubble size (db) and bubble surface area flux which are considered to be variables directly
associated with flotation kinetics and examines the link between them. A series of experiments
have been conducted using a laboratory flotation column (height 1.66 m, diameter 0.1 m) at
various slurry concentration, slurry flow rate, gas flow rate, etc. Experimental results obtained
in the column operating with three phases (slurry-gas) and a two phase (water-gas) systems has
been presented and discussed. Results indicate that åg and Sb increases with gas flow rate while
increase in slurry rate, slurry concentration and collection zone height inhibit these parameters.
Slurry flow rate enhances db which is also reduced at higher slurry concentration. A strong
correlation has been found between as holdup and bubble surface area flux.

Keywords: Flotation column; gas holdup; bubble surface area flux; sphalerite flotation.

flotation cells have resulted in important

1. Introduction
It is widely acknowledged that separation of
valuable mineral from gangue particles by
froth flotation is dependent on several factors.
One of the most important factors is the
hydrodynamic condition within flotation cells.
The recent studies performed regarding the
hydrodynamic characteristics of mechanical
* Correspending Author:Kamalendu Bhunia, Indian Insti-
tute of Technology Kharagpur, Chemical Engineering
Department, West Bengal, Kharagpur, 721302, India,
kamalendu.bhunia@rediffmail.com, Telephone: +91 3222
283934, Mobile: +91 9681304195
contributions to the understanding of the
flotation process (Nesset et al., 2006; Schwarz
and Alexander, 2006; Vinnett et al., 2012;
Yianatos et al., 2001). The main measurement
parameters whic h c harac terize the
hydrodynamic performance include superficial
gas velocity Ug (ms-1), bubble size db(m), gas
holdup åg(-) etc.
Bubble surface area flux Sb(s-1) which is the total
bubble surface area flowing across the cross
sectional area of the cell per unit time is
expressed in terms of these parameters and
presented by Equation (1).

160

6Ug
Sb  (1)
db
Superficial gas velocity is the ratio of gas flow
rate measured by gas flow meter to the cross
sectional area of column presented in Eq 2.
Qg
Ug  (2)
Ac
It has been demonstrated that Sb (s-1) describes
the hydrodunamic condition of the flotation
cells (both mechanical and column) (Xu et al.,
1991).
Several works have been conducted to study
the effect of bubble size on flotation efficiency.
Equation (3) describes the classical model for
kinetic rate constants in flotation systems
(Ahmed and Jameson, 1985; Dobby and Finch,
1986; Jameson et al., 1977; Yoon and Luttrell,
1989).
3 Ug
k . .E C .E A (3)
2 db
This equation indicates that the gas dispersion
plays a role in flotation rate through both the
mec hanic al proc esses (U g/d b) and the
elementary processes of particle collection.
Collection efficiency (Ek), which describes the
partic le– bubble interac tions, has been
represented as the produc t between the
collision efficiency EC (-) and the attachment
efficiency EA (-) (Duan et al., 2003).
In case of flotation column, the recovery of
mineral has been estimated using both the axial
dispersion model and the tank in series model.
Both models indicate that recovery enhances
with increasing rate constant k (s -1) and
residence time  (s) and decreasing cell
mixing. So, recovery can be represented as
R = f (k,  , cell mixing) (4)
Equation 5 describes kinetic rate constant (k) in
terms of Sb using Eqs. (1) and (3).
k = P.S (5)
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MPT-2013
P = Ek/4 (6)
where P (-) is the floatability factor of mineral
particles.
(Gorain et al., 1998 and Hernandez et al., 2003)
have reviewed effect of gas dispersion on
flotation rate (k). The study by (Massinaei et al.,
2009) is an example of the application of gas
dispersion analysis in industrial flotation
process. Many researchers have performed
experiments to establish k-Sb relationship in
different flotation cells (Gorain et al., 1997;
Heiskanen, 2000; Hernández et al., 2003;
Hernandez-Aguilar et al., 2005; Kracht et al.,
2005; Massinaei et al., 2009). The authors have
used the drift-flax model to estimate the average
bubble size in order to calculate Sb (s-1). Hence,
Sb (s-1) is an important parameter for flotation
process. In addition, (Yianatos and Contreras,
2010) have reported that S b (s -1) is a key
parameter for carrying capacity evaluation in
flotation equipment.
Therefore, it is essential to study the
hydrodynamic characteristics of column.
Besides bubble surface area flux, gas holdup is
also an important parameter that determines
the circulation and mixing patterns of gas
slurry dispersions. Therefore, it determines the
flotation efficiency and affects the residence
time of materials in the flotation system.(
Ahmed and Johnson 1989) have reported that
gas holdup favors flotation kinetics because it
increases the number of bubbles, and therefore
the superficial area available for particle
collection. (Barigou and Greaves et al., 1992)
have found that the presence of electrolytes give
rise to a considerable bubble coalescence
retardation which reflects the reduction of
bubble size and more uniform dispersions.
Bubble size strongly depends on the surface
tension of the used slurry and the utilized
bubble generation system (Chamarasa et al.,
1999). It has been found that the bubble size in
bubbly flow zone of a flotation column increase
with increasing distance from the bottom due
 MPT-2013

to coalescence, which in turn, indicates that the
characteristics of gas dispersion depend on the
axial position (Majumdar et al., 2006). In another
investigation, (Zhou et al. 1993). have reported
that a hydrophobic characteristic of particle
affects the gas holdup in flotation column. A
study on axial gas holdup profile in flotation
column has also been tested by (Zhou and
Egiebor 1993).
Henc e, it c an be seen that the overall
performance of a flotation process is affected
by the gas dispersion characteristics and
physicochemical characteristics of the system.
As a research focus, gas dispersion is also closely
related to fluid dynamics. Changing one
condition in flotation operation (e.g., gas
velocity) may lead to a significant change in
rate constant and c onsequently flotation
recovery. Thus, it is concluded that the gas
velocity has a significant effect on the flotation
W
rate. Likewise, changing slurry concentration
may lead to a change in recovery. However,
very limited information is available in the
literature regarding bubble surface area flux in
flotation column. Also, there are no literatures
available on sphalarite flotation. Therefore, this
study has been devoted to analyze this effect
on laboratory flotation column using Indian
sphalerite ore. This paper will also focus on
bubble size and gas holdup as well as bubble
surface area flux and gas holdup relationship.
2. Methods and materials
Flotation was carried out in the Perspex column
whic h is shown in Fig. 1. The detailed
specifications of the experimental column are
given in Table 1. Air compressor was used to
produce compressed air (at about 5 kg.cm -2)
which was passed through a c ylindrical
ceramic porous sparger (S, pore diameter of 0.9-

MF
M2 ST

FT
M1 S

BV
SLP
T
A
CP
SV
AR AC

Fig. 1: Schematic diagram of experimental setup

Legends: A: Air flow meter, AC: Air compressor, AR: Air regulator, BV: Butterfly valve,
C: Concentrate, CP: Centrifugal pump, FT: Feed tank, MF: Magnetic flow meter, M:
Motor, M1, M2: Pizometer, S: Sparger, SLP: Slurry pump, ST: Stirrer, SV: Solenoid
valve T: Tailings, W: Wash water

162
 MPT-2013

1.5 µm) producing air bubbles at the bottom of
the column. The feed flow rate was measured
by Magnetic flowmeter (MF). A calibrated gas
flowmeter and controller were used to measure
and control the air flow rate respectively. The
liquid level in the column was controlled by
adjusting the tailings flow rate using butterfly
valve. Piezometers (M1 & M2) have been
provided at the lower portion of column for
pressure drop studies. A butterfly valve (BV) is
also installed in the tailing line of column for
gas holdup study. Sphalerite from Hindustan
Zinc Ltd. (India) was used to prepare slurry for
flotation experiment. The size of the particles is
given in Table 2. The density of sphalerite was
3.16 gm/c m 3 , as determined by a gas
pycnometer.
Table 1: Laboratory columns specifications
Parameters Column
Diameter (m) 0.1
Height (m) 1.68
Gas sparger type Internal-porous ceramic
Feed point from sparger (m) 1.3
Table 2 :Particle size distribution of sample
Size (µm) Wt %
+150 1 1988).
-150 +106 1 Table 3: Operating variables of column
-106 +75 7 experiments
-75 +53 26
sparger by switching on the air compressor
before sending the feed to the column. The
column was operated continuously for about
30 min to reach steady state, which was
confirmed by constant flow of tailings and
froth. Wash water was not used to avoid
diluting the slurry. Moreover, the objective of
the work was focused on the phenomena
occurring in the collection zone, hence the role
and performance of the cleaning zone was not
of partic ular interest. All the tests were
performed at room temperature (25 - 30oC). The
ranges of operating variables utilized in
experiment are listed in Table 3. Phase
separation method was used to measure gas
holdup in the flotation column. Before gas
holdup measurement, sparger performance
was conducted using air-water and air-slurry
system. This test shows that there is no settling
or clogging of sparger. It is obvious that sparger
pore is much smaller than the solid particle (8-
15 µm). So, there was no possibility to clog the
sparger. Bubble surface area flux in various
experiments was calculated from Equation 1.
Bubble size was estimated using drift flux
analysis. This technique has been used to
estimate mean bubble size in flotation columns
(Banisi and Finch, 1994; Dobby et al., 1998; Li et
al., 2004; Xu and Finch, 1990; Yianatos et al.,
Parameters Column

-53 +38 10 Superficial gas velocity (cm/s) 0.64 – 2.76

-38 +25 20 Superficial feed/slurry velocity (cm/s) 0.64 – 2.76

-25 35 Slurry concentration (Kg /m 3 ) (mass of 0-10

solid/liquid volume)

Slurry of desired concentration (0-10 wt %) was

prepared. This prepared feed slurry was fed
using the slurry pump (Bornemann India,
Faridabad, India) to the flotation column at
desired feed flow rate. Air was supplied to the
3. Results and discussions
3.1 Effect of gas velocity
Figure 2 presents the gas holdup as a function
of superficial gas velocity showing that the gas

163
 MPT-2013

holdup increases as gas velocity increases due 3

to the fact that amount of gas increases in 2.5

Bubble diameter (mm)

column with gas flow rate. On the other hand,
2
for a given gas flow rate, increase in slurry flow
rate diminish gas holdup. At higher slurry 1.5
velocity more solid particles come into the Usl=2.12 cm/s
1
column which saturates the bubble surface and Usl=1.92 cm/s

0.5 Usl=1.48 cm/s

therefore increases bubble particle density. This
mineralized bubble particle in the tailing 0
stream is the main reason for lowering of gas 0 1 2 3
holdup. Similar study has been performed using Gas velocity X 10 (m/s)
-2

coal by (Shukla et al. 2010), and they have
reported the opposite effect of slurry flow rate
on gas holdup. This fact can be attributed to
the specific gravity of coal (1.6) being much less
than sphalerite (3.6). So, less dense mineralized
bubble present in column and slightly increase
gas holdup in case of coal.
0.18
0.16
0.14
as
Fig. 3 Effect of slurry flow rate on bubble
diameter
Figure 4 indicates the effect of gas velocity on
bubble surface area flux. The relationship
between Sb and Ug has been investigated for
mechanical cells and tank cells with the aim of
identifying the maximum value of Sb (Nesset et
al., 2006). In addition, Finch et al. reported that
Sb has a maximum value of about 110s-1 for gas
water system and 88 s-1 for slurry system (Finch

et al., 2000, Yianatos and Henriquez, 2007) have

d-

(-)
ol
G

u
p

0.12

0.1 indicated that a combination of bubble size in

0.08 the range of 1-1.5 mm with gas velocity of 1-2
0.06 cm s-1 produces Sb of 50 -100 s-1. According to
0.04 Usl = 2.12 Figure 4, the maximum value of Sb (82 s-1) for
cm/s
Usl = 1.48
0.02
cm/s
sphalerite flotation in column has been
0 observed. It is also found the Sb increase with
0 0.5 1 1.5 2 2.5 3
gas velocity almost linearly. Again, there is a
Superficial gas velocity X10 -2 (m/s)
decreasing effect of slurry flow rate on Sb at a
particular gas velocity.
Fig. 2 Effect of gas velocity on gas holdup
90

80
)

Usl = 2.12 cm/s

The behaviour of bubble diameter as a function
-1

70
Bubble surface area flux (s

usl = 1.91 cm/s

of gas veloc ity and slurry flow rate at a 60 Usl = 1.48 cm/s

particular slurry concentration (10 kg.m -3) has 50

40
been shown in Fig. 3. This figure shows that
30
bubble size slightly increases with increase in 20
gas velocity due to the higher probability of 10

bubble coalescence at higher gas flow rate. An 0

0 0.5 1 1.5 2 2.5 3
increase in slurry flow rate also causes the Gas velocity X 10-2 (m/s)

enhancement of bubble size. Fig. 4 Effect of gas velocity on bubble surface

area flux

164
 MPT-2013

3.2 Effect of collection zone height 3.3 Effect of slurry concentration

Another issue to address is collection zone Figure 7 presents the effec t of slurry
height. There is no publication on the effect of concentration on gas holdup. From the results
collection zone height on gas holdup and bubble shown in Fig. 7, a strong dependence between
surface area flux which have been presented in
the gas holdup and slurry concentration has
Figs 5 and 6 respectively. Decrease in gas holdup
and also Sb with increase in collection zone been observed. The result also shows that it
height was observed within the operating range decreases linearly with slurry concentration at
of gas velocity (Figs 5 and 6). In addition, about the partic ular gas flow rate. A physic al
14-20 % decrease in gas holdup has also been explanation for lowering gas holdup can be
found with increasing collection zone height by explained by the following phenomena.
38 cm. Gas holdup reduction can be attributed Bubbles in c olumn at higher slurry
to the fact that the gas distribution has concentration get more solid particles which
considerable effect on bubble behavior in imply more bubble-particle aggregate density.
column. The size of the bubble generated at the As a result of more bubble particle density, some
sparger is not equal to the equilibrium size in of the bubbles travel to the tailing stream which
the collection zone. Bubbles experience more
indicates the reduction of bubble concentration
hydrostatic pressure and forms smaller bubble
in collection zone. It has also been found that
size in case of higher collection zone height. The
probability of bubble coalescence also increases bubble size increases with slurry concentration
with increasing pressure as height of the column due to coalescence (Fig. 8). So, the residence time
increases. Therefore, coalescence effect produces of bubbles decrease and consequently rising
larger bubbles. The larger bubbles travel up velocity increases. Bubbles escape the column
faster through the column and results in which results in the lowering of gas holdup.
lowering of gas holdup. 0.2

0.18
0.18
0.16
0.16
Hc = 1.28 m 0.14 Ug = 0.64 cm/s
0.14
Gas holdup (-)

Hc = 1.66 m
0.12 Ug = 1.06 cm/s
0.12
Gas hold-up (-)

Ug = 1.48 cm/s
0.1
0.1 Ug = 1.91 cm/s
0.08 Ug = 2.33 cm/s
0.08
0.06 ug = 2.76 cm/s
0.06
0.04
0.04
0.02
0.02
0
0
0 5 10 15
0 1 2 3
-2
Slurry concentration (wt %)
Superficial gas velocity X 10 (m/s)
Fig. 5 Effect of gas collection zone height on Fig. 7 Effect of solid concentration on gas holdup
90 2.5
gas holdup 80
Bubble diameter (mm)

90
Bubble surface area flux (s )

2
-1

70
80 Hc=1.66 m
Bubble surface area flux (s -1)

60
70 Hc=1.28 m 1.5
50
60
40
50 1
30 Cs=5 wt%
40
Cs=10 wt%
20 0.5
30 Cs = 5 wt%
10
20 Cs = 10 wt%
0 0
10
0 0.5 1 1.5 2 2.5 3
0 Gas velocity X 10-2 (m/s)
0 0.5 1 1.5 2 2.5 3
Fig. 8 Effect of solid concentration on bubble size
Gas velocity X 10-2 (m/s)

Fig. 6 Effect of collection zone height on bubble and bubble surface area flux
surface area flux

165

Figure 8 presents the behaviour of bubble
diameter and bubble surface area flux as a
function of slurry concentration, showing that
Sb decreases as slurry concentration increases.
In addition, Figure 8 shows that bubble size
slightly increases with increase in gas velocity
and is affec ted by slurry c oncentration.
Relatively high mixing conditions at high gas
flow rate would enhance the probability of
bubble collision and coalescence which in turn
increases bubble size. It is also shown that
bubble size increases with increasing solids
content of slurry due to bubble coalescence. The
bubble diameter whic h is used in the
computation of the bubble surface area flux
varies from 1.6 mm to 2.4 mm (Fig. 8). In general,
reduction in bubble surface area flux can be
attributed to bubble size enhancement. Increase
in bubble size by inc reasing slurry
concentration has also been reported by direct
measurement of bubble size in flotation column
for pulp and paper slurry and in mechanical
cell (Grau, and Heiskanen, 2005; Reese et al.,
1996).
3.4 Bubble surface area flux and gas holdup
relationship
All the above plots suggest that there exists a
relationship between gas holdup and bubble
surface area flux. Figure 9 shows that gas
holdup and bubble surfac e area flux for
sphalerite flotation in column over a wide range
of operating conditions are linearly related
which was shown by the work performed by
Finch et al., (2000) for pilot scale flotation cell
and mainly mechanical flotation cell. The figure
indicates that the data are correlated by a
straight line presented in equation (7).
Sb  519. g (7)
-1
The slope of the above equation is 519 s , which
is nearly similar to the slope that reported by
(Finch et al. 2000) based on the analysis of the
166
MPT-2013
studies performed by (Szatkowski, 1987) in
mechanical flotation cell. Bubble surface area
flux has established a powerful way to
characterize floatation machine. This surface
area flux can be substituted with gas holdup
which has some advantage as it is easier to
measure in flotation cell. The above equation
will be useful for calculation of flotation rate
constant applying the measured gas holdup
data if the floatability of ore is to be known.
Fortunately a number of online gas holdup
measurement sensors have been developed in
recent years, so that it has become easier to
measure gas holdup (Gomez et al., 2003).
90
80
Bubble surface area flux (s )
S b = 519 εg
-1
70 R
2
= 0.99
60
50
40
30
20
10
0
0 0.05 0.1 0.15 0.2
Gas holdup (-)
Fig. 9 Bubble surface area flux and gas holdup
relationship
4. Conclusions
Fac tors that affec t the gas dispersion
characteristics are superficial gas velocity
determined by air flow rate, collection zone
height and slurry concentration quantified by
mass of solid per unit volume of water. These
properties of flotation column have been
studied using sphalerite ore. Observed results
for gas holdup, bubble surface area flux and
bubble size are from 4 % to 17 %, from 15 s-1 to
85 s -1and from 1.6 to 2.6 mm respectively,
within the operating range of gas velocity from
0.64 cm/s to 2.76 cm/s. Results also show that
bubble surface area flux is a function of gas
holdup through a linear relationship, which is
consistent with other studies. This linear

equation can be used to estimate flotation rate
constant using experimental gas holdup. The
identification of gas dispersion is useful for
process modeling and process control criteria
for industrial cells.
Acknowledgements
The authors would like to thank the Indian
Institute of Tec hnology, Kharagpur for
supporting this research.
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Sulphide Mineral Flotation – A New Insight into Oxidation

Mechanisms
Alireza Javadi Nooshabadi and Kota Hanumantha Rao*
Division Of Sustainable Process Engineering
Department Of Civil, Environmental And Natural Resources Engineering
Luleå University Of Technology, Se-971 87 Luleå, Sweden
Abstract
The formation of hydrogen peroxide (H2O2), an oxidizing agent stronger than oxygen, by sulphide
minerals during grinding was investigated. It was found that pyrite (FeS2), chalcopyrite (CuFeS2),
sphalerite (ZnS), and galena (PbS), which are the most abundant sulphide minerals on Earth,
generated H2O2 in pulp liquid during wet grinding in the presence and absence of dissolved oxygen
in water and also when the freshly ground solids were placed in water immediately after dry
grinding. Pyrite generated more H2O2 than the other sulphide minerals and the order of H2O2
production by the minerals was found to be pyrite > chalcopyrite >sphalerite> galena. The pH of
water influenced the extent of hydrogen peroxide formation where higher amounts of H2O2 were
produced at highly acidic pH. The amount of H2O2 formed also increased with increasing sulphide
mineral loading and grinding time due to increased surface area and its interaction with water.
The sulphide surfaces are highly catalytically active due to surface defect sites and unsaturation
because of broken bonds and capable of breaking down the water molecule leading to hydroxyl
free radicals. The type of grinding medium on formation of hydrogen peroxide by pyrite revealed
that the mild steel produced more H2O2 than stainless steel grinding medium, where Fe2+ and/or
Fe3+ ions played a key role in producing higher amounts of H2O2.
Furthermore, the effect of mixed sulphide minerals, i.e., pyrite–chalcopyrite, pyrite–galena,
chalcopyrite–galena and sphalerite–pyrite, sphalerite–chalcopyrite and sphalerite–galena on the
formation of H 2O2 showed increasing H 2O2 formation with increasing pyrite fraction in
chalcopyrite–pyrite composition. In pyrite–sphalerite, chalcopyrite–sphalerite or galena–
sphalerite mixed compositions, with the increase in pyrite or chalcopyrite proportion, the
concentration of H2O2 increased but with increase in galena proportion, the concentration of H2O2
decreased. By increasing the pyrite proportion in pyrite–galena mixture, the concentration of
H2O2 increased. Similarly, in the mixture of chalcopyrite–galena, the concentration of H2O2 increased
with increasing chalcopyrite fraction. The results of H2O2formation in pulp liquid of individual
sulphide minerals and in combination at different experimental conditions have been explained
by Eh–pH diagrams of these minerals and the existence of free metal ions that are equally
responsible for H2O2 formation besides the catalytic activity of surfaces. The results of the amount
* Correspending Author: Kota Hanumantha Rao
Tel.: +46920491705; Fax: +46920491199;
E-Mail: Hanumantha.Rao@Ltu.Se

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of H2O2 production also corroborate with the rest potential of the sulphide minerals; higher the
rest potential more is the formation of H2O2. Most likely H2O2 is responsible for the oxidation of
sulphide minerals and dissolution of non-ferrous metal sulphides in the presence of ferrous
sulphide besides the galvanic interactions.
This study highlights the necessity of revisiting the electrochemical and/or galvanic interactions
between the grinding medium and sulphide minerals, and interaction mechanisms between
pyrite and other sulphide minerals in terms of their flotation behaviour in the context of the
inevitable existence of H2O2 in the pulp liquid.

Keywords: Hydrogen peroxide; oxidation; pyrite; chalcopyrite; sphalerite; galena.

1. Introduction mineral, the second mineral oxidized more

Hydrogen peroxide, which is a strong oxidizing
agent, stronger than oxygen, causes non-
selective oxidation of sulphide minerals. The
oxidation of sulphide minerals takes place
during the grinding process when the particle
size is reduced for flotation. Recently it was
shown that formation of H2O2 take place in the
pulp liquid during wet grinding of complex
sulphide ore (Ikumapayi et al., 2012).Other
studies highlighted the significance of reactive
oxygen species (ROS), H 2O2 and hydroxyl
radical (•OH), generated from milled sulphide
concentrates and their potential effect on
thermophilic Fe- and S-oxidizing bioleaching
microorganisms through oxidative stress
(Jones et al., 2011; Jones et al., 2012). To date,
most studies dealing with sulphide mineral-
induced ROS formation have made use of
natural or synthetic mineral samples, of very
high purities, suspended in neutral solutions.
Pyrite induced ROS formation has been studied
most; however other sulphide minerals such
as chalcopyrite (CuFeS 2), sphalerite (ZnS),
pyrrhotite (Fe(1"x)S) and vaesite (NiS2) have also
been studied with respect to ROS generation
(Borda et al., 2001;Jones et al., 2011), and
reactivities have been found to differ between
sulphide minerals.
Buehler and Gottschalk (1910) noted that when
pyrite was mixed with a second sulphide
rapidly. Harvey and Yen (1998) observed that
addition of galena to the sphalerite selective
leaching system diminished the dissolution of
sphalerite. Alternatively, a pyrite or
c halc opyrite addition inc reased zinc
extractions. Many authors have reported that
galvanic interactions are known to occur
between conducting minerals and play a
significant role in flotation (Rao and Finch,
1988;Kelebek et al., 1996; Zhang et al.,
1997;Ekmekçi and Demirel, 1997; Huang and
Grano, 2005), leaching (Mehta and Murr, 1983;
Abraitis et al., 2003;Akcil and Ciftci, 2003),
supergene enrichment of sulfide ore deposits
(Thornber, 1975; Sato, 1992), environment
governance (Alpers and Blowes, 1994), and
geoc hemical proc esses (Sikka et al.,
1991;Banfield and Nealson, 1997). In addition,
other researchers (Koleini et al., 2010;Koleini et
al., 2011; Dixon and Tshilombo, 2005; Mehta and
Murr, 1983; Holmes and Crundwell, 1995)
reported when the amount of pyrite in contact
with chalcopyrite increases, the leaching rate
of chalcopyrite mineral increases.
The participation of H2O2 and•OH, if any, in
non-selective oxidation of the sulphide ore pulp
components and hence in deteriorating of the
concentrate grade and recovery of metal-
sulphides has not yet been explored. Likewise,
the influence of H2O2 has been recognized lately
on bioleaching of metal sulphides (Jones et al.,

170

2012). In an attempt to fill the gap, we have
estimated the concentration of H2O2 in pulp
liquid during different times of grinding and in
different grinding environments. The effects of
pH, type of grinding (wet or dry grinding), and
varying proportion of pyrite, chalcopyrite and
galena mixed with sphalerite on the formation
of hydrogen peroxide were investigated and the
results have been presented and discussed in
this paper in the context of flotation and leaching
phenomena of sulphide minerals.
2. Experimental
2.1 Materials and reagents
Crystalline pure sphalerite (Sp), galena (Ga),
pyrite (Py) and chalcopyrite(Cp) minerals used
in this study were procured from Gregory,
Bottley& Lloyd Ltd., UK. Sphalerite contains
39.92% Zn, 20.7% S, 4.2% Fe, 1.32% Pb and 0.17%
Cu. Galena contains 73.69% Pb, 13.5% S, 1.38%
Fig. 1. XRD analysis of the sample (a) pyrite (1- pyrite). (b) chalcopyrite (1- chalcopyrite and 2-
pyrrhotite 3- sphalerite) (c) sphalerite (1- sphalerite 2- galena 3- quartz), (d) galena (1- galena 2-
sphalerite 3- quartz).
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MPT-2013
Fe, 1.26% Zn, 0.2% Cu and some silica (quartz)
impurity. Pyrite contains 44.4% Fe, 50.9% S, and
0.2% Cu, and chalcopyrite contains 29% Fe,
29.5% S, 25.8% Cu, 0.54% Zn, and 0.22% Pb. The
XRD analyses of the samples showed that the
main mineral phases present were pyrite (Fig.
1a), chalcopyrite (Fig. 1b), sphalerite (Fig. 1c),
and galena (Fig. 1d) in the respective mineral
samples. All the mineral samples used in this
study were separately crushed through a jaw
crusher and then screened to collect the –3.35
mm particle size fraction. The homogenized
sample was then sealed in polyethylene bags.
Potassium amyl xanthate (KAX) was used as
collector and the frother was MIBC in flotation
tests. Solutions of sodium hydroxide (AR grade)
and HCl (1 M) were added to maintain the pH
at the targeted value during flotation. Deionised
water was used in both grinding and flotation
processes. Solutions of 2, 9-dimethyl-1, 10-
phenanthroline (DMP),copper (II) (0.01 M), and

phosphate buffer (pH 7.0) were used for
estimating the amount of H2O2 in the pulp liquid
by UV-Visible spectrophotometer (Baga et al.,
1988). Zinc sulphate, copper sulphate, lead
nitrate, ferrous sulphate and ferric sulphate
chemicals were also used to investigate the
effect of metal ions (Zn2+, Cu2+, Pb2+, Fe2+ and Fe3+)
on the formation of H2O2.
2.2 Dry grinding
100 g of –3.35 mm size fraction of pure
sphalerite, pyrite, galena and chalcopyrite
minerals in each grinding test were separately
ground in a laboratory stainless steel ball mill
(Model 2VS, CAPCO Test Equipment, Suffolk,
UK) with stainless steel medium for 60 min. 5 g
of sphalerite, galena, pyrite or chalcopyrite
single mineral and 12.5 g of mineral mixture
either sphalerite-pyrite or sphalerite-
chalcopyrite or sphalerite-galena or galena-
pyrite or galena-chalcopyrite or chalcopyrite-
pyrite that was < 106 µm was mixed with 50
cm3 water using magnetic stirrer and then the
slurry sample was collected at 0.5, 5 and 11 min,
filtered and was analysed for hydrogen
peroxide. The pH was regulated with HCl and
NaOH solutions.
2.3 Estimation of hydrogen peroxide
The spectrophotometric method of using
copper (II) ions and DMP has been found to be
reasonably sensitive when applied to advanced
oxidation processes (Kosaka et al., 1998).For
DMP method (Baga et al., 1988), 1 mL each of 1%
DMP in ethanol, 0.01M c opper (II), and
phosphate buffer (pH 7.0) solutions were added
to a 10 mL volumetric flask and mixed. A
measured volume of liquid (filtrate) sample was
added to the volumetric flask, and then the flask
was filled up with ultrapure water. After
mixing, the absorbance of the sample at 454 nm
was measured with DU ® Series 700 UV/Vis
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MPT-2013
Scanning Spectrophotometer. The blank
solution was prepared in the same manner but
without H2O2.
3. Results and discussion
3.1 Formation of hydrogen peroxide (H 2O2)
after dry grinding and mixing with water
Formation of hydrogen peroxide was observed
when the freshly dry-ground solids were mixed
in water. The effect of pH of the mineral
suspension on the formation of hydrogen
peroxide is shown in Fig. 2. It can be seen that
for pyrite, chalcopyrite and sphalerite with an
increase in pH, the concentration of H 2O2is
decreased up to pH 8 and then is increased
above this pH, but in the case of galena, H2O2is
generated at pH <4.5 only. Further, pyrite
generates more H2O2 than the other minerals.
Kocabag et al. (1990) using the Eh-pH diagram
(Fig. 3a) of pyrite showed that oxidation of
pyrite yields S°, Fe 2+, Fe (OH)2+ species in the
solution for pH < 6 and Fe (OH)2 ,Fe (OH)3 species
in the solution for pH > 6. At pH < 6, Fe2+ ions are
increased with decreasing pH and therefore, in
the presence of dissolved molecular oxygen,
ferrous iron associated with pyrite can form
superoxide anion (O2•)” (eq. 1), which reacts
with ferrous iron to form H2O2 (eq. 2) as shown
in Fig. 4a (Cohn et al., 2006).
FeII(pyrite) + O2’ FeIII(pyrite) + (O2•) (1)
FeII(pyrite) + (O2•) + 2H+’ FeIII(pyrite) + H2O2 (2)
Fig. 2. Effect of pH on production of H2O2 after 5
min mixing of dry ground solids with water.

Fe (III) can also generate H2O2in such a way that
an electron is extracted from water and a
hydroxyl radical is formed (eq. 3).Combining
two hydroxyl radicals leads to the formation
of H2O2 (eq. 4) (Borda et al., 2003):
III + II
Fe + H2O’OH + H + Fe
•
2 OH ’ H2O2
Fairthorne at al. (1997) using the Eh–pH stability
diagram of chalcopyrite (Fig. 3a) exemplified the
formation of insoluble ferric oxide/hydroxide
at neutral and basic pH values but also in acidic
conditions at high E hvalues. Notably the
divalent Fe and Cu ions exist at low pH values
from negative to high Eh values. These divalent
ions are reported to aid the formation of H2O2
(Valko et al., 2005; Jones et al., 2011; Jones et al.,
2012) from water and our present results shown
in Table 1 demonstrate that Fe2+ ions generate
substantial H2O2 followed by Fe3+ and Cu2+ ions.
Fig. 3b displays that the concentration of ferrous
ions decreases at the expense of ferric oxide/
hydroxides at higher pH and Eh values (oxygen
conditioning).The schematic diagram of H2O2
formation in the presenc e of dissolved
molecular oxygen is shown in Fig. 4b, where at
acidic pH (pH < 5) superoxide anion (O2•) “ (eq. 5)
is formed, which reacts with ferrous iron to
form H2O2 (eqs. 6-8). This is in agreement with
other studies where it was observed that metal
ions-induced formation of free radical has been
evidenced and that ferrous ion generates
superoxide and hydroxyl radical (Valko et al.,
2005; Jones et al., 2011).
Table 1. H2O2 generation in the presence of
metal ions at natural pH and at 22 °C.
H2O 2 (mM)
Concentration of
ions 1 mM 10 mM
water 0 0
Fe 2+ 0.552 4.656
Fe 3+ 0.004 0.059
Cu 2+ 0 0.015
Pb2+ 0.013 0.096
Zn 2+ 0.004 0.088
MPT-2013
O2 +Fe2+ ’ Fe3++ (O2•) “ (5)
(O2•) “ + Fe2+ + 2H+’Fe 3++H2O2 (6)
2+ 3+ • ”
Fe + H2O2’ Fe + OH + OH (7)
2•OH ’ H2O2 (8)
(3) Above pH 5, the stability diagram shows the
(4) Fe2O3 solid phase, that also generates hydrogen
peroxide. This is in agreement with other
studies where hematite and magnetite solids
in water were shown to induce H2O2 formation
(Cohn et al., 2006).Fig. 4b exhibits that copper
ions also generate hydrogen peroxide. The metal
ions induced formation of hydroxyl free radical
has been established, where copper ions
generate the superoxide and hydroxyl radical
(eqs. 9-12) (Valko et al., 2005).
O2 + e”’! O2•– (9)
2O2•– + 2H+ ’ H2O2 +O2 (10)
Cu++ H2O2=Cu2++ •OH + OH– (11)
2•OH ’ H2O2 (12)
In acidic pH, the formation of higher amounts
of hydrogen peroxide compared to that at
alkaline pH is due to the presence of copper and
ferrous ions in acidic pH, which are capable to
generate hydrogen peroxide (Table 1).
Huai Su(1981) showed by the Eh-pH diagram
of sphalerite that at pH < 6, Zn2+ and Fe2+are
formed (Fig. 3c). Table 1 show that Zn2+ and Fe2+
ions generated H2O2. In the presence of dissolved
molecular oxygen, ferrous iron can form
superoxide anion (O2•) “ (eq. 5), which reacts
with ferrous iron to form H2O2 (eq. 6). Also Zn2+
ions can form superoxide anion (O2•) “ to form
H2O2 (eq. 13) as shown in Fig. 4c .
2(O2•) +2H+’H2O2+O2 (13)
Woods (1981) by the Eh-pH diagram (Fig. 3d) of
galena showed that at pH < 4, Pb2+ ions exist.
Fig. 4d shows that in the presence of dissolved
molecular oxygen and in acidic pH (pH < 4), lead
ions can form superoxide anion (O2•)” which
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 MPT-2013

reacts with H+ to form H2O2 (Eqs. 14-17). It can generate superoxide and hydroxyl radical
be seen from Table 1 that Pb 2+ ions generate (Ahlberg and Broo, 1996a; 1996b; 1996c).
H2O2 (Blokhina et al. 2001; Ni et al. 2004). This is O2 + e”’ (O2•) “ (14)
in agreement with other studies where metal 2(O2•) “ + 2H+’ H2O2+O2 (15)
ions induced formation of free radicals has been PbS + H2O2’ Pb2+ +S0+2e”+2 •OH (16)
significantly evidenced for Pb 2+ ions that 2•OH= H2O2 (17)

(a) (b)

(d)
(c)

Fig. 3. a)Eh–pH stability diagram for the Cu–Fe–S–H2O system with the preponderant copper
and iron species shown in each domain (Fairthorne et al. 1997) b)Eh–pH diagram for FeS2–H2O
system at 25 0C and for 10-5M dissolved species (Kocabag et al. 1990). c)Eh–pH stability diagram
for the sphalerite–H2O system (Huai Su, 1981)d) Eh–pH diagram for the Pb–S–H2O system
where [Pb] =10-3 M (Woods, 1981).

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 MPT-2013

(a) (b)

(c)
(d)

Fig. 4. Proposed mechanisms for formation of H2O2 by a) chalcopyrite b) pyrite c) sphalerite d)

galena. The numericals in this figure represent the equation numbers.
For investigation of the effect of mineral loading,
they were mixed with 50 ml water at pH 4.5.
The concentration of H 2O 2 increased with
increasing loading as shown in Fig. 5. Fig. 6
shows that the c onc entration of H 2O 2 is
increased with increasing mixing time, most
likely due to increased minerals interaction
with water.
Fig. 6. Effect of mixing time on H2O2 production
at pH 4.5.

3.2. Effect of minerals mixture on formation of

H 2O 2

Fig. 7 shows the effect of pyrite–chalcopyrite,

pyrite–sphalerite, pyrite–galena, chalcopyrite–
Fig. 5. Effect of solids loading on H2O2 production sphalerite,chalcopyrite–galena or sphalerite–
after 5 min mixing with water at pH 4.5. galena mixture on formation of hydrogen

175
 MPT-2013

peroxide at pH 4.5. Fig. 7a shows the effect of
pyrite or sphaleritepercent in sphalerite–pyrite
mixture on the formation of hydrogen peroxide.
It can be seen that with an increase in pyrite
percent, the concentration of H2O2is increased
but with an increase in sphalerite percent, the
concentration of H2O2is decreased. This result
of non-ferrous metal sulphide oxidation with
increasing pyrite fraction could be due to the
increased H 2O 2 generation and that of an
increase in the rate of sphalerite leaching with
increasing pyrite proportion (Harvey and Yen,
1998). This is in agreement with other studies
where it was shown that the oxidation of
sphalerite increases with increasing hydrogen
peroxide concentration (Adebayo et al., 2006;
Aydogan, 2006).
Fig. 7b shows the effect of chalcopyrite or
sphalerite percent in sphalerite–chalcopyrite
mixture on the formation of hydrogen peroxide
where an increase in chalcopyrite percent
increases the concentration of H2O2 but with

Fig. 7. Effect of percent of a) Sp or Py b) Sp or Cp c) Sp or Ga d) Ga or Py e) Cp or Ga f ) Cp or Py in

their mixture on H2O2 formation with total 12.5 g sample after 5 min conditioning in water at pH
4.5.

176

an increasing sphalerite percent in the mixture,
the concentration of H 2O2is decreased. This
result of increasing chalcopyrite proportion
leading to an increase in the formation of
H2O2can be explained by the observation of
increased leaching rate of sphalerite with an
increase in chalcopyrite proportion (Harvey
and Yen, 1998).
Fig. 7c shows the effect of galena or sphalerite
percent in sphalerite–galenamixture on the
formation of hydrogen peroxide. It can be seen
that with an increase in galena percent, the
concentration of H2O2is decreased but with an
increase in sphalerite percent, the concentration
of H 2O 2is increased. This result could be
attributed to a decrease in the rate of sphalerite
leaching with increasing galena proportion
(Harvey and Yen, 1998).
Fig. 7d shows the effect of pyrite or galena
perc ent in galena–pyrite mixture on the
formation of hydrogen peroxide. It can be seen
that with an increase in pyrite percent, the
c onc entration of H 2O 2 inc reases but by
increasing galena percent, the concentration of
H2O2 decreases.
Fig. 7e shows the effect of chalcopyrite or galena
percent in galena–chalcopyrite mixture on the
formation of hydrogen peroxide. It is evident
that by increasing chalcopyrite percent, the
concentration of H2O2 increases. However, by
an increase in galena percent in the mixture,
the production of H2O2 decreases. This result
could perhaps explain that galena has no effect
on the kinetics of chalcopyrite leaching (Nazari
et al. 2012).
Fig. 7f shows the effect of pyrite or chalcopyrite
percent in chalcopyrite–pyrite mixture on
formation of hydrogen peroxide that with an
increase in pyrite percent, the concentration of
H 2 O 2 inc reases but with an inc rease in
chalcopyrite percent, the concentration of H2O2
decreases. The increase in the concentration of
H2O2due to the increase in pyrite proportion
could be explained by the fact that as the
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MPT-2013
amount of pyrite in contact with chalcopyrite
increases, the leaching rate of chalcopyrite
increases (Koleini et al. 2010;Koleini et al.
2011;Dixon and Tshilombo, 2005;Mehta, and
Murr 1983;Holmes and Crundwell, 1995).
Fig. 8 shows the effect of single or mixture of
minerals on the formation of hydrogen peroxide
at pH 4.5. It can be seen that pyrite and a mixture
of pyrite and other sulphide minerals generated
more H2O2. This is in agreement with other
studies where it was noticed when pyrite was
mixed with a second sulphide mineral, the
second mineral oxidized more rapidly (Buehler
and Gottschalk, 1910). The formation of higher
amounts of H2O2 when pyrite was mixed with
a second sulphide mineral may explain the effect
of interaction between pyrite and second
sulphide mineral on flotation, leac hing,
environment governance and geochemical
processes while the entire literature describes
so far of galvanic interaction between two
contacting sulphide minerals and electron
transfer from one to the other (Rao and Finch,
1988; Kelebek et al. 1996; Zhang et al. 1997;
Ekmekçi and Demirel, 1997; Huang and Grano,
2005; Mehta and Murr, 1983; Abraitis et al.
2003;Akcil and Ciftci, 2003; Thornber, 1975; Sato,
1992;Alpers and Blowes, 1994; Sikka et al. 1991;
Banfield and Nealson, 1997).
Fig. 8. Effect of minerals either individually or
in their mixture on H2O2 formation with 12.5 g
blend sample after 5 min conditioning in water
at pH 4.5.

So far two mechanisms have been proposed for
the action of microorganisms that increases the
leaching rate of metals from ores over that due
to purely physico-chemical processes. In direct
action, microorganisms will directly oxidize
minerals and solubilize metals (eqs. 18-19) (Fig.
9a):
MS+H2SO4+ (1/2) O2’MSO4+S0+H2O (18)
S0+ (3/2) O2+H2O’H2SO4 (19)
Where M is a divalent metal. In indirect action
of microorganisms, ferric ion (Fe 3+) is the
oxidizing agent for minerals and the role of
organisms is simply regeneration of Fe3+ from
Fe2+ (eqs. 20-21)(Fig. 9b):
MS+2Fe3+’M2++2Fe2++S0 (20)
2Fe2++ (1/2) O2+2H+’2Fe3++H2O (21)
In the actual microbial leaching of metals, both
direct and indirect leaching as well as physico-
chemical reactions can contribute (Suzuki,
2001). (Ehrlich,1999) mentions a number of
studies in support of the direct cell attachment
on the surface of minerals and the role of
Fe3+bound on the cell surface for sulphide
oxidation. Fowler and Crundwell (1998)
concluded that the leaching of zinc from
sphalerite (ZnS) by T. ferrooxidans was strictly
by indirect mechanism and the only bacterial
contribution was the regeneration of Fe3+ from
Fe2+ (eqs. 22-23):
(a) (b)
Fig. 9. Proposed mechanisms of microorganisms for oxidize minerals by a) direct action b) indirect
action c) both indirect action and formation of H2O2.
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MPT-2013
2Fe2++ (1/2) O2+2H+’2Fe3++H2O (22)
ZnS+2Fe3+’Zn2++S0+2Fe2+ (23)
Sand et al. (1995) suggested that bacterial
leac hing of metal sulphides proc eeds
essentially by indirect mechanism initiated by
ferric ion, Fe3+. Sand and colleagues (Gehrke et
al. 1998;Sand et al. 1995;Sand et al.
1999;Schippers and Sand, 1999) consider all of
these bacterial contributions as ‘indirect.’ It is
c urrently believed that the leac hing of
sphalerite proceeds according to an indirect
mechanism (Boon et al. 1998; Fowler and
Crundwell, 1998), and it has been postulated
that this mechanism is applicable to all other
sulphide minerals of the form Me2+S2"(Boon and
Heijnen, 1993), such as galena. Using these
routes, bacteria are thought to accelerate the
reaction rate by oxidizing the elemental
sulphur product layer (Boon et al. 1998).
It is worth mentioning that H2O2 could also be
the oxidizing agent for minerals and the role of
organisms is simply generation of Fe3+ ions, and
Fe2+ ions can generate H2O2 as shown in Fig. 9c .
The concentration of H 2O2 generated from
contacting Fe 2+ ion with water for 1 h, is
presented as a function of Fe2+ concentration in
Table 1. This is in agreement with other studies
where the dissolved ferrous iron concentration
was found to be an important secondary factor
contributing towards ROS generation (Jones
et al. 2012).
(c)

4. Conclusions
In the scope of this paper, fundamental studies
were carried out to resolve or reveal one of the
main problems, i.e., oxidation, in sulphide ore
flotation. For this reason, the oxidation of
sulphide mineral at the grinding stage was
evaluated. For the first time in mineral
processing applications, it was found that
during grinding (especially fine grinding)
formation of H 2O2 in pulp liquid takes place. It
is known that hydrogen peroxide is a strong
oxidizing agent and can easily oxidize sulphide
minerals and can even cause dissolution of
some metal ions from ore surface. That’s why
H2O2, rather than oxygen, can be the main
reason for oxidation, inadvertent activation and
non-selectivity in the sulphide ore flotation.
Prevention or reduction of H2O2 formation may
result in improved flotation results and we are
working on these aspects.
The following preliminary conclusions were
drawn from the results of our initial
investigations. Formation of hydrogen peroxide
takes place in the pulp liquid and its significance
in mineral processing applications hitherto not
considered in flotation literature has been clear.
It was found that pyrite, c halc opyrite,
sphalerite, and galena generated H2O2 in pulp
liquid during wet grinding in the presence or
devoid of dissolved oxygen in water and also
when the solids were plac ed in water
immediately after dry grinding. Pyrite
generated more H2O2 than other minerals and
the order of H2O2 production by the minerals is
found to be pyrite > chalcopyrite >sphalerite>
galena. The pH of water influenced the extent of
hydrogen peroxide formation where higher
amounts of H2O2 are produced at highly acidic
pH. H 2 O 2 c onc entration inc reased with
increasing conditioning time and solids loading.
H 2O 2formation increased with inc reasing
pyrite fraction in chalcopyrite-pyrite, pyrite–
galena and sphalerite–pyrite compositions.
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MPT-2013
Also with increasing chalcopyrite fraction in
chalcopyrite–sphalerite and chalcopyrite–
galena mixtures, the concentration of H 2O2
increased but with an increase in galena
proportion in galena–sphalerite mixture, the
concentration of H2O2 decreased.
Acknowledgements
Financial support from the research Centre for
Advanced Mining and Metallurgy (CAMM),
Luleå University of Technology, Luleå, Sweden,
and Boliden Mineral AB, Boliden, Sweden, is
gratefully acknowledged.
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Optimisation of Operating Variables in Cassiterite Flotation

Ho-Seok Jeon1*, Sang-Ho Baek2, S. I. Angadi3 and B. K. Mishra3

1
Korea Institute of Geoscience & Mineral Resources, Daejeon 305-350, Korea
2
University of Science and Technology, Daejeon, 305-350, Korea
3
CSIR-Institute of Minerals and Materials Technology (CSIR-IMMT), Bhubaneswar, India

Abstract
Gravity concentration was the only process for the beneficiation of tin ores till 1970s. Later,
introduction of chemical reagents such as sulphosuccinamates, phosphonic acid and arsonic
acid for collection of cassiterite mineral lead to the introduction of flotation. Nowadays, gravity
concentrators and flotation cells became prime beneficiation units in many tin plants in the
world.
Flotation is a physico-chemical process of separation of hydrophobic particles from hydrophilics.
The hydrophobic particles collected at the froth phase whereas the hydrophilic remained in the
pulp. In the present investigation cassiterite sample containing 6.39 % Sn, 59.1 % SiO2, 13.4 %
Al2O3, 5.2 % Fe was collected from Uljin deposit, South Korea. The feed material has been subjected
to X-ray diffraction and analysed that the tin mineral present in the ore is cassiterite, which is
assaying about 7.2 %. The gangue minerals present in the sample are quartz, albite, biotite,
hornblend, and chlorites. Batch flotation experiments were performed on a self-aerated laboratory
Denver flotation machine by varying different types of collectors, collector dosage, slurry pH,
dispersant dosage etc. the results indicate that a product grade of 44-45 % Sn with recovery of 93-
94 % could be recovered at optimized levels of operating parameters.

Keywords: Cassiterite, Flotation, AERO-6493, Oleic Acid.

1. Introduction
The important property of the tin metal like
malleability, ductility, and non-oxidizing in air
made it suitable for metal coatings, which helps
to prevent corrosion. The tin was used in
alloying with copper to form bronze metal that
found wide applications like making weapons,
metal objects, sculptures, cutting tools etc.
during the Bronze Age. The melting point of the
metal is very low of about 232 0C, when made
alloy with lead, the temperature further
* Correspending Author: Ho-Seok Jeon, Principal Researcher,
Korea Institute of Geoscience & Mineral Resources, Daejeon
305-350, Korea, Email: hsjeon@kigam.re.kr
reduces to 183 0C and is largely used in soldering
in electronics and plumbing applications. The
metal finds many more applic ations in
chemical, alloy making, decorative metals etc.
China is the leading producer of tin followed
by Indonesia, Peru, Bolivia, Brazil, and Congo.
Minor amount of tin production is also reported
from Australia, Portugal and many other
countries. The primary production of the
refined tin of 320,000 tonnes from the world
reserves could not meet the demand during the
year 2009, as a result, the tin consumers have
utilized 59,000 tonnes of refined tin from the
secondary sources like

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alloys and scraps. The demand for tin is present in the ore are quartz, albite, biotite,
increasing day-by-day due to increased end hornblend, and chlorites.
uses of the metal. Table 2. X-ray Diffraction analysis of the feed
The cassiterite ore beneficiation flowsheet material
mostly incorporates the combination of gravity
concentrators and flotation cells (Falcon, 1982). Mineral Chemical formula Weight %
The coarse particles would be recovered using Quartz SiO2 37.5
jigs while the fines recovered by spirals, gravity NaAlSi3O8
tables and flotation cells. In the present Albite or 22.1
Na1.0-0.9 Ca0.0-0.1 Al1.0-1.1 Si3.0-2.9 O8
investigation cassiterite ore containing 6.39 %
Biotite K(Mg,Fe)3(AlSi3O10)(F,OH)2 17.7
Sn collected from Uljin deposit, South Korea has
Hornblend Ca2(Mg, Fe, Al)5 (Al, Si)8O22(OH)2 13.6
been subjected for flotation studies to enrich Denver
Cassiterite SnO2 7.2
the tin content.
Chlorite (Fe, Mg, Al)6 (Si, Al)4 O10 (OH)8 1.9
2. Materials and Methods 100
The cassiterite sample collected from Uljin
mine, South Korea for the present research sub-aeration flotation machine was used in the
work. The tin occurrence is a hard rock deposit investigations. The cell capacity of 2 lit was used
along with pegmatite host rocks. As collected in all optimization and rougher flotation
sample was subjected to Jaw crusher followed studies, whereas, cleaning operation has been
by cone crusher to reduce the particle size. carried out in 1.2 lit capacity cell. Different
Hence produced material has been sampled and operating variables and reagents and their
was used for the following characterization levels studied are also summarized in the
studies. succeeding section. Following chemicals are
The chemical analysis of the cassiterite feed used in the investigation.
material is presented in Table 1. It can be AERO-6493
observed from the table that the feed material Cytec’s alkyl hydroxamate-based collector, the
contains about 6.4 % Sn, 59.0% SiO2, 13.4 % Al2O3, AERO® 6493 promoter, is used in the flotation
5.2 % Fe2O3. of a cassiterite ores. It is more selective, easier
Table 1: Chemical analysis of the feed material to use, and provide better yields than
Chemicalconstituents, % commonly used fatty acids, with which they
Sn SiO2 Al2O3 Fe2O3 CaO MgO K2O Na2O TiO2 MnO P2O5 LOI share a similar structure.
6.39 59.06 13.41 5.17 2.72 2.22 2.36 2.0 0.43 0.10 0.20 1.80

Quantitative XRD analysis of the feed material

is presented in Table 2. The tin mineral present
in the ore is cassiterite assaying about 7.2 %,
which is confirmed from the chemical analysis
presented in Table 1. The gangue minerals

These promoters are used in conventional or

column flotation. They are liquid above 15ºC,
though they may start solidifying below 20ºC.
At room temperature, they can be added neat

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to the conditioners. They perform well in a pH Many new reagents have been introduced for
range of 7.0 to 9.0. The optimum pH range for tin flotation over the past four dec ades
oxide mineral flotation is 8.5 to 10.0. These (Bulatovic, 2010). The toxic reagents like arsonic
reagents have frothing characteristics, which acid, phosphonic acid etc are replaced by oleic
c an be regulated through c ontrolled acid, sodium oleate, alkyl phosphoric acid and
manufacturing processes. AERO 6494 promoter hydroxamates. In the present investigations an
produces more froth than AERO 6493 promoter, attempt has been made to study the flotation
and may be preferred where this quality is performance with oleic acid and AERO 6493
desirable. (hydroxamate supplied by Cytec, US).
Oleic Acid
Table 3: Influence of oleic acid and AERO 6493
Oleic acid is a member of carboxylate group of
on flotation of cassiterite
collectors generally used in oxide mineral
Flotation constant parameters
flotation. Oleic acid is an unsaturated fatty acid
d80 particle size : 180 microns
bearing a chemical formula
Feed % solids :5
CH3(CH2)7CH = CH(CH2)7COOH
Dispersant dosage : 150 g/t Sodium silicate,
[molecular weight 282.47]
conditioning time – 5 min
Sodium Silicate
pH : 8.5-9.0
Sodium silicate is widely used in mineral
Collector dosage : 750 g/t, conditioning time
flotation as a depressant of silicate minerals and
– 15 min
dispersant of slimes coating on the valuable
Flotation time : 3 min
mineral particles. It has general formula
Na2SiO3. Recovery of
Collector type Products Wt., % Sn, %
Sn, %
3. Results and Discussion
F 23.5 19.30

Flotation is a physico-chemical process for the AERO - 6493 NF 76.5 0.62 90.5

separation of hydrophobic particles from 100.0 5.02

hydrophilics. The hydrophobic partic les F 24.9 13.50

collected at the froth phase whereas the Oleic Acid NF 75.1 2.25 66.6

hydrophilic remained in the pulp. In many 100.0 5.05

operations hydrophobic particles constitute the
valuable minerals that are embodied in the
froth phase/zone of the flotation cell, hence
resulted forth product is of prime metallurgical
concern.
Batch flotation experiments were performed on
a self-aerated laboratory Denver flotation
mac hine by varying different operating
variables. Following sec tions will give
information about the effect of process variables
on cassiterite flotation.
Influence of collector type (Oleic Acid and
AERO 6493)
The influence of AERO-6493 and oleic acid on
rougher flotation of cassiterite is presented in
Table 3. Both the experiments were carried out
in identical operating conditions like particle
size, feed pulp density, pH, reagent quantity etc.
It can be observed from the table that AERO-
6493 could enrich Sn values to 19.3 with
recovery of 90.5 %. The oleic acid at similar
conditions could produce poor grade and
recovery (Sreenivas, 2002). In view of this, it
was decided to carry out all the flotation
experiments with AERO-6493.
Influence of Dispersant Dosage
Sodium silicate was used in the investigations
to disperse the fine particles from the valuable
mineral particles and depress the silicate

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 MPT-2013

gangue minerals. Sodium silicate quantity 0 to 100

90
1500 g/t varied in the tests. The influence of
80
sodium silicate on the flotation performance is

Recpvery of Sn, %
70
depicted in Fig. 1. The results presented in the 60
figure shows that increased sodium silicate 50
40
doses increases quality of the product on the
30
other hand reduces the recovery of tin values. 20
Increase in sodium silicate from 0 to 1500 g/t 10
increases dispersion of fine silicates attached 0
3 4 5 6 7 8 9 10 11 12
with the cassiterite particles as a result grade pH
is improving from 28.8 to 34.3 %. Sodium silicate Fig. 2: Influence of pH on cassiterite flotation
is also responsible for depression of silicate (d80 particle size 180 microns; Feed % solids 5;
particles; few un-liberated (cassiterite-silicates) Sodium silicate 500g/t, Collector dosage 2000
particles are depressed as a result recovery of g/t AERO-6493)
tin values is decreasing from 78 to 72 %.
Influence of collector dosage
Influence of collector dosage on the flotation of
79 35
Recovery of Sn, %
78
34
cassiterite can be seen from Fig. 3. Generally,
Sn, %
77
1500-2000 g/t of hydroxamates (AERO-6493)
Recpvery of Sn, %

76 33
75 are used in flotation of oxide minerals. An
Sn, %

32
74
73 31 attempt has been made to estimate optimum
72 30 quantity of AERO-6493 required for the flotation
71
70
29 of cassiterite ore. It can be observed from the
69 28
0 500 1000 1500 2000
figure that increased AERO-6493 dosage from
Sodium silicate dosage, g/t
1400 to 2200 g/t decreases product grade from
39.10 to 13.3 % and subsequently recovery
Fig. 1: Influence of sodium silicate on values are increasing from 73.4 to 88.7 %. Similar
cassiterite flotation (d 80 particle size 180 results are evident from the literature (Trahar,
microns; Feed % solids 5; pH 8 . 5 - 9 . 0 ; 1981).
Collector dosage 2000 g/t AERO-6493) 100 45
90 40
Influence of pH 80 35
Recovery of Sn, %
Pulp pH play very important role in flotation.
Recpvery of Sn, %

70
30
60 Sn, %
The selec tivity of partic ular mineral in
Sn, %

25
50
suspension is dependent on a delicate balance 40
20
15
between reagent concentrations and pH. Most 30
20 10
hydroxamates require alkaline pH for the 10 5
successful adsorption to the mineral phases. 0 0
1200 1400 1600 1800 2000 2200 2400
They are effectinve in the pH range 8.5 to 9.5.
Collector dosage, g/t
Increase pH from 4 to 11 increases recovery of
Fig. 3: Influence of collector dosage on
tin values up to pH 9 thereafter again decreases.
cassiterite flotation (d 80 particle size 180
microns; Feed % solids 5; Sodium silicate 500g/
t, pH 8.6)

186

4. Conclusions
Following conclusions can be drawn from the
above investigations.
 Cassiterite sample collected from the Uljin
deposit, South Korea was a hard rock
deposit, wherein tin values are mainly
associated with silicate gangue.
 The feed material assays 6.39 % Sn, 59.06 %
SiO2, 13.4 % Al2O3, 5.2 % Fe2O3 contents.
 Flotation studies carried out with oleic acid
and hydroxamate (AERO 6493) shows that
selec tivity of hydroxamate is muc h
superior than oleic acid.
 Influence of sodium silicate on the recovery
and grade of tin shows that increased
sodium silicate dosage increases the quality
of the product. On an average 500-1000 g/t
sodium silicate is sufficient to generate
required product.
*******
187
MPT-2013
 Maximum recovery of tin is observed at pH
9.
 Collector dosage increases recovery of tin.
About 1500-2000 g/t of AERO-6493 is
needed to float cassiterite values.
References
L. M. Falcon, 1982. The gravity recovery of
cassiterite, Journal of the South African
Institute of Mining and Metallurgy, April,
112-117.
Srdjan M. Sulatovic, 2010. Handbook of
Flotation Reagents, Vol.2, Elsevier.
T. Sreenivas, N.P.H. Padmanabhan, 2002,
Surfac e c hemistry and ûotation of
cassiterite with alkyl Hydroxamates,
Colloids and Surfaces A: Physicochemical
and Engineering Aspects 205, 47–59.
W.J. Trahar, 1981. A rational interpretation of
the role of partic le size in flotation,
Int.J.Miner.Process.8:289-327.
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DEWATERING & TAILING DISPOSAL

189
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190
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Studies on Settling Characteristics of Coal Preparation Plant

Tailings by Flocculation
Shravan Kumar*, N. R. Mandre and S. Bhattacharya
Department of Fuel and Mineral Engineering, Indian School of Mines, Dhanbad, India

Abstract
Human activities like mining, construction and agriculture contribute markedly to the
contamination of water which is globally jeopardizing the ecosystem. In mining industry, the
tailings generated from the coal preparation plants contain fine solid particles which present
many environmental and economic challenges to the society and industry. This also results in
toxicity problems due to the stable presence of soluble materials which have significant adverse
effect on aquatic life, agriculture, plant and animal. The present study intend to show the settling
characteristics of tailing generated from coal preparation plants using different flocculants, dosing
rate, pH of slurry etc. This will improve the basis for the selection of dewatering equipments such
as thickener and filter for tailing dewatering purpose.

Keywords: Mining; tailing; dewatering; flocculation; settling.

1. Introduction high percentage of water causing continuous

A typical coal preparation plant (CPP) produces
about 20% of the mined coal as minus 0.5mm.
Generally, this fine fraction is discarded due to
its high cost of processing. However with the
development of advanced technology, the
cleaning of fine size coal to low ash is feasible.
But the main issue for not operating the fine
coal treatment circuit in India, though installed
in most of the plants, is the presence of high
level of moisture in the products which creates
dewatering problems and c onsequently
increases the processing cost. Therefore, in most
of the coal preparation plants the tailings are
subjected to settling in tailing ponds usually at
* Correspending Author: Shravan Kumar, Assistant Professor,
Department of Fuel and Mineral Engineering,
Indian School of Mines, Dhanbad - 826004, Jharkhand, India,
Contact no.: +91-9771421510
Email: shravankumar.ism@gmail.com
loss of water. That results in higher rate of make-
up water input to the plant. Hence, solid-water
separation including those for tailings has
become an important and complementary
process for the plants.
Most of the dewatering circuits continue the
usage of some chemical reagents to enhance the
settling behavior of the solid particle; but this
also is not giving remarkable change to the
efficiency of the dewatering circ uit. The
dewatering processes generally cause problems
due to the presence of coal particles of different
sizes, shapes, surface area and specific gravities
and their unique behavior in the aqueous
environment. The objective of the present work
is to describe some basic characterization
studies of plant tailing of Jharia coal field,
flocculent selection and other relevant

191

parameters and to find the options for
enhancing the water recovery from the plant
tailings.
2. Area description
2.1 Practices abroad
South Africa has large coal reserves, and is one
of the world’s leading producers and exporters
of c oal. The c ountry c urrently produc es
approximately 290 Mt of ROM coal per annum,
out of which about 14% is believed to be finer
than 500 micron (fine coal) and 2–3% finer than
100 micron (ultra-fine coal) (Le Roux et al, 2005).
The fines c ontent in the ROM had been
increasing in recent years. Coal producers have
a few options as to what to do with the fines.
Initially, fines and ultra-fines were dumped
with the discard streams or tailings ponds, but
sinc e the value of these fines had been
recognized, it was either added to the product
streams as it is, or alternatively, upgraded and
sold. The main reason for not fully exploiting
this energy source is the high levels of moisture
associated with the fines fraction of coal.
Efficient removal of this moisture will yield
definite benefits in finances and handling of the
fine coal, while it will also have a positive
impact on the environment. A 2001 survey of
South African coal beneficiation plants showed
that of the then 24 operations, some 18 plants
employed processes for fine coal beneficiation.
At seven of these plants, the ultra-fine slurries
were dewatered using centrifuges or filters.
With Tao et al. (2000) showing that a 1%
decrease in the final moisture of 3 Mt of clean
coal can lead to a saving of US$ 300,000. These
amounts of moisture left in the fines are adding
up to become a big financial liability.
In Australia, c urrent prac tic e at c oal
preparation plants is to thicken fine coal tailings
with high-rate thic keners utilizing high
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MPT-2013
molecular weight polymeric flocculants (Götz,
Bickert., 2004). The thickener underflow is
either dewatered further or disposed of.
Disposal is either in fine tailings ponds or
together with coarse reject by co-disposal.
Commonly belt press filters are used if
thickener underflow has to be dewatered
further. Decanter centrifuges are no longer
common, while membrane filter presses have
just been introduced at Dartbrook due to the
high clay content and the need to achieve
consistent dry cakes for co-disposal.
For the United States of America, it is forecasted
that coal will constitute a principal source of
energy for the next several decades. A typical
coal preparation plant produces about 20
percent of the mined coal as minus 0.5 mm (28
mesh). Generally, this fine fraction is discarded
due to its high cost of processing. One of the
biggest hurdles in utilization of fine coal
cleaning technology by the coal industry is the
economic dewatering of the fine clean coal
product. Until an economical and practical
solution to dewatering of fine clean coal is
achieved, the efforts devoted to developing fine
clean coal technology will be wasted (Parekh,
B. K., 2009).
2.2 Characterization studies of plant tailings
Dewatering process is known to depend largely
on physico-chemical properties of the coal
particle surface, and is substantially related to
the rank, mineral matter, size distribution and
oxidation of the coal (Rong, and Hitchins, 1995).
The rate of settling of any given particle
depends on its size, its density relative to that
of the suspending medium, the viscosity of the
medium, and the interactive forces between the
medium and other suspended particles. The
degree of diffic ulties assoc iated with
mechanical dewatering increases as the surface
area of the particles increases. Solid

concentrations of slurry also pay a role on
settling behavior. As these increase, the settling
rate progressively slows and above a critical
solids concentration known as the gel point, the
slurry exhibits a network structure and forms
a bed at the base of the vessel. The design
considerations of dewatering equipments such
as thickeners are based on the settling rates of
the slowest settling particles and conditions for
minimum disturbance of the medium (water)
through which the solid particles are allowed
to settle ( Gupta and Yan 2006).
In the coal preparation plants, the desliming at
500 micron of the crushed coal produces fine
coal slurry which is sent to the fine coal
treatment circuit. The size analysis of the
tailings generated from the fine coal treatment
circuit indicate that the amount of particles
which are below 44 micron is in the range of 18
percent. These ultrafine particles are mostly
responsible for the poor performance of the
solid liquid separation circuit, because it has
been found in the settling jar test that a major
portion of the solid settles without use of any
flocculants. The size analysis of the plant tailing
particles in slurry was also carried out for those
particles which are not settling after 5 minutes,
10 minutes and 15 minutes respectively by
using Malvern mastersizer. The result shows
that the particles which remain in suspension
even after considerable amount of time are
about -10 micron in size.
2.3 Flocculation and zeta potential
The major interac tive forc es between
suspended solids are of two kinds - attractive
and repulsive. The attractive forces arise from
short-range Vander Waals’ forces, which is
c ounter balanced by the repulsive forc e
between the particles due to the presence of
electrical charge on them. If a repulsive force
dominates, particle aggregation cannot occur,
whereas, if attrac tive forc es take over,
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MPT-2013
aggregation and settling of the much larger
aggregates will take place. Hence the aim is to
reduce the repulsive force between the particles
so that the attractive force will dominate. This
will accelerate to make large aggregate of fine
solids, so as to be settled at faster rate. Such
process of aggregation of fine particles to make
large flocs using chemicals is called flocculation.
Zeta potential is has significant role in the
stability of very fine particles. The zeta potential
indicates the degree of repulsion between
adjacent, similarly charged particles in a
suspension. For molecules and particles that are
small enough, a high zeta potential will confer
stability, i.e., the partic les will resist
aggregation. The stability behavior of a
colloidal solution, as reported in literature, can
be understood from the following value of zeta
potential mentioned in Table 1.
Table 1: Stability change with respect to zeta
potential of particles.
Zeta potential [mV] Stability behavior of the colloid
from 0 to ±5, Rapid coagulation or flocculation
from ±10 to ±30 Incipient instability
from ±30 to ±40 Moderate stability
from ±40 to ±60 Good stability
more than ±61 Excellent stability
Most of the aqueous solutions are either neutral
or basic and hence the particles are negatively
charged. To reduce the repulsive force between
two particles due to presence of negative
charges on them it is essentially required to add
some elec trolytes whic h have opposite
(positive) charge to cause charge neutralization.
Such electrolytes are called coagulants. If the
aqueous solution is acidic in nature i.e. particles
are positively charged then electrolytes with
negative charges are to be added.
Coagulants could be either from inorganic or
organic sources. The commonly used inorganic
 MPT-2013

coagulants used for wastewater treatments are The preliminary settling studies on this plant
alum, ferrous sulphate, ferric chloride. On the tailing slurry were c arried out using
other hand the organic coagulants may be polyacrylamide at very dilute condition. A good
either synthetic of natural flocculants. The settling rate was obtained at floc c ulant
major drawback of inorganic coagulants is the consumption of 16 gpt. The operating condition
huge requirement of coagulant for achieving a
for the settling test are mentioned in Table 2.
effective settling rate causing a huge sludge
Table 2: Operating condition for the settling test.
volume which creates disposal problem. On
Solid concentration : 5% (w/w)
the other hand organic flocculants are highly :
Flocculant added Polyacrylamide
efficient flocculant though both the synthetic PH of slurry : 8.2 (Natural pH of slurry)
and natural ones have some advantages and Flocculant concentration : 0.1% (w/w)
some limitations. Synthetic polymers are Dosing rate, gpt : 16

highly efficient polymers, however they are

The curve of height of mudline against time has
not biodegradable and their degradable
been shown in figure 2. This indicates that the
product is considered as a hazard because of
release of toxic monomer which may cause major portion of the particles was settled in
about 60 seconds.
serious threat to environment. Hence, natural
polymer based flocculant are more appreciable
bec ause, they are shear resistant,
biodegradable and eco-friendly, but at the same
time less efficient as flocculant.
The zeta potential of the suspended solid was
also calculated by using Zetameter-4; the has
been shown in Figure 1.
Figure 2: Settling behavior of solid particles.
Although, further investigation is under
progress to study the effect of other parameters
on the settling behavior, so that, the higher
settling rate may be obtained.
Fugure 1: Graph of zeta potential Vs pH of slurry.
2.5 Plant circuit design
The results indicate that the high zeta potential
is observed at slurry pH of around 9.2. The The concentrate generated from fine coal
treatment circuit is generally dewatered using
natural pH of the plant tailings was observed
thickener followed by filter and the water
in the range of 8-8.2.
removed from the dewatering c irc uit is
2.4 Settling characteristics of coal particles recycled back to the plant. But for fine coal
tailings slurry we generally use only thickener
To develop effective dewatering and disposal
and avoid other equipments such as filter due
methods, it requires an improved
to high capital and operating cost. This results
understanding of the role of flocculant on high significant amount of water lost with the
settling that promotes better water recovery plant tailings. A typical schematic diagram of a
and higher sediment density during settling coal preparation plant can be seen from the
and consolidation of flocculated solids. Figure 3.

194

Raw Coal
Fresh Water
Coal Preparation Plant
Recycled Water
Dewatering of Clean
Coal Fines
Tailing Thickener
Figure 3: A schematic illustration of a coal
preparation plant
The loss of water results in higher rate of
makeup water to the plant. So it becomes
essential to improve the efficiency of tailing
thickener. The tailing received from the fine coal
treatment circuit shows the concentration of
solid is about 8 percent (weight / weight). This
dilute slurry is generally sent to the tailing
thickener which produces the final plant
tailings at the solid concentration of about 28
percent (weight / weight). In terms of total solid,
about 6-8 percent of run of mine coal is disposed
to tailing dam at very low pulp density as
mentioned above. This clearly shows that we
have to enhance the performance of solid liquid
separation equipment which is generally a
thickener.
The thickening process, although operated
successfully in a large range of sites around the
world, is poorly understood and predictive
design of thickening equipment is still empirical
(Gupta and Yan 2006). The performance can be
enhanced through improved design of the
circuit along with the correct selection of the
flocculants.
MPT-2013
3. Conclusion
Coarse Clean Coal
The size analysis of the particles indicate that
Coarse Middling/Tailing
the particles below of 44 micron size contribute
Fine Clean Coal
significantly to the separation of solid and
liquid. The zeta potential has its peak value at
To Tailing Pond
around 9.2 pH which is close to the natural pH
of the slurry. The settling behavior can be
improved appreciably at neutral pH by the
addition of some acidic chemicals such as HCL
to the slurry, because at neutral pH the value of
zeta potential is very low in comparison to its
natural pH value.
References
Tao, D., Groppo, J.G., Parekh, B.K., 2000.
Enhanced ultrafine coal dewatering using
flocculation filtration processes. Minerals
Engineering, 13(2), 163-171.
Götz, Bickert., 2004. http://www.acarp.com.au/
abstracts.aspx?repId=C14012
Parekh, B. K., 2009. Dewatering of fine coal and
refuse slurries problems and possibilities.
Procedia Earth and Planetary Science 1, 621-
626.
Rong, R.X., Hitchins, J., 1995. Preliminary Study
of Correlations between Fine Coal
Characteristics and Properties and their
Dewatering behavior. Minerals
Engineering, 8(3), 293-309.
Gupta, A., Yan, D.S., 2006. Introduction to
Mineral Processing Design and Operation,
First Edition
Gladman, B.J., Usher, S.P., Scales, P.J., 2006.
Understanding of Thickening Process.
Keynote Address, Australian Centre for
Geomechanics, Perth, ISBN 0-9756756-5-6.
*******
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Effective Control of High-Rate Thickener Process Parameters with

Respect to Run-of-Mines in Wet Processing Plant at Noamundi
Iron Mines
S. Mishra1, V. Agarwal2, A. Kumar3 and D. Mukherjee4
1
Wet Processing Plant, Noamundi, 833217, Jharkhand, India.
2
Katamati Iron Mines, Noamundi, 833217, Jharkhand, India.
3
Natural Resources Division, Noamundi, 833217, Jharkhand, India.
4
Noamundi Iron Mines, Noamundi, 833217, Jharkhand, India.

Abstract
Beneficiation of the Run-of-mines is utmost essential because of stringent quality requirements of
the customer. In the process of beneficiation, there is a considerable amount of slime generated,
and needs to be disposed. At Noamundi Iron Mines, the Wet Processing Plant uses a High Rate
Thickener (HRT) as an integral part of its slurry disposal system for maximising the flocculation
efficiency of flocculants used in the slurry disposal system. As a consequence, change in the solids
feed rate or the settling characteristics of the solids will change the sludge level much more
rapidly, therefore, high rate thickeners require someform of automatic control. The control pa-
rameters used to maintain stable operation in high rate thickeners are underflow solids density,
underflow withdrawal rate, flocculants dosage, solids inventory in the tank, solids feed rate, and
mechanical torque limit restriction of rotating rake arm mechanism. In order to improve the
reliability of the HRT, it was important to understand the behaviour of HRT process parameters
with respect to material feed (ROM- Run-of-mines). Strategic parameters were analysed in order
to find out which input parameters affected the nature of slime generated and thereby affect the
process parameters of HRT. Based on the analysis, it is observed that the process parameters of
HRT bear a direct co-relation to the feed rate of the processing plant and the flocculent dosage rate
in the HRT. Thickener overflow at Normandy Processing Plant is recirculated and used as process
water. A very integral role of HRT is in providing greater clarity of overflow water so that
beneficiation process quality is not hampered. On analysis, it is observed that the clarity of water
bears a direct correlation with the dosing rate of flocculent at HRT.
Keywords: High-Rate thickener; run-of-mines; slurry handling system; flocculation.

1. Introduction: southwest from JSR on the eastern limb of the

Noamundi Iron Mines (NIM) is one of the cap-
tive sources of iron ore and caters to almost
60% requirement of Tata Steel Limited,
Jamshedpur Works. It is located 120km due
Corresponding Author: Sailesh Mishra, Manager Opera-
tions, Wet Processing Plant Noamundi, 83 321 7,
Jharkhand, India, + 91-926 363 567 7,
Email: sailesh.mishra@tatasteel.com
major Iron Ore Group Synclinorium within
Singhbhum-Orissa Cratonic block.
NIM is a fully mechanized truck and shovel
operation with drilling and blasting carried out
for all waste and ore materials. Iron ores as they
occur in the mine are classified into four major
geotypes, namely hard ore, friable-flaky ore,
soft-lateritic ore and blue dust purely based on
their physical properties and appearance. A

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cut-off grade on the alumina content in ROM 3. Slurry Handling System at Noamundi Wet
combined with physical characteristics such Circuit Plant
as lump yield and strength defines the Dry (high 3.1. Conventional Slurry Handling System
grade) and Wet (low grade) crusher feed. The Clear water
Dry processing plant is quite simple, compris- Slurry
ing crushing and dry screening with no tail- Slurry formed during the beneficiation process
ings. Low grade material is concentrated
in the wet processing plant and jig plant is col-
through primary and secondary crushing fol-
lected in the Annex Pit (Fig. 1). Two negative
lowed by screening and oversize crushing and
re-screening, washing and sizing, scrubbing, suction pumps are operated in parallel to pump
classifying, jigging and passing through this slurry into the distribution tank. The role
hydrocyclone, with overall recovery of ~80%. of the distribution tank is to channel the flow of
In the process of beneficiation slurry generated the slurry into two separate identical thicken-
is disposed into tailing pond by a Slurry Han- ers. Each thickener receives the slurry centrally
dling System. and the slurry is allowed to settle in the thick-
ener. The rake arm of the thickener moves at a
2. Background
very low rpm raking the slime from the sides
The disposition of ore types, like many other
to the centre of the thickener. At the central cone
iron ore deposits across the globe records hard
of each thickener there are three bypass lines
formation at the top with occurrence of ore
which carry the compacted slime into the un-
type e.g. friable and blue dust towards bottom
derflow pump house pit. Two underflow
of the deposit. With time, as the mine pro-
pumps with a capacity of 250 m 3each,pump
gressed deeper into the ore body availability of
slime from the pit into the tailing pond. The
hard ore became limited resulting in lesser
line diagram of the conventional slurry han-
hard ore feed to the Wet Circuit plant with in-
dling system is shown in Fig 1.
crease in friable-soft/lateritic ore proportions
in recent years posing challenges to the plant
operators as the change in feed mix not only
resulted imbalance in lump:fines recovery pat-
tern but also led to increase in slime loss sub-
stantially. The situation became worse with
mine having patches of bluedust/powdery ore
within friable ore, quality of which did not al-
low to process them in dry circuit plant. Ma-
jority of the cases ore types such blue dust and
powdery ore having high content of super-fines
(<100 mesh) in-situ, tend to report to slime
making slurry handing and recovery of Fe-val-
ues further through hydrocylone, more diffi-
cult. Subsequently it was required to relook into
the conventional slurry handling system of the
plant and to make it suitable with change it
feed grade and ore mix.

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Table 1: Components of conventional slurry · Greater availability and reliability of

handling system slurry handling system
Table 1: Components of conventional slurry handling system
Table 2: Technical Specifications of HRT at Processing Plant, Noamundi
Number of thickener 2 Diameter of tank 35m
Slurry feed rate 2500 m3/hr
Diameter of thickener 50 mm Solid TPH 250 TPH
Conventional High-Rate Thickener Rake Feed Solid %
Height of thickener tank 5.5 m 11%
Thickener specifications Rake Speed 0.9 rpm
Number of bypass lines 3 Rake lifts travel 600 mm

Thickener rake arm speed 0.7 rpm

Number of pumps 2x3
Underflow pump discharge 300 m3 Tailing Pumps Make and Model Metso HP 150
Underflow Pump Flow Rate 315 m3/hr
Underflow pump head 64 m Head 56.2 m
House Tailing Pumps (contd.)
Number of pumps 2x2 Pump rotation speed 1660 rpm
Power 150 kW
Number of pumps 2
Make and Model Kirloskar UP350-66
Flow Rate 2000 m3/hr
Recirculating Pumps Head 40 m
Motor RPM 980
The Conventional Slurry Handling System in Power 315 kW

the Wet Processing Plant had been designed for

Table 3: Process Monitoring Instruments installed in HRT at Wet Plant, Noamundi
greater hard ore percentage in ROM feed (mini-
Bed Level sensor For control of flocculation rate
mum 35%). Due to increase in fines in ROM feed,
Process Monitoring Bed Mass sensor For In-tank inventory and
and increase in clay content in ROM, the con- Instruments Underflow control
Rake Level sensor For rake level indication
ventional system proved to be inadequate. Un- Pressure Transducer
Limit Switches
For rake level control
For rake level tripping (up/down)
derflow bypass lines could not handle the
higher solid percentage in slurry. The mouth of
the bypass lines suffered regular jamming. The The High-Rate Thickener consists of three
only control executed was to cut off the plant zones:
feeding whenever thickener load exceeded 3.5 · Consolidation zone- The slurry material
Amperes. Compaction of solids was not suffi- along with the flocculent gets consolidated
cient in the conventional thickeners; hence, in this zone. The height of the consolidated
wastage of water and clear water recovery was material in this zone is monitored using an
a major concern. It was a purely mechanical ultrasonic sensor and is called BED MASS.
system with only two process parameters be- Bed mass is measured in percentage of the
ing monitored hourly viz. thickener rake arm maximum height of the consolidation zone.
motor load and underflow slime density,
thereby posing a challenge for process control. · Settlement zone- This is the zone where the
The High Rate Thickener (HRT) at Wet Process- actual interaction takes place between the
ing Plant Noamundi is designed to cater to this slurry and the flocculants dozed.
requirement. It provides higher compaction, · Clarified zone- This zone forms the topmost
greater clarity of overflowing water, lower set- zone of the HRT where clear water is gener-
tling time and greater process control. ated due to the settling of suspended solids
3.2. High Rate Thickener and its integra- into the consolidation zone. The height of
tion in existing beneficiation circuits this zone is measured as BED LEVEL. Bed
Requirements for a new slurry handling sys- level is measured in percentage of the maxi-
tem: mum height of the clarified zone and is con-
· More slime tonnage to be disposed stantly monitored by another sensor.
every hour.
· Higher clarity of process water

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The Annex Pumps referred to in Section 3.1 The correlation observed between the Bed Mass
pump the slurry collected from the Process- and the Feed Rate (measured in TPH) is given in
ing plant into the HRT via a sky-launder Fig 3(a).
chute (shown in Fig 2). The slime entering
HRT gets mixed with the flocculants dozed
in the Settlement Zone of the HRT. Once the
reaction between the flocculants and the
slime particles is complete, the heavier slime
particles settle into the consolidation zone.
Twosets of three underflow pumps each (one
set in standby; specifications are mentioned
in Table 2) get their suction from the central
cone of the HRT and discharge the slime
formed into the slime dam (also referred to as Fig 3(a) Relation between the Bed Mass and
Tailing Pond). the Feed Rate

On changing the dosing rate, the bed mass is

also affected. This relative change is depicted
in Fig 3(b).

Fig.2: Process Flow Diagram of HRT at Wet

Processing Plant, Noamundi
4. Control of HRT Process Parameters
During initial integration of HRT in the
beneficiation circuit, real-time control was dif-
ficult as the process control parameters were
not established in relation to the ROM feed com-
position. Therefore efforts were taken to estab-
lish cause effect relationships, and it was found
that the bed-mass, essentially impacted by
higher super-fines content in ROM exhibits
good correlation with the feed rate in the pro-
cessing plant and the flocculent dosing rate.
Fig 3(b) Relation between the Bed Mass and
the Dosing Rate
The results can be summarised as:
· Increasing TPH increases bed mass,
· Increasing the Dosing Rate increases bed
mass, and
· Increasing the Dosing Rate increases the bed
level.
Increasing bed mass implies a rate of slime feed
into the HRT higher than the underflow dis-
charge rate. Higher bed mass implies greater

199

torque on the rake arm. This increases the
chances of mechanical damage to the rake arm.
Therefore, containing the increase in bed mass
is important.
There are three ways in which the bed mass
can be reduced:
· Increase the underflow discharge so that
slime discharge is greater than the slime en-
tering into the thickener tank. This is facili-
tated by increasing the underflow pump
speed.
· Decrease the consolidation or settling rate of
the material-flocculent mixture. This is facili-
tated by reducing the flocculent dosing rate.
· Decreasing the feed rate. Increasing feed rate
increases the rate at which slime enters into
HRT tank. Containing the bed mass can be
facilitated by reducing the feed rate.
The bed level is the measurement of the clear
water that is available at the HRT for recircu-
lation and further use as process water. It is
observed in Fig 3(c) that Bed Level bears a
strong correlation with the dosing rate.
Fig 3(c) Relation between the Bed Level and
the Dosing Rate
200
MPT-2013
5. Conclusion
With diminishing hard ore proportions in ROM,
the quantity and quality of slurry generated in
the processing plant changed. This change
could not be accommodated by the conven-
tional slurry handling system. Process control
measures proved ineffective because of insuffi-
cient process parameters. A major advantage
with the HRT was the numerous process pa-
rameters that could be monitored on a real-time
basis. Two major parameters were identified
as Bed Level and Bed Mass. Few important fac-
tors affecting the bed mass and bed level were
recognised as the ROM feed rate into the pro-
cessing plant and the dosing rate of flocculants
into the HRT. On analysis, it was observed that
the Bed Mass increases with the increase in the
feed rate as well as the flocculent dosing rate.
To contain the increase in bed mass, the HRT
operators adjust the underflow pump rotation
speed thereby adjusting the slime discharged
from the HRT, adjust the feed rate of the pro-
cessing plant or adjust the dosing rate of
flocculants.Bed Level being the measure of the
clear water in the HRT tank was analysed with
dosing rate. More flocculants dosed per hour
results in increased settling rate and hence,
more bed level. The operators adjust the plant
feed rate and the dosing rate by keeping a bal-
ance between the bed mass and the bed level.
Acknowledgement
The authors are thankful to the management of
Tata Steel Limited who have provided us their
complete co-operation and guidance. We are ex-
tremely thankful to the employees of Process-
ing Plant, Noamundi who have contributed
significantly to the success of this research. We
are thankful to Mineral Processing Technology
2013 for giving us an opportunity to publish
our field work.
 MPT-2013

References Pradip, 1994, Met. Mater Processes, 6, p179.

Roy,S. and Das, A., 2009, Minerals and Metal-

Delkor Global, Tata/Noamundi High Rate
lurgical Processing, 26, p141.
Thickener Operation/Commissioning
Course
Suresh, N., Kumar, S. and Banerjee, P.K., 2007,
Characterisation and Beneficiation of Low
Federation of Indian Mineral Industry (FIMI)
Grade Iron Ore
Report, 2008, creating a Vibrant Iron Ore
Industry in India a survey. http://mining-
Vishwanathan, S. and Pranjpe, V.G., 1968,
t e c h n ol ogy. b log sp ot . c o m /2 009 /0 5/
Trans. Ind. Inst. Met.,p 77.
beneficiation of low grade iron ore.html.
Wills, Mineral Proc essing Tec hnology,
Indian Mineral Year Book, 2008, Indian Bureau
Pergamon Press
of Mines, Nagpur p47.

*******

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Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Parametric Optimisation for Filtration of Iron Oxide Concentrate

S. S. H. Naqvi*, P. S. Maji, Aslam Khan and Sushil Dubey

Orissa Manganese & Minerals Limited, Kandra, (Adhunik Group of Industries)

Abstract
The demand for iron ore has increased drastically in the last few years and is forecast to remain on
a stable high production level for years to come. It is expected that the existing and known high
grade ore resources will decline, and the iron ore industry will be forced to implement more and
more advanced beneficiation plants in which filtration is one of the important stages. The filtration
of fine particles derived from iron ore processing is a topic of increasing importance to mineral
industries. With little previous published work in this area, it is difficult to predict how these
materials will behave during filtration, in particular during vacuum filtration. Conventional
vacuum filtration methods have been the most prevalent in fine iron ore dewatering. This paper
describes effects of different parameters (pulp density of the slurry, particle size distribution of the
feed, rotation of ceramic disc and Basin number) on filtration process. Performance of advanced
filtration technology (Ceramic Disc Filtration) for iron ore applications have been studied, and the
findings are based on day to day plant operation data and laboratory reports.

1. Introduction expansion plans are implemented as per

India has emerged as the fourth largest steel
producing nation in the world, as per the recent
figures released by World Steel Association in
April 2011. In 2010, India was the 5th largest
producer, after China, Japan, USA and Russia
and recorded a growth of 11.3% in steel
production as compared to 2009. Overall
domestic crude steel production grew at a
compounded annual growth rate of 8.4% during
2005-06 to 2009-10. The Indian steel industry
accounted for around 5% of the world’s total
production in 2010.
Total crude steel production in India for 2010-11
was around 69 million tonnes and it is expected
that the crude steel production in capacity in
the country will increase to nearly 100 million
tonne by 2012-13. Further, if the proposed
* Correspending Author:
mail id: sshnaqvi@adhunikgroup.co.in
schedule, India may become the second largest
crude steel producer in the world by 2015-16.
The demand for steel in the country is currently
growing at a rate of over 8% and it is expected
that the demand would grow over by 10% in
the next five years. However, the steel industry
in the country remains well below the world
levels. India’s per capita consumption of steel is
around 50 kg as compared to 150 kg for the global
average. This indicates that there is a lot of
potential for increasing the steel consumption
in India.
Blast furnac e produc tivity has gained
momentum over the years with utilisation of
higher and higher proportions of quality
agglomerates in the burden. It has been observed
that 1% replacement of calibrated lumps by
agglomerated products like sinter or pellet
reduces the coke rate by 1.5 kg/t of hot metal
produced.

202

With high-grade Iron ore rapidly depleting, the
necessity of Iron ore beneficiation is becoming a
reality. Beneficiation of Iron ore is much more
economical than getting rid of gangue at higher
end of value chain like in BF or BOF / Electric
furnace. It is believed that it will cost 5 to 10
times more to remove gangue in BF / BOF or
Electric arc furnace than in beneficiation plant.
In order to beneficiate, the Iron ore is needed to
be crushed to the liberation size to maximize
the benefits from the process. Typically Iron ore
is liberated when the ore is ground to sub micron
size.
Up-gradation of lower grade ores/fines
necessitates beneficiation for making of sinter
and pellet. Any iron ore beneficiation process
primarily is governed by grinding, gravity
separation, and filtration processes.
The purpose of filtration is either clarification
of liquids or solids recovery. In clarification the
liquid is typically the valuable product and the
solids are of minor quantity and are often
discarded with out any further treatment. If
however the solids are to be recovered, they very
often have to be washed, deliquored and dried.
In this article, washing means the cleaning of
the product (filter cake) and is distinguished
from cleaning parts of the filter itself, which will
be called rinsing (like rinsing a filter screen/filter
disc or a filter cloth by jets of water).
The filter cake thus obtained need to have
optimum moisture content for proper green ball
formation and needs to be dewatered.
Generally, the term drying means thermal
drying, but the elimination of liquid from the
filter cake by mechanical forces is called
deliquoring or dewatering. Filtration is effected
by application of capillary, vacuum, pressure,
or centrifugal force.
Vacuum filters have the great advantage that
the cake is freely accessible. This facilitates
automatic cake handling. However, vacuum
filters cannot handle hot liquids, or solvents
with high vapor pressure. Also, the pressure
difference across vacuum filters is very limited,
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MPT-2013
and the residual moisture of the filter cake is
higher than that obtained with pressure filters.
Pressure filters in turn are preferred when the
product must be kept in a closed system for
safety reasons, or if the residual moisture
content is important. The handling of the filter
cake is obviously more difficult in a pressure
filters. Filtration by centrifugal force requires
more expensive technical equipment, but as a
general rule it yields solids with lower residual
moisture
Apart from the operating functions of the
filtration system, the speed of filtration depend
on many factors of the slurry being filtered viz.
amount of ultra fines, slime content like kaolinite
especially alumina content etc.
The present investigation deals with the
investigations carried out on high grade iron
ore samples for filtration by ceramic filter. The
results obtained from the experiments were
compared and presented in this paper.
2. Results and Discussion
Nowadays pellets are frequently used as raw
materials for iron making. The parameters
needed for proper pellet making needs to be
identified and studied for optimum productivity
and desired quality. The important part of
pelletization is green ball formation, and the
formation of green ball is interrelated with
various parameters viz. properties of filter cake,
types of additives, inclination and RPM of
balling disc, water addition for maintaining
proper moisture etc. The properties of filter cake
for perfect ball formation have been discussed.
Major properties of filter cake of iron oxide for
proper green ball formation for subsequent
pellet formation are:
1. Moisture %
2. % of -10µ (slimes)
3. % of -45µ
4. % of +150 (coarser grinding)
5. Blaine Number
 MPT-2013

The table below shows the physical & chemical and higher -10 micron will give satisfactory
parameter of filter cake & its range for getting Blaine number which will still be problematic
the best quality green ball. for settling and filtration and would have bad
balling characteristics. Determination of Particle
Table 1: OMML Filter cake specification
Size Analysis (PSA) along with Blaine number
will actually represent the grinding and the
Chemical& Physical properties
suitability of the filter cake for the filter cake
Parameter Range produced.
Fe( Total ) 62.80 – 63.50 % It is observed that as we increase the Blaine of
SiO2 3.00 – 4.00 % filter cake the moisture in filter cake also
increaseswhichisshowninFigure-2
Al2O3 1.90 - 2.50 %
LOI 2.70 - 3.50 %
+150 µ 5.00 % max.
-10 µ 20 – 25%
-45 µ 60 to 65%
Moisture 9.0 – 10.0%
Blaine Number (cm2/gm) 1800 – 2200

Figure 2: Variation of moisture with respect to

2.1. Blaine number and grind
Blaine Number and Grind both represent the
finesses of the particles in a sample. As the
fineness increases the Blaine number will
increase and the grinding i.e. is amount of -45
mic ron partic les in sample will also
increases.Figure-1 clearly shows that the Blaine
number and grinding of filter cake varies
simultaneously.
Figure 1: Variation of grinding and blaine
number
Blaine number is one of the most important
parameters which determine the settling and
filtration behaviour, moisture content and
balling formation in the balling disc. However,
only Blaine number may not be a true
parameter as the presence of higher +150 micron
blaine no.
Thus from the above figure it can be clearly seen
that the moisture is directly proportional to the
Blaine number of the filter cake. This suggests
that to maintain a low level of moisture in the
filter cake, the residence time in the ball mill
should be reduced. This will decrease the
unnecessary generation of ultra-fines particles
and thus increasing the quality of the filter cake.
Moreover there should always be a closed
circuit grinding adopted in comparison to the
general high reduction ratio open circuit
grinding.
A study was conducted to asses the effect of
Blaine/ grinding(-45 micron particle) on various
green ball factors. Figure 3 shows the effect of
GCS with percentage fines. Initially it was
found to increase with increasing percentage of
-45 micron size as the compaction increased
with higher -45 micron particles. But higher
grinding also decreased the amount of coarser
particles which help in binding the smaller
particles leading to decrease in GCS value of the
green balls. The study was carried out to
determine appropriate grind time so that -45

204
 MPT-2013

micron particle did not exceed 60 percent. Drop
number as shown in Figure 4 depicts similar
trend.
2.2. Coarse grinding
The coarse grinding will lead to ease of filtration
and decrease in moisture content but will
adversely affect the balling behaviour. The plot
below (Figure 6) shows the variation of
moisture with increasing +150 micron size
fraction present in the filter cake:

Figure 3: Variation of GCS with grinding

Figure 6: Variation of moisture with coarse

grinding
From Figure 7 it can be clearly seen that as the
percentage of +150 micron increases it results
into decreasing the moisture content but the
Figure 4: Variation of drop number with porosity of pellets leads to increase in CCS value
grinding of the pellet, the ultimate product as shown in
Figure 8.
The porosity of the pellets as expected found to
decrease with increasing -45 micron size
fraction and is shown at Figure 5. Keeping a -45
micron fraction at around 50 – 55 percent gave
the highest porosity which will result in better
reducibility.

Figure 7: Variation of porosity with oversize

fraction

Figure 5: Variation of porosity with grinding

From the above three plots it can be interpreted
that as the Blaine/grinding increases the GCS,
Drop number of green ball increases and reaches
an optimum point and then decreases while on
increasing the grinding the porosity of pellets
decreases. Thus it can be deduced that the Blaine/
grind value of the filter cake should be such that
-45 micron particle range between 55 – 60%. Figure 8: Variation of porosity and CCS

205
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2.3. Flocculant 2.5. Variation of different factors effecting Filter

Capacity
Flocculants generally do not affect the moisture of
a filter cake directly. But it has been seen that high Pant operation data was studied to analyse the
amount of flocculants results in poor quality of effect of various factors on filter capacity as that
filter cake i.e. when used to make pellets, the green ultimately decides the filter cake productivity
pellets become plastic in nature thus rather than whic h is directly proportional to pellet
breaking they tend to change their shape. production.
Although the addition of flocculants to slurry can
One of the most important difficulties being
lead to significant improvements in sedimentation
faced while using Ceramic Plate filter is that the
characteristics, it also affects dewatering
pores of the Ceramic plates get choked with
behaviour, flocculation generally being
ultra fines present in Iron Ore fines and those
detrimental to final consolidation of the sediment.
generated during grinding. To circumvent the
It is usually beneficial, however, to filtration
problem it is suggested that Ceramic filter boots
processes, and flocculants are widely used as filter
should be provided with an overflow so that
aids. It may also be worth mentioning that while
the ultra fines are over flown and does not get
designing the thickener, care should be taken to
access to the Ceramic plates. Also care needs to
design it with respect to the settling rate of the
be taken to get the chemistry of back wash
iron ore fines being used to keep the flocculant
checked to ensure proper cleaning. That way
addition low to ensure least plasticity in the filter
both choking problem can be reduced and the
cake. However, the specific requirements of a
life of Ceramic plate shall also increase.
flocculants used to promote sedimentation are not
necessarily the same as for one used as a filter aid. 2.5.1 Effect of Slurry density on Filter capacity
The behaviour of the flocculated suspension and
The data was captured for filter capacity with
the performance of solid-liquid separations are
varying slurry densities. The capacity of filter
determined by the size of the flocs and by their
varied from 12000 to 35000 kg/hr during the thirty
structure. Large flocs promote settling and are
experiments conducted. The capacity of ceramic
desirable for clarification and thickening.
filter increases with increase in solid
2.4. Filter cake moisture concentration. This is easily illustrated in the
Figure 10. There is a change of nearly 900kg/hr
From the Figure 9, it can be seen that the as the
when the slurry density was raised from 50% (w/
percentage of moisture in filter cake increases
w) to 60% (w/w). So, to increase the total capacity
the GCS of the green ball formed increase up to
the solid concentration of the feed should be high.
an extent. It may also be noted that the GCS of
the green ball can be increased with the
addition of additives (Bentonite). The trend is
almost the same for both as the data was taken
from the day when the specific consumption of
bentonite addition is almost the same.

Figure 10: Filter capacity with respect to slurry

Figure 9: Variation of GCS with moisture
density
2.5.2. Effect of Slurry density on the moisture
content of the Filter Cake
The moisture percent of the filter cake varied
from 9% to 11% during the thirty experiments.

206

Figure 11 illustrates that as the solid
concentration increases the moisture content of
the filter cake also increases. This shows that
increasing the solid percent the moisture and
filter capacity will move in opposite direction.
Thus needs to optimised in such a way that the
productivity increases but the moisture content
is within a controllable value.
Figure 11: Moisture of filter cake with solid
concentration
3. Conclusions
From the above experimental data & analysis it
can be concluded that the filtration process is
affected by so many factors and getting all the
parameter in one plane is a difficult task but by
controlling major factors we can achieve our
desirable result in industry. Since our aim is the
formation of metallurgical grade pellet which
can be achieved by proper proportioning of raw
material (i.e. filter cake, lime, bentonite & coke).
To understand the effect all the parameters of
filter cake viz. the Blaine number (degree of
fineness), Presence of +150µ, Moisture, and Pulp
Density on green ball formation were studied
and the following conclusions are drawn from
the test results:
A. Increasing the Blaine Number of cake the
moisture content increases. This is due to
generation of ultrafine during grinding. Thus,
to maintain optimum moisture the Blaine no.
should be around 2000.
B. On increasing the fraction of +150µ the
moisture decreases and we get optimized
*******
207
MPT-2013
moisture cake but at the same time the GCS
of green ball decreases which results in poor
CCS. Hence, for the good ball the +150µ
should be less than 3%.
C. High dosage of Flocculants will result in poor
quality of filter cake i.e. when used to make
pellets, the green pellets become plastic in
nature thus rather than breaking they tend
to change their shape.
D. Increase in moisture in filter cake leads to
formation of uneven ball with low GCS
leading to low CCS. So for proper balling the
moisture should be in the range of 8-10 %.
Table 2 indicates the optimized parameters
to be achieved for better balling.
Table 2. Parameters and their Optimum points
Sl. No. Parameters Optimum Point
1 Blaine Number and Grind (-45 Micron %) 2000 cm2/gm & 60-65%
2 Coarse Grinding (+150 Micron %) Should be <5%
3 Flocculant 5gm/ton ()
4 Filter cake moisture 9-10%
5 Filter feed density 60% (w/w)
Acknowledgement
The authors gratefully acknowledge the help,
encouragement, guidance received from Mr.
Manoj Agarwal, MD, Adhunik Group of
Industries for the paper.
References
http://ibm.nic.in/ch4.pdf
htt p://www.im-m ining. c om/wp -c ontent/
themes/immining/pdfs/Larox DewateringTech-
20100615.pdf
h t t p : / / w w w. i n d i a s t e e l e x p o . i n /
IndustryOverview.php
Laboratory procedures to measure green pellets
and fired pellets properties by “pellet plant lab
procedure manual”.
OMML Laboratories Report.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Enhancement of Fine Coal Dewatering in Screen Bowl Centrifuge

Arijit Das, Soni Jaiswal and PK Banerjee
Research & Development Division, Tata Steel, Jamshedpur-831001, India

Abstract
At Tata Steel Washery, fine clean coal from froth flotation cell is usually dewatered in screen bowl
centrifuge. The tailings of froth flotation process is taken to thickener for concentrating the slurry
suspension as well as to recover clarified water for re-use in the plant. One of the limitations of the
centrifuge is the loss of ultrafine coal as centrifuge centrate. This complete dewatering process
needs to be improved by developing suitable technique for preventing the escape of carbon values
into the tailings pond with the application of reagents.
Due to presence of high amount of ultra-fine coal (0.038 mm) in feed to flotation circuit, dewatering
process is not working well at Tata Steel washery. Different reagents are tried in laboratory to
reduce moisture content of fine clean coal. Among these reagents surfactants are found superior in
reducing moisture content of fine clean coal compared to application coagulant and flocculant. It is
observed that there is a potential in reducing moisture content of fine clean coal by about 23% from
current moisture level observed in the plant at moderate dosage of 0.25 kg/t. Coagulant application
is found to be more effective in vacuum filtration though at higher dosage of 0.5 kg/t with reduction
in moisture content of about 17% from base level. Moisture content of fine clean coal was reduced
by 15.3% from base level by application of another surfactant at low dosage of 0.1 kg/t.

Keywords: Coal dewatering; reagents; centrifuge; filtration; thickener.

1. Introduction Due to high ash c ontent and uniform

distribution of mineral matters in coal
All washing plants use vast quantity of water
substance, coal washing in India needs finer
for beneficiation of coal. This water allows the
crushing even to a level below 13 mm, in
movement of particles throughout the
particular at coal washeries of Tata Steel. This
processing plant and the upgrading of the
also leads to a generation of excess fines. West
material. When the process is complete the
Bokaro Division of Tata Steel treats around 6.6
finished product must be dewatered. This is due
milliontonnes of medium coking coal to
to storage concerns, in which the water takes
produce about 2.5 million tonnes of clean coal
up a majority of the spac e, and high
having 14% ash. Fines (-0.5 mm) which is
transportation costs, in which no compensation
around 20% of the feed to the Washery is treated
is obtained from the buyer for the shipment of
in the flotation circuit and the rest in the coarse
the liquid. Dewatering is accomplished by many
circuit using Dense Media cyclones. The water
devices, with the two most common pieces of
added to coal before desliming allows the
equipment being the screen-bowl centrifuge and
movement of particles throughout the
filters operating under vacuum or pressure.
processing plant and the upgrading of the
material. When the process is complete the
* Correspending Author: finished product must be dewatered.

208

Froth coming out of froth flotation cell is treated
in screen bowl centrifuge to reduce its moisture
content. Tailings from froth flotation cell is
treated in thickener for recovering clear process
water for reuse in the washery and to settle
agglomerated coal particles with the addition
of flocculant, before final dewatering in high
frequency screens. Dewatering of froth as well
as flocculation of tailings is not efficient in the
washery. Moisture content of dewatered froth
is around 24% whereas clarified water coming
out from the overflow launder of thickener
contains high ppm of suspended solids. Due to
flooding condition at the entry part of screen
bowl centrifuge, coal slurry with very fine coal
particles (<0.038 mm) overflows into the effluent
pond. This stream is called centrifuge centrate
and it accounts for considerable loss of low ash
coal particles into tailings. Sometimes, this low
ash material also get mixed with the feed to
flotation cell which results in increase of
consumption of reagents as well as reduction of
throughput to the cell.
Fig. 1 shows a schematic diagram of fine coal
dewatering circuit of the washery. As explained
above, the performanc e of the fine c oal
dewatering circuit is not entirely satisfactory.
An effort is therefore, essential to investigate the
causes of the poor performance of the fine coal
dewatering process and to find out the ways
for improving the recovery of clean coal from
the fines. The major concerned area is to reduce
the fine clean coal moisture.
Fine clean coal from screen bowl centrifuge
generally contains about 24% moisture. The
high moisture content in the coal reduces its
heating value, creates shipping and handling
problems, increases transportation cost, and
reduces the input and coke yield of metallurgical
charges. The effective dewatering of fine and
ultrafine coal is bec oming inc reasingly
important for the coal industry. Even relatively
modest reductions in product moisture will lead
to large financial savings in an output of
hundreds of millions of tons per year.
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MPT-2013
Both in centrifuge and filtration, cake bed is
formed which imparts resistance to the passage
of water. The cake bed can be considered as
complete packed bed with parallel capillaries
which vary in size. Moisture in small pores is
difficult to remove due to high capillary
pressure as determined by the Laplace equation.
(Tao et al, 1999) estimated that, for coal with a
contact angle of 600, a vacuum of 25 in. Hg or 85
KPa will be unable to remove the capillary
water from pores smaller than 0.87 µm (Tao et
al, 1999).It was reported in the literature that a
linear relationship exist between cake moisture
and the average feed particle size with solid and
screen bowl centrifuges (Sargent et al, 1979)
another factor, which affects both fine and
coarse particles, is the size distribution of pores
in a packed bed (Hogg, 1995). Within a packed
bed is where surface properties such as contact
angle and surface tension affect dewatering. The
size distribution of the pores in a packed bed is
directly related to the size distribution of
particles within the feed.
Vacuum filtration is one of the dewatering
processes widely used in the coal industry. It
has some substantial advantages, e.g., low cost
and easy to design and maintain, over
hyperbaric filtration and centrifugal filtration
(Parkh et al, 1988). The most significant
advantage is that of continuous operation under
relatively simple mechanical conditions.
Continuous vac uum filter mac hines,
particularly rotary drum filters and rotary disc
filters, have long proved themselves to be
capable of producing satisfactory performance
in various commercial applications.
Efforts for enhanced fine coal dewatering were
presently focused on using chemical reagents
to alter coal surface characteristics and slurry
rheology for favorable dewatering conditions.
It has been demonstrated that enhanced fine
coal dewatering can be achieved by a number
of different approaches such as the use of
flocc ulants and surfactants (Palmes and
Laskowski, 1993). This has also been
demonstrated in another research work for

ultra-fine coal dewatering (Groppo and Parekh,
1996).The same trend also found in works of
Tata Steel professionals (Banerjee et al, 1998 and
Mukherjee et al 2003). Flocculants have been
used in vacuum filtration to decrease the
moisture of the product cake. This has been tried
in centrifuges with minimal results, due to the
weakness of the long polymer chain present in
flocculants and the strong forces occurring in a
centrifuge (Mishra, 1988). These strong forces
break apart flocculants before they can aid in
dewatering. Even though flocculants cannot be
effectively used in centrifuges, fuel oil has been
well known to aid in dewatering which lowers
interfacial tension results in lower pressure
differences needed to dewater. Surfactants and
coagulant can also be used for dewatering of
coal fines in centrifuge. Different combination
of reagents can also be used for reduction of
moisture of fine as well as ultrafine coal in
filtration.
Coagulants are electrolytes having an opposite
charge to the particle thus causing charge
neutralization, when dispersed in the system
and overcoming their resistance to approach
each other and form large aggregate upto 1mm
in size. Alum (Aluminium sulphate), ferric salt,
lime and sulfuric acid are commonly used
coagulants. Flocculants are high molecular
weight, water soluble, long chain organic
polymers known as polyacrylamides and are
very effective in producing large, rapidly settling
flocs upto 1mm size.
2. Experimentation
The froth samples were collected from washery
of West Bokaro. The slurry contains about 12-
15% solids. The granulometry tests were
conducted with these samples. In dewatering
study, a batch centrifuge, simulating the plant
centrifuge, was used for experimentations.
Different flocculants (F), surfactants (S) and
coagulant (C) were studied for reduction of fine
clean coal moisture as given in Table No.1. The
reagents used in this study were procured from
suppliers M/s. Daiichi Chemicals, M/s. Suyog
Chemicals, M/s SNF India Pvt. Ltd., M/s. Nalco
Chemicals, M/s Tel Labs Chemicals. To study the
filtration performance of fine clean coal, vacuum
210
MPT-2013
filtration tests were performed with filter cloth
as medium. Some of the tests were also
conducted with the froth generated in the
laboratory froth flotation cell to control the pulp
density (PD) of the feed. The PD of fine clean coal
was varied between 15 and 20%. Moisture in
the clean coal before and after centrifuging as
well as filtration was determined as per the
standard procedure.
3. Results and Discussion
3.1. Assessment of Present condition of
Dewatering of fine clean coal
The plant moisture data have been collected
from washery of West Bokaro periodically. The
salient points of fine clean coal moisture content
and froth flotation cell load are summarized
below
· Moisture content of clean coal fines primarily
varies between 21-26%. Sometimes it went
beyond this range.
· Fines (-0.5 mm fraction) treated in West
Bokaro vary around 20% of ROM. Sometimes
this fraction went up to 25%.
3.2. Laboratory dewatering tests with froth
samples of washery
The granulometry of fine clean coal samples was
given in Table 2. It was observed that mean size
distribution of the coal is about 0.05 mm. High
ultrafine fraction present in froth was actually
responsible for poor dewatering characteristics
of this coal.
3.2.1. Tests with coal fines in centrifuge
The preliminary test was conducted with
flocculant F1 in lab centrifuge at 15 % PD. Table
3 showed the moisture retention by fine coal
after centrifuging in presence of this reagent. For
making comparison to the same base level, tests
were also c onduc ted without using any
flocculants. It was observed that with increase
in this flocculant addition, moisture retention
in solids increases. This increase in moisture can
be attributed to the entrapped moisture within
the flocs formed due to addition of flocculant.
This entrapped moisture could not be taken out

by centrifuging and this resulted in increase in
moisture of fine coal.
Tests with surfactants and coagulant were also
carried out in batch centrifuge as shown in Table
4. The surfactants S2, S3, S4 and C had shown
reduction in fine clean coal moisture while the
reagent S1 had shown negative impact on
moisture reduction of fine coal. Out of these
surfactants tried in the laboratory, S2is found
to be most effective on fine coal moisture
reduction. The reduction in moisture content
was found to be about 23% for S2 at dosage of
0.25 kg/t. The required higher dosage of
surfactant for fines was attributed for the higher
surface area of coal particles, (since the material
was finer and c ontribution of -0.038 mm
fraction was about 43%), where surfactants
primarily adsorbed on the surface of the coal
particles and drained out the surface adsorbed
moisture and pore moisture.
Another set of tests were performed with
surfactants S2, S4 and coagulantC at higher
density of froth (20% PD) to study the effect of
pulp density of froth on dewatering process. For
making comparison to the same base level, tests
were also c onduc ted without using any
reagents. It was observed that the moisture
content of dewatered cake in batch centrifuge
was 21.8% which was lower than that obtained
in tests with PD of 15%. The results were
summarized in Table 5. It was observed that
effectiveness of the reagents was reduced at
higher concentration of solid in froth. It was
found that the moisture content reduced by 13%
from the base level of 21.8% for surfactant S4.
As the tests with batch centrifuge did not yield
expected results, filtration tests with coal fines
from both the washeries were explored under
vacuum condition. The tests were performed at
vacuum condition to obtain faster kinetics in a
generally slow filtration process.
3.2.2. Tests with coal fines in vacuum
filtration
Since centrifuge is not effective is arresting
escape of ultra-fine coal particles, filtration is
211
MPT-2013
also tried out to enhance dewatering process of
coal. In this context, dewatering tests were
conducted without any reagent addition to
assess filtration behaviour of fine clean coal
under vacuum condition with laboratory
Buchner funnel fitted with filter cloth. The
performance of this blank test was compared
with tests at various dosage of dewatering aids
(flocculant, coagulant and surfactant). The
results of vacuum filtration at 15% PD are
summarized in Table 6. Flocculant behaved in
the same way as that observed in batc h
centrifuge tests. Encouraging results were
observed at high dosage of 0.5 kg/t for
c oagulantC. Dewatering process is also
enhanced with surfactant addition also. The
results indic ated about 15.3% moisture
reduction from base level at low dosage of 0.1
kg/t of surfactant S4. This may be caused by
formation of smaller agglomeration of coal fines
as compared to that produced with flocculants.
These agglomerations, due to their smaller size
and characteristics did not entrap much
moisture.
4. Conclusions
Among the various reagents tried for
dewatering of fine coal slurry, the
surfactantS2was found to be best among the
dewatering aids tried for reduction of moisture
in centrifuge. The reduction of moisture was
found to be good with lowering of moisture by
23% from the present level of moisture of fine
clean coal (24%). Flocculants and coagulant were
not found effective in reducing the moisture level
in centrifuge.
As centrifuge is not effective in retaining low
ash containing ultra-fine coal, vacuum filtration
is tried for enhancing dewatering process of fine
coal. In vacuum filtration, coagulant C was
found to be most efficient among different
dewatering aids used. However to achieve this
reduction in fine coal moisture, consumption of
coagulant C will be higher at 0.5 kg/t. Whereas,
almost same reduction in moisture is observed
for surfactant S4 at a relatively lower dosage of
 MPT-2013

0.1 kg/t. The maximum reduction in moisture
was found to be 16.8 % for C and 15.2% for S4.
The findings of the laboratory experimentations
tried at plant level in a planned manner and
shown encouraging results. The potential of the
above mentioned reagents will help to enhance
the current dewatering practices employed in
West Bokaro washery and composite clean coal
with lower moisture content from the current
level could be produced in a continuous basis.
Acknowledgements
The authors are thankful to Tata Steel
Management and R&D support staff for their
active involvement for carrying out the plant
trials and laboratory studies.
Ultrafine Clean Coal, Coal Preparation, 17,
61.
Banerjee, P.K., Chakraborty, D.S., Choudhury,
B.R., Rao P.V.T., 1998. Reduction in Moistureof
Composite Clean Coal of West Bokaro and
Jharia, Report No. R&D-RAP-003/96-01-14/
98, R&D Division, Tata Steel.
Mukherjee, A.K., Banerjee, P.K., Bhatnagar, A.K.,
Dutta, A., Prasad, S., 2003. Strategy to
Improve Fine Clean Coal Yield at West
Bokaro, Tata Search, 57.
Mishra, S.K., 1988. Princ iples of
Dewatering,Industrial Practice of Fine Coal
Processing: Proceedings of the Conference at
Hidden Valley, Somerset, Pa, Klimpel and
Luckie, pp. 213.

References Table 1: Different reagents used for testing

Flocculant (F) Coagulant Surfactant (S)
Tao, D., GroppoJ, G., Parekh ,B.K.,1999. Effects of
Polymers and Metal ions on Vacuum Poly amide (F1) amide (C) Copolymer of
amide and acrylate
Filtration of Fine Coal, Coal Preparation, 20, (S1)

207. Poly amide (S2)

Sargent, D.H., Cheng, B.H., Contos,G.Y., 1979. Functional groups

Poly amide (S3)
Dewatering and drying of fine c oal:
equipment performance andcosts. In: Rogers, Poly acrylate (S4)
S.E., Lemmon, A.W. (Eds.). Proceedings of
Symposium on Coal Cleaning to
AchieveEnergy and Environmental Goals, Table 2: Size analysis of fine clean coal samples
Hollywood, FL. US Environmental Protection of West Bokaro
Agency, Office of Researchand Development
(USEPA), 464. Size, mm Weight%
Hogg, R., 1995. Dewatering of Fine Coal, High + 0.5 2.05
Efficiency Coal Preparation: an International -0.5+0.25 9.71
Symposium, Kawatra, 409. -0.25+0.15 9.1
Parekh, B.K., Groppo, J.G., Stotts W.F., 1988. A -0.15+0.075 17.86
Review of Fine Coal and Refuse Dewatering/ -0.075+0.053 9.02
Drying Techniques, Technical Report,
-0.053+0.038 9.15
University of Kentucky.
-0.038 43.28
Palmes, J.R., Laskowski, J.S., 1993. Effect of the
Properties of Coal Surface and Flocculant
Type on the Flocculation of Fine Coal, Table 3: Dewatering tests with fine clean coal
Minerals and Metallurgical Processing, 10 (4), using flocculant F1 in centrifuge
218. Sl. No Dosage of Time of Moisture in
reagent, g/t centrifuging, s solid,%
Groppo, J.G., Parekh, B.K., 1996. Pilot-Scale 1 0 10 24.2

Evaluation of Hyperbaric Filtration of 2 5 15 25.7

3 10 15 27.8
4 20 15 28.2
5 40 15 32.5

212
 MPT-2013

Table 4: Tests with Surfactants and coagulants Table 6: Tests with different reagents at various
for coal fines at PD 15% in batch centrifuge dosages with coal fines at 15% PD in Vacuum
filtration
Sl. No. Dosage, kg/t Moisture content
in fines, %
Sl. No. Reagent Dose, kg/t Moisture, Reduction
With S1 added % in
moisture,
1 0 24.2 %
2 0.0625 27.6
1 Blank - 23.1 -
3 0.125 28.2
4 0.250 28.2 4 C 0.06 22.3 3.5
5 0.500 29.5 5 -do- 0.35 21.7 6.1
With S2
6 -do- 0.50 19.2 16.8
6 0.0625 19.3 7 S3 0.05 22.1 4.3
7 0.125 18.6
8 -do- 0.1 21.6 6.5
8 0.250 18.6
9 0.500 19.9 9 -do- 0.3 21.3 7.8
With S3
10 S3 0.05 22.2 3.9

10 0.0625 21.9
11 -do- 0.10 21.8 5.6
11 0.125 20.5 12 -do- 0.3 21.4 7.4
12 0.25 21.1
13 S4 0.050 21.4 7.4
13 0.5 21.2
With S4 14 -do- 0.1 19.6 15.2
15 -do- 0.50 19.6 15.2
14 0.125 20.9
15 0.25 20.5
Fine clean coal
16 0.5 19.8
With C
Froth Screen
Bowl
Centrifuge
17 0.125 22.4
Centrate
18 0.250 21.4
Thickener
19 0.50 20.8 Flotation feed
Flotation
Cle a r wa te r
Overflow (Re circula te d in
Table 5: Tests with Surfactants and Coagulants Tailings
pla nt)

for coal fines at PD 20% in batch centrifuge Thickener

High
Underflow frequency Ta ilings
Sl. No. Dosage, kg/t Moisture content screen
in fines, %
With S2
Fig. 1: Generalized flow diagram of fine coal
1 0 21.8 dewatering circuit
2 0.0375 20.9
3 0.0625 19.5
4 0.125 19.8
5 0.250 18.9
6 0.500 20.0
With S4

7 0.0375 20.8
8 0.0625 20.4
9 0.125 20.1
10 0.250 19.4
11 0.500 19.8
With C

12 0.125 20.7
13 0.250 20.2
14 0.500 20.6

213
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Sedimentation Studies on Non-Coking Coal Fines with Some

Industrial Flocculants
K M P Singh1*, G Udayabhanu2, T Gouricharan1 and J.K. Panday1
1
CSIR- CIMFR, Dhanbad, Jharkhand, India-828108
2
Indian School of Mines, Dhanbad, Jharkhand, India- 826004

Abstract
The Indian non-coking coal deposits are characterized as high ash and difficult-to-wash. Quality
improvement by beneficiation is almost mandatory due to MoEF notification to use < 34% ash coal
for all power plants except those located at pithead. With the ambitious target of adding another
2,00,000 MW of power generation by the year 2017 in India the demand for coal is bound to grow
and washing capacity is to be increased. The coal washeries will require to handle about 25 to 30
mt of coal fine (– 0.5mm). Waste waters produced from coal preparation plants contain high
percentages of ultrafine particles and inorganic impurities, which are composed of clay minerals
such as kaolinite, illite, muscovite, quartz, and coal particles. The natural sedimentation rate of
these particles present in colloidal and finely divided suspended form is very slow. To enhance the
settling rate a few flocculants were applied to a Non – Coking coal collected from an operating coal
washery. The main objective of clarification is to obtain clear water with a low turbidity value. It
is important to produce good quality recirculation water for the smooth operation of the plant;
otherwise the presence of suspended and dissolved solids in the wastewater can lead to a reduction
in the efficiency of the washing process. The paper discusses the details of studies and its observation
on the settling behavior of non-coking coal fines suspension by using different commercial
flocculants.
Keywords: Coal fines; thermal coal; sedimentation; flocculation.

1. Introduction notification, new washeries, both in public

With the ambitious target of adding another
2,00,000 MW of power generation by the year
2017 in India the demand for coal is bound to
grow and also has plan to wash 250 mt of non –
coking coal (http://coal.nic.in). The Indian non-
coking coals are categorized as high ash and
washing of high ash coal was made mandatory
by the Ministry of Environment & Forests
(MOEF) from environment angle (http://
moef.nic.in). To abide by the government
* Correspending Author:
singh_kmp@yahoo.co.in
sector & private sector are coming up in big
way. The wet c oal washing is generally
practiced in India and abroad, it requires a huge
amount of water for its beneficiation. Starting
from coal mining to its end use fines were
generated, due to handling and crushing down
to the desire size as per the washing equipment
limitation. During the whole process the fines
below -0.5 mm size is generated at the rate of
10 % of the whole coal in general and needs care.
If we consider coal fines at the tune of 10% of
the whole coal as we need to wash by 2017,
about 25 Mt of coal fines will have to handle in
total.

214
 MPT-2013

The coal fines are usually fed to thickeners to Table 1: size analysis data of all the coal fines
recover the water and depending upon the ash with determined ash and moisture
content of these fines, they are either mixed with
JSW -1 JSW -2 Washery ‘J’ Washery ‘K’
the clean coal or sent as rejects. The heavy and
large particles of effluent are allowed to settle Size μm
Wt
%
M
%
Ash
%
Wt
%
M
%
Ash
%
Wt
%
M
%
Ash
%
Wt
%
M
%
Ash
%

automatically, but the fine and c olloidal 500-250 45.8 1.7 34.8 48.4 1.7 33.5 44.7 3.6 56.5 21.9 1.6 52.0
250-125 21.8 1.4 33.2 19.3 1.7 33.0 15.2 3.9 51.0 37.0 1.3 38.9
particles remain suspended due to high surface 125-63 12.0 1.4 34.1 9.7 1.8 32.7 6.1 3.8 51.3 5.0 1.5 44.2
area to mass ratio and electrical charge between -63 20.4 1.4 41.4 22.6 1.8 42.5 34.0 3.0 67.6 36.1 1.8 51.5

the particles. Various workers (Sabah and Erkan, 100.

0
1.7 34.8
100.
0
1.7 35.4 100 3.4 59.1
100.
0
1.6 46.6

2006; Farrow and Swift, 1996; Singh et al, 2010

and 2011; Das et al, 2006) found that the coal fine
partic les require adding some external
chemicals for flocculating, charge neutralization
to enhance the settling rate through addition of
appropriate chemicals. The interaction of multi-
component fine coal tailings (suspended coal
fines, associated clay/ mineral matter particles)
with various coagulants and flocculants are
important in the process of settling (Das, et al.
2006). The flocculants used are of cationic,
anionic and non anionic in nature and the
effectiveness of any type of flocculants depends
upon the molecular weight and charge density
of the polymer. The actual effect of flocculent on
the multi-component system coal is still not
very clear. The present paper highlights the
effect of flocculent on the multi-component
system and discusses the settling behavior of
thermal coal fines suspension by using different
flocculants. The instrumental analyses like
XRD, ICP and contact angle measurement were
conducted to understand effects of mineral and
2.1. Instrument used
The instrument DCAT – 11, is used for contact
angle and sedimentation rate determination,
ICAP-6300 Duo of M/S Thermo Fisher Scientific
used to determine minerals present in the coal,
XRD were used to studies the mineral phase
present in the fines of the coal slurry.
The sedimentation experiments were carried
out using the freshly prepared flocculent stock
solutions. The stock solutions were prepared by
dissolving per calculated amount of flocculent
with de-ionized water. Hand blender was used
to uniform/ homogenized mixing of the
flocculent.
2.2. Flocculent used
The list of flocculants used is shown in Table 2.
Table 2: Chemicals/Flocculants tested in the
experiment
Sl.
No.
Flocculants Supplier/Manufacturer

related parameters in the process of settling. An 1 SUPERFLOC16 (off white granular solid) Cytec Industries Inc, USA
attempted was made to understand the settling
LABUFLOCC 300 (off white granular B.K. Giulini Gmbh,Giulini
behavior of thermal coal fines suspension using 2 solid) Str.2
industrial polymers. LABUFLOC N 036 (off white granular B.K. Giulini Gmbh,Giulini
3 solid) Str.2
2. Experimental
4 LABUFLOC C 301(off white granular
solid)
B.K. Giulini
Str.2
Gmbh,Giulini

A portion of all the four collected coal fines

sample were wet screened at – 0.5 mm (500 µm) 5 CAT floc N-8102 plus (Pale Yellow Liquid) NALCO Chemicals Ltd.

size and further wet screened at 250, 125 and 63

µm size to know the percentage distribution of 6 NALCO N-83384 (white amorphous solid) NALCO Chemicals Ltd.

the particle. The ash and moisture as per Indian

7 NALCO (off white liquid) NALCO Chemicals Ltd.
standards were determined for different size
fractions. The analysis result for all the four coals 8 CRISTOL T50 (Clear, Pale Yellow liquid) Krishna Antioxidant, Mumbai
is depicted in the Table 1 below
9 CRISTOL N50 (Clear, Pale Yellow liquid) Krishna Antioxidant, Mumbai

215

The experiment on sedimentation/ Flocculation
study was also carried out using the DCAT 11
instruments with an attac hment of a
sedimentation cone. The whole experiments
were carried out at 5 % solid concentration of
coal sample. The repeatability of the experiment
was assured for every test run.
3. Result and Discussion
The wet screen analysis reflect that the
laboratory crushed coal and the coal under
actual plant run condition -63 ìm size particle
varies significantly as depicted in the Table 1.
The ash and moisture analysis of the
representative coal slurry sample confirms that
the coal fines are non-coking, medium coking
coal and c oking in nature it was further
confirmed by pertographic reflectance.
It may be seen from the size analysis data as
presented in Table 1, that 34.0 % is of – 240 mesh
size for both the washery slurry and about 20
percent is for the laboratory crushed coal
sample. For both the laboratory crushed coal
the ash of the below – 0.5 mm is about 35 percent
while ash of the two washery varies from 46.7
to 59.1 percent.
Figures 1: XRD Graphs of -0.5 mm coal sample the coal A & B ‘JSW-1’ & ‘JSW-2’ from laboratory
crushed and the two coal C & D, ‘J’ & ‘K’ from coal washery
216
MPT-2013
The contact angles of the sample were studies
to know the hydrophobicity of the coal fines
(Arnold, B J, and Aplan, F F, 1989; Singh, K M P,
Udayabhanu, G, Gouri Charan, T and Haldar D
D, 20; Singh, K M P, Udayabhanu, G and Gouri
Charan, T; 2013). It was determined by powder
method using the instrument DCAT-11 and
noted that the coal is very hard to float rather
not to float. It was in the order of ‘K’ > ‘JSWA’ ³
‘JSWB’ > ‘J’.
Petrography reflectance ‘Ro’ value is in the order
of; ‘K’ > ‘JSW-1’³ ‘JSW-2’ > ‘J’
The coal slurry even at 5% of solid contain is
very difficult to study the sedimentation rate
without using any floc culent under
c onventional jar test method. The
sedimentation studies with & without
flocculent were carried out using DCAT-11 this
inc lude c ontact angle determination.
Repeatability of the experimental results
confirmed in all the cases (Singh et all 2013 in
press).
Coal is a multi-c omponent system, the
associated gangue (clay, mineral matter, etc.) and
the nature of exposed outer coal surface varying
extensively. The polymeric flocculent were used
 MPT-2013

for faster settling rate to recover the coal slurry present in the coal. The ICP analysis data revels
and recirculation water in the coal washing that all though the two laboratory crushed coal
plant. having almost similar ash contain but differ
significantly in minerals containing Al, Na and
The XRD analysis suggests that the minerals
Ba as recorded higher for JSW-1 with respect to
present in the coal fines are almost in similar
JSW-2.
phase but differ in percentage for the laboratory
crushed coal while the two coal washery slurry The coal washery slurry fines ‘J’ having higher
sample the phase and percentage also differ. The elemental concentration of Al, Mn, Na, Pb and
figures 1 (A, B, C & D) of the XRD of coal slurry Zn for all the tested coal minerals, while the Fe
sample are as below: Ca and Mg is recorded higher for the washery
Table 3: ICP result of the – 500 µm for all the coal ‘K’. This may also be observed in the XRD
four coal fines (concentrations in ppm). graphs for the coal fines which have altered the
sedimentation behavior markably.
Where, BDL= below detection limit
The figure. 2 shows the sedimentation results of
Wt % J JSW A JSW B K
coal slurry at 5 % solid concentration recorded
AI 20.275 13.243 12.351 14.684
Fe 6.653 6.101 6.444 9.764
through instrument for two laboratory crushed
As BDL BDL BDL BDL
coal size -500 µm. Initially the larger size heavier
Ba 0.071 0.133 0.118 0.085 particle settles faster than the colloidal particle
Ca 0.233 0.452 0.445 0.652 without using any flocculent. The anionic floc
Cd 0.0004 0.0002 0.0003 0.0004
at 20 gm/t of dosages, there is about only 3-4
Co 0.005 0.004 0.004 0.005
Cr 0.023 0.017 0.016 0.022
times increase in settling rate for the coal larger
Cu 0.011 0.01 0.009 0.013 size particle, but for the colloidal particle the
K 1.313 1.546 1.835 1.604 increase in sedimentation rate recorded to about
Li 0.010 0.005 0.005 0.005 15 times of the natural sedimentation rate.
Mg 0.469 0.376 0.424 0.542
Mn 0.152 0.081 0.116 0.118 Further in Figure 3 at similar solid concentration
Na 0.211 0.135 0.096 0.194 of coal slurry but higher presentation of colloidal
Ni 0.005 0.005 0.005 0.008
particle settle slower and for complete settling
Pb 0.034 0.016 0.016 0.017
Sr 0.008 0.019 0.015 0.021
takes longer time with respect to the laboratory
Zn 0.076 0.028 0.027 0.025 crushed coal.
The mineral present in the coal slurry sample Retarded flocculation/ sedimentation were also
were studied by Inductively Coupled Plasma- observed in some cases, even from the normal
Optical Emission System (ICP – OES), model sedimentation rate, i.e. having negative effect on
ICAP-6300 Duo of M/S Thermo Fisher Scientific. the sedimentation rate during the experiment.
The samples for ICP analysis were prepared
followed by the ASTM standard (D6357)
Standard Test Methods for Determination of
Trace Elements in Coal, Coke, and Combustion
Residues from Coal Utilization Processes by
Inductively Coupled Plasma Atomic Emission
Spectrometry, Inductively Coupled Plasma
Mass Spectrometry, and Graphite Furnace
Atomic Absorption Spectrometry. Figure 2: Natural Sedimentation behavior of -
.5 mm two laboratory crushed coal fines at 5
The instrument ICAP-6300 Duo of M/S Thermo percent of slurry solid concentration (without
Fisher Scientific used to determine minerals any flocculent)

217

Figure 3: Natural sedimentation behavior of
below -0.5 mm coal washery fines below at 5
percent of slurry solid concentration (without
any flocculent)
The two laboratory crushed coal having almost
similar in ash content reflectance value, contact
angle/ hydrophobicity and -240 mesh size
partic les but differ signific antly in their
sedimentation behavior with flocculent. On
other hand the two slurry sample from coal
washery varies significantly in their size, ash
content, reflectance value, contact angle/
hydrophobicity but similar in colloidal size are
considerably similar in sedimentation behavior
without flocculent but varies with flocculent.
On the application of suitable polymeric
flocculent more than 15 times higher rate was
recorded but the same flocculent may not found
suitably effective for all the four coal fines.
To come at any final conclusion a more detail
studies of the coaly matter is also required to
understand the adhesion mechanisms of the
fines and flocculent are required and a few of
them are in progress like SEM, FTIR etc.
4. Conclusion
The detailed sedimentation studies on the four
different samples showed that apart from size
of the fines, its ash, mass to surface area, surface
charge/ maturity of the coal have notable role
on the sedimentation rate. With particular
types of flocculent system the sedimentation rate
may be enhanced to more than 15 times of
natural sedimentation rate from normal settling
218
MPT-2013
behavior. For better utilization, towards zero
waste & to conserve our natural resources an
extensive study is required.
Acknowledgements
The authors are thankful to the Director CIMFR,
Dhanbad for giving his consent for publishing
this paper. The authors are also thankful to the
washery management for providing the sample
and flocculent, and to all the staff members of
the division for providing valuable support.
Thanks are extended to Dr R E Masto for
providing the ICP analysis data.
References
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http://moef.nic.in
Sabah, E., Erkan, Z.E., 2006. Interaction
mechanism of flocculants with coal waste
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Farrow, J.B., Swift, J.D., 1996. A new procedure
for assessing the performance of flocculants,
Int. J. Miner. Process., 46, 263-275.
Brostow, W., Pal, Sagar., Singh, R.P., 2007.A model
of flocculation, Materials Letters 61, 4381–
4384.
Karagüzel, C., Demir, U., ªahbaz, O., Çýnar, M.,
Uçar, A., Öteyaka, B., Kelebek, ª., 2008. Effects
of oleate and calcium chloride on the settling
behaviour of fines from a lignitic coal, The
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Paste Backfill and Thickened Tailings Disposal – A Solution for

Sustainable Development in Mining Industry
Gautam Chatterjee1, Atul Gandhe1, Primeau Pierre2 and Chris Lee2
1
Golder Associates Ltd., India.
2
Golder Associates Ltd. Sudbury, Ontario, Canada.

Abstract
The technology to ‘engineer mining waste’ is now available. As we are very much aware there are
many burning issues now in India related to the Mining Industry - such as land availability for
surface storage of the waste, environmental and social impacts, health and safety demands,
utilization of mine waste products, backfill with adequate strength to restrict surface subsidence
and to improve productivity etc. A solution for sustainable development of mining in India calls
for Paste and Thickened Tailings Technology.
This paper examines the importance and positive impact the development of Paste and Thick-
ened Tailings technology has brought to the worldwide mining industry. It examines the technol-
ogy and via examples also presents the challenges, broad environmentalbenefits it can bring and
finally, lists some recommendations. The technology enables maximum water recycling, limits
fresh water usage, requires smaller surface footprints for waste storage, reduces risks of dam
failures, reduces likelihood of seepage from waste facilities, ensures faster reclamation etc. The
major recommendation for sustainable development in mining is to maximize the return of
tailings underground as paste backfill and for the rest -the elimination or conversion of tradi-
tional tailings dams and opting for thickened tailings disposal facilities. Reclamation can and
should then occur concurrently with the tailings placement. Similarly, Paste / Thickened Tailings
Technology enables remote filling of abandoned and working underground mines or naturally
occurring voids below surface in order to mitigate the risk of collapse or neutralize subsidence
issues. The advantages include direct and indirect benefits to the mining operation which create
opportunities to improve key aspects such as stope cycle time, production scheduling, water
consumption and re-handling, mine environment and many other factors.
This paper intends to describe the properties of an “engineered waste” and illustrate some of the
environmental and economic benefits of using paste thickened tailings technology. The objective
of this paper is to introduce the concept and disposal of mine waste in the form of paste or
thickened tailings to outline the potential improvements to underground mining and surface
mineral waste management.
1. Introduction India. This paper presents some specific ex-
amples where a new tailings disposal technol-
Availability and permitting of land for disposal ogy- dewatered or “thickened tailings”- is prov-
of mine wastes and tailings is an increasing
ing to be advantageous over “conventional
problem in many parts of the world, including

220

slurry” impoundmentsin regions of the world
where space limitations and/or water scarcity
are dominant factors in determining the feasi-
bility of mining projects. Additional examples
of studies which compared “conventional
slurry” and “thickened tailings” that favoured
the “thickened tailings” alternative for new or
existing Tailings Storage Facilities (TSF) due to
significant gains in storage capacity are also de-
scribed.
The dewatering process is the primary method
of producing high solids slurries for the miner-
als industry. Thickener outputs can produce a
range of tailings consistencies for surface dis-
posal options from low to moderate yield
stresses, easily pumpable using either centrifu-
gal or positive displacement pumps. When
thickeners are combined with filtration equip-
ment they can produce more concentrated slur-
ries for delivery to ‘dry disposal’ and./or back-
fill applications. The thickening process, al-
though operated successfully in a large range of
sites around the world, is poorly understood
and predictive design of thickening devices is
still empirical. Although predictive models of
thickening do exist, the correlation to reality is
often poor and there is a desperate need to bring
the two together to make rational improve-
ments to thickener design and operation. There-
fore, whilst some would dismiss the models as
being unacceptable for predictive design, they
are very useful in formulating expected opera-
tional trends and providing an understanding
of the directions one should take in improving
operational performance.
Interest in the potential use of high density,
thickened tailings has recently increased signifi-
cantly. Reasons for considering this new tech-
nology vary across projects, but commonly in-
clude the need to conserve water, to lower risk
of TSF dam failure, to facilitate closure and site
rehabilitation and to even reduce overall costs.
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MPT-2013
As with any new technology, there has been
some tendency to overstate its potential ben-
efits. This paper reflects on whether or not the
potential benefits ascribed to the new paste and
thickened tailings technology some years ago
have been realised. It is suggested that the key
proven benefits appear to be reduced operat-
ing costs in some cases, reduced wall-building
costs and reductions in water consumption.
One key potential benefit that has not been uni-
versally achieved is a reduction in the footprint
of the tailings facility. Reports in the literature
highlight the sometimes confusing nature of
trade-off studies. Unless full life-of-mine costs
are considered, these studies can be mislead-
ing and incorrect. The need is to establish a con-
sistent basis for comparative studies.
2. Background of underground Mine
Backfill and Surface Disposal
Underground Mine Backfill
The use of paste for backfill purposes was con-
ceived in the early 1970s. The Bad Grund Mine
in Germany applied concrete mix design and
pumping know-how to continuously deliver a
paste backfill mixture of tailings, coarse rejects
and cement underground. During the 1980s,
cycloned tailings, further processed in a thick-
ener and drum filter, was combined with ce-
ment and water in a batch mixer to deliver
paste backfill underground at Lucky Friday
Mine in the United States. These two systems
represent some of the first approaches to paste
backfill processes (Ahmed et. al., 2010). Paral-
lel studies taking place during the 1980s and
early 1990s in South Africa and Canada have
collectively led to a greater understanding of
paste backfill operations and system require-
ments. The research work performed in the
South African mines illustrated that mix de-
signs — varying the coarse and fine solid frac-
tions — plays an important role for pipeline
 MPT-2013

flow resistance and eventual strength gain for we will see in the next section it is clear that
ground support. paste technology has evolved from its main use
as backfill for underground mining applica-
In Canada, much of the research was gener-
tions to find further uses in the mining indus-
ated from the Sudbury area. Here, substantial
try and beyond. The reasons for adopting its
insight was gained in understanding paste rhe-
use are evident in the inherent benefits it pos-
ology and preparing the mix recipe (Ahmed et.
sesses both operationally and environmentally
al. 2010). It is very important to understand
(Ahmed et. al. 2010). In the Indian coal mining
the tailings material which is used to prepare
industry the hydraulic sand stowing method
the paste and to control the addition of the
for the underground mines has been predomi-
recipe constituents with proper proportions.
nant for the past few decades. However, the
The idea of paste preparation is to develop a
scarcity of river sand is resulting in the need to
composition which is flowable and at the same
search for other appropriate backfill materials
time can provide good backfill strength while
for the sustainable and complete extraction of
minimizing cement addition. An appreciation
future resources. In the Indian metal mining
of the colloidal properties in paste backfill re-
industry, cemented hydraulic fill has been in
vealed that it was generally necessary that the
use at many mines and due to its own safety
fines portion (less than 20 microns) be at least
related problems a better alternative is being
15 weight % (wt%) of the solids. These fines
looked into by the mining industry.
enable a suitable level of water retention, coarse
Surface disposal
suspension and lubrication that assists with
In the early 1970s the idea of thickening metal
pipeline transport. Further testing showed that
mine tailings for surface disposal was also be-
the coarse fraction (greater than 20 microns)
ing developed and this strategy was first em-
could be varied significantly without adversely
ployed at the Kidd Creek mill site located in
affecting the paste backfill’s flow properties.
northern Ontario (Robinsky 1999). However,
This in turn has allowed mines to optimize their
paste concepts for surface disposal gained in-
solids particle size distribution to allow for the
creasing acceptance in the metal mining in-
disposal of a variety of solid wastes (such as
dustry in the year 2000 with the success of
acid generating rock). Balancing the need for
Bulyanhulu in Tanzania (Landriault 2006).
backfill strength gain against the blending of
Bulyanhulu became the first mine/mill com-
coarser solids combined with lower water con-
plex to incorporate both surface and under-
tent allows the mine to custom design “engi-
ground paste disposal techniques for the com-
neer” their paste backfill. Another important
plete treatment of mill tailings (Landriault et
aspect stemming from this research was that
al. 2001). Concurrently, other factors such as
paste backfill could, in some instances be de-
improvements in dewatering/thickening tech-
livered in a controlled manner underground
nologies, mounting government pressure for
by gravity alone, without pump assistance, by
operations to reduce their environmental im-
varying the viscosity (water content) of the
pact as well as the realization of the true ben-
paste.
efits of paste for surface disposal drove mining
Paste backfill has its origins in the mining in- companies to consider and adopt this means of
dustry. A robust paste backfill mix design tak- tailings management. The co-disposal of mine
ing into consideration the underground envi- waste rock with paste is also gaining momen-
ronment is critical to operational success. As

222

tum under the premise that reactivity (acid
generation) of the waste rock containing
sulphides is greatly reduced if enveloped by
paste (Wilson 2001).
Surface disposal of tailings is also a major area
of concern in India. The main challenges faced
by the mine management are the land and en-
vironmental issues, practical problems in tail-
ings transportation and water handling. The
Indian mining industry can therefore look into
the introduction of paste technology not only
for underground backfilling but also for sur-
face disposal which is currently being prac-
ticed successfully in various countries. In 1973
the Falconbridge owned Kidd Creek Metal-
lurgy Plant in the town of Timmins, Ontario,
Canada was the first site to utilize disposal of
thickened tailings (Engels and Dixon-Hardy
2004). The conventional storage facility was
converted to High Density Thickened Tailings
(HDTT) to eliminate further raising of the tra-
ditional retaining embankments that were situ-
ated on very soft and sensitive clay founda-
tions (ICOLD and UNEP 2001). The tailings are
discharged from spigots on a central ramp that
as of 2005 was 20m in height. At the base of
this ramp is the 32 m diameter, high compres-
sion thickener that produces a slurry density
of 60 – 65% solids (Golder 2005).
3. Understanding slurry, thickened tailings
and paste
The tailings or the waste mixed with water to
allow the mixture to flow is termed “slurry”.
“Thickened Tailings”, as the name suggests, in-
volves the mechanical process of dewatering
low solids concentrated slurry (Fourie 2003).
This is normally achieved by using compres-
sion (or high rate) thickeners or a combination
of thickeners and filters. High Density Thick-
ened Tailings (HDTT) is defined as tailings that
have been significantly dewatered to a point
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MPT-2013
where they will form a homogeneous non-seg-
regated mass when deposited from the end of a
pipe (Welch 2003). They are not to be confused
with paste tailings which are a higher (and
more expensive) degree of dewatering o pro-
duce very dense slurry that is often pumped to
its final storage facility using positive displace-
ment pumps (however, centrifugal pumps can
be used to pump paste where the tailings prop-
erties are favourable). HDTT is often defined in
industry where the tailings have a high yield
stress (typically higher than 20 Pa but no higher
than 100 Pa) and typically do not require deep
cone or paste thickening technology. The bleed
water from the thickened tailings released upon
deposition can be collected and transported
using conventional centrifugal pumping.
The idea of HDTT is to stack the pulp to form a
self-supporting conical pile thus reducing the
height and retention forces of the containing
perimeter embankments. Increasing the con-
sistency (thickness) of the tailings pulp (i.e. in-
creasing the %solid concentration) creates
higher beach slopes angles in comparison to
tailings discharged as a slurry The tailings are
generally discharged from topographical high
points within the tailings storage facility or by
riser towers or central ramps (ICOLD and
UNEP 2001). Liberated water after deposition
and any surface runoff is collected in a pond at
the toe of the pile. Typical slope angles of 1 – 3.5
degrees can be achieved to form a self-draining
easy reclaimable shape (ICOLD and UNEP
2001). Paste tailings disposal often achieve
higher beach slope angles compared to HDTT.
A “Paste”is”tailing slurry” that is sufficiently
dewatered or a dry granular material which is
mixed with sufficient water to fill the interstices
between the particles so that the material be-
haves as a fluid. The material retains all the
water between the particles because of colloi-
dal electrical particle charge of the fines which

bonds the solid particles to the water mol-
ecules. In this state, the paste can be trans-
ported through a pipeline but has no critical
flow velocity, i.e., the velocity at which the solid
and liquid components separate into two dis-
tinct phases. If more water than can be held
between the particles is added to the paste, it
becomes slurry and the material does have a
critical flow velocity. In this state, the mate-
rial will flow through the pipeline but will sepa-
rate out (segregate) into two distinct phases if
the velocity in the pipeline drops below the
critical value (Landriault 1998).
In general, a material with less than 15 wt% of
fines (20 microns or less) will typically not pos-
sess the colloidal properties to form a paste and
cannot be transported as such. However, the
colloidal properties of the material are gov-
erned not only by the size but also by the
chemical content and mineralogical composi-
tion of the particles. This means that different
materials will form a paste with different size
distributions. Each granular material must be
tested independently to determine its proper-
ties and its behaviour as a paste (Landriault
1998). Both the production plant and the pipe-
line distribution system have to be designed
with these specific properties in mind.
“Paste” is a densified uniform material of such
mineralogical makeup and particle size distri-
bution, that it will bleed only minor quantities
of water when at rest, experience minimum
segregation and can be moved in a pipeline at
velocities well below that of critical velocities
for similar sized materials at lower pulp or
solids densities (Ahmed et. al. 2010). Pastes can
remain sitting in a pipeline for extended peri-
ods of time when no cementitious material is
present. The slump is normally measured us-
ing an American Society for Testing and Mate-
rials (ASTM) 30.5 cm (12 in.) slump cone, a stan-
dard tool used in the concrete industry. Miner-
224
MPT-2013
alogical make up is very important as not all
materials even within the outlined size distri-
bution may make a paste. Different mineral
types have different tendencies to retain col-
loidal water. A fundamental paste property is
its non-segregating nature, i.e., the ability to
retain water. From a backfill perspective some
minerals may be inherently weak while oth-
ers may react with components (including
binder) in the paste matrix to produce poor
strengths.
Mathematically, the behavior of paste can gen-
erally be described using the Bingham plastic
model, where the material possesses a defined
minimum shear stress (or yield stress) to ini-
tiate flow. Once this is overcome, the paste be-
haves like a fluid exhibiting a linear shear rate
to shear stress relationship and can be de-
scribed by the following equation (Ahmed et.
al. 2010):
τ           = τy+ηγ                                              
Where,
τ           = shear stress [Pa]
τy = yield stress [Pa]
η           = plastic viscosity [Pa s]
γ           = shear rate [1/s]
In practice, many parameters contribute to the
rheological behavior of paste, including par-
ticle size distribution, particle angularity, sol-
ids density, mineralogy and the general nature
of the suspension (colloidal chemistry). There-
fore, rheological testing is integral to examin-
ing a material’s paste-making properties. Once
defined for a particular material, its rheologi-
cal profile (Equation 1) can be established to
predict pipeline friction loss or pressure drop.
In paste processes, one of the key items to un-

derstand is its rheological behavior as it dic-
tates pipe and pump sizing. One of the funda-
mental prerequisites for the design and imple-
mentation of a successful thickened tailings or
paste systems is a comprehensive [1]understand-
ing of the rheological characteristics of the ma-
terial. Although rheological characterisation is
often out-sourced, it is essential that design
engineers and plant operators have a grasp of
the variables which must be considered, the
questions that need to be addressed and famil-
iarity with rheological assessment principles
in order to determine the validity of data pro-
vided for the purpose intended. Good rheologi-
cal data for one particular sample under one
specific set of testing conditions is generally
insufficient for design and/or optimisation of
entire processing systems and the related
equipment. An ‘up-front’ understanding of how
rheological parameters affect and influence op-
erations will result in more efficient and sus-
tainable plant performance and can mitigate
many potential problematic issues.
4. Type of backfill methods& thickened
tailings disposal
Historically backfill has tended to be sand (or
coarse tailings) and cement placed as a slurry
into the mined stope. This is often referred to as
cemented hydraulic fill (CHF). This method is
used in many operations today. Variants on this
are also used including the placement of aggre-
gate or rock into the stope with the cemented
fill, such as those described by Bloss et al. (1993).
The application of paste backfill is used in many
operations and in many cases it is the preferred
choice of backfill to use in an underground mine
for a variety of reasons addressed in this pa-
per. Backfill has two functions in underground
mining. The first is as a construction material
that is used to create a floor to mine on top of, a
wall to mine next to, and a roof or head-cover
to mine under. The second function is to pro-
225
MPT-2013
vide an important means of providing support
to the surrounding rockmass.
The following are the underground backfills
used in the mines (Grice 1998):
· Hydraulic backfill
Deslimed mill tailings slurries, with average
densities 70%Cw (solids by weight). The coarser
fractions are placed underground as hydraulic
backfill and the slimes rejected to the surface
dam.
· Paste backfill
Total mill tailings filtered or thickened to around
75-80%Cw to which cement and water is then
added to achieve the required rheological and
strength characteristics. Any rejects to the dam
are at the full tailings sizing range.
· Rock backfill
Waste rock from surface or underground and
crushed or screened to a specified top size. This
can be placed as is or with cemented hydraulic
backfill slurry or cement water slurry. Crushed
rock with cement slurry is typically called ce-
mented aggregate fill (CAF) while waste rock
with cement slurry is typically called cemented
rock fill (CRF).
Backfill source materials are largely made up
from the tailings waste generated due to min-
ing and mineral processing operations. The
hydraulic fill uses the coarse tailings (sands)
from cyclone underflow, whereas paste gener-
ally includes the full mill tailings, though varia-
tions on this do exist. While this differentiates
the two fills from a perspective of particle gra-
dation, the major aspect for the performance
differs is that paste has a reduction of excess
water, modified pipeline rheology (or pipeline
flow), greater consistency as an engineered
backfill and the ability to be placed in the stope
at a faster delivery rate. This thereby results in
 MPT-2013
Properties CAF/CRF CHF Paste Fill
generating significant opportunities for in- PlacementState Dry (90-95% solids) 60-73wt%solids 65-85wt%solids

creasing productivity in the underground mine TransportSystem Raise, mobile equip.,

separate cementsystem
Borehole/pipelineviagravity or Borehole/pipelineviagravity
pumped or pumped

(Slade 2010). In CHF there are basically two sig- Cementedvs.UncementedCementedoruncemented Cementedoruncemented Cementedonly

nificant disadvantages. The first is to design Water/Cement(w/c)Ratio Low w/c ratio, high
binder strength
High w/c ratio, very low
binder strength
Lowtohighw/cratio,lowto
highbinderstrength
and construct permeable barricades to retain Segregation Stockpile segregation, Slurry settlement segregation, Nosegregation
reduced strength&stiffness low strengths in areas
the backfill and permit the free drainage of ex- Stiffness High stiffness if Lowstiffness Lowtohighstiffness

cess transport water. Barricades construction TightFilling

correctly placed
Hardtotightfill Cannottightfill Easytotightfill

is the critical path activity between the comple-

tion of production in a stope and the commence-
ment of filling. The second disadvantage is the
management of water in the fill and the require-
ment to pump this water out of the mine and
wait for percolation to be complete before add-
ing subsequent lifts to the fill mass.
The type of backfill used by an underground
operation will depend on the configuration of
the mining process, the mining method, the
depth and the orientation of the orebody, as
well as the materials available for use as fill.
As stated above the three most important types
of modern backfill are rockfill/aggregate fill
(CRF or CAF), slurry or cement hydraulic fill
(CHF) and paste fill and the choice between
these three types is site-specific and will de-
pend on the particular requirements of each
mining operation (Landriault 1998).
The different backfill systems have different
capital and operating costs attached to them
but these costs have to be considered in the con-
text of the cost structure of the particular min-
ing operation. The different characteristics of
the three types of fill can be described as ad-
vantages and disadvantages in terms of the
configuration of the particular mining opera-
tion and it is these advantages and disadvan-
tages which determine the most suitable type
of backfill for that operation rather than the
generic costs of the system. A summary of the
characteristics of the three types of backfill is
presented in Table 1.
Table 1: Comparison of different under-
ground backfills
A more technical appreciation of paste is com-
monly said to include the following character-
istics:
1. non-segregating mixture of solids and
water
2. exhibiting minimal water bleed when left
idle
3. a measurable slump and yield stress
4. with no critical flow velocity
5. percent solids dependent on particle size
distribution (PSD) and other factors.
The benefits of utilizing paste technology in a
backfill application for underground mining
include:
1. Typically lower cement content
2. Pipeline delivery (more efficient delivery
method for high volume flow rates than
trucking)
3. Minimal dilution compared to CHF and CRF
4. Utilization of tailings / waste materials
readily available on site
5. Complete filling of a void to the back of the
opening
6. Homogeneous strengths in the paste mix
design (no zones of weakness) compared
to CHF and CRF
7. Flexibility in formula design for different
applications
8. Reduced stope cycle time compared to
both CHF and CRF
9. Reduced mine dewatering costs compared
to CHF
10. Reduction of in-rush risk in the mine due
to fill barricade failure compared to CHF

226

Figure 1 shows what the slump looks like for
the differing natures of material and as this is
the most simple and common test for evalua-
tion.
Paste–177mmslump Paste–253mmslump Slurry–no slump
Figure 1: Generic examples of the
slumpconetest for differing back fill mix
designs
5. Advantages of paste backfill
One of the biggest opportunities presented by
the application of paste fill is in the increased
production rates achievable in the mine, as a
result of quicker filling and curing. Filling time
may be reduced by up to 70% compared to CHF
due to the ability to pour the paste fill in ex-
tended lifts without waiting for a previous lift
to drain and cure before starting the next lift.
Filling time is also typically much faster that
CRF since CRF is delivered by truck and it is
quite common that the filling rates will be re-
stricted by traffic considerations and even with
the use of additional trucks, no further in-
creases in CRF haulage rate can be obtained.
Mostly in a variety of situations the cost of the
backfill is also reduced compared to CHF, as a
backfill with less water in its matrix, requires
less cement to achieve the same strength char-
acteristics. This is though not always true as it
depends on the mineralogical composition and
its interactive behavior. The ability to increase
production rates and reduce stope cycle sched-
ule times has the potential to add significant
value to an operation. This is simply driven by
mining more ore at a quicker rate which al-
lows greater revenue to be made in a shorter
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MPT-2013
period of time than would otherwise occur
(Slade 2010).
In other situations the use of a paste backfill in
combination with changes to a mining method
in an underground mine can also provide op-
portunities to an operation that may not have
been achieved by the use of a paste backfill alone
(Li et al. 2002).
The significance of designing, planning and
scheduling the backfill system requirements for
an underground mine with as much focus as
the ore production requirements cannot be
underestimated in achieving its strategic plan
for the underground mine. Many cases exist
where backfilling has not had the same focus
as the production of ore. In such scenarios
schedule flexibility is reduced, grade flexibility
and opportunities to optimise the mining plan
are constrained. This can result in some short
term benefits but the medium term production
plans and ore reserves may be put at risk (Slade
2010).
The benefits achieved from the indirect and di-
rect factors in an underground mine will vary
dependent on a case by case scenario for any
given mining operation. In the majority of sce-
narios, if increase in mineral production rate
can be achieved, this will provide the greatest
gain to the business. Where multiple stopes
are being mined in one or more ore bodies,
the mine production schedule is constrained
by the time taken to fill and cure any stope, the
greatest gain can be delivered through the use
of paste backfill.
6. Advantage of thickened tailings for
surface disposal
A reasonable question might be ‘what is the
real difference between conventional and high
density thickened tailings’ (referred to as TT
from now on)? Key differences are that a TT

releases very littlebleed water, there is virtu-
ally no particle segregation down the beach and
the material exhibits a finite, measureable yield
stress. One of the key potential advantages of
TT is the reduction in the volume of water de-
posited in the TSF that needs to be managed.
As an example, increasing the solids content
from 32% (a common value for conventional
tailings) to 60% (noting that values in excess of
70% have been achieved (McPhail et al., 2004)),
1.35 m3 less water per dry tonne is transported
to the TSF. This additional water is recovered
during the thickening process and is potentially
available for re-use. Upon deposition at the TSF,
very little bleed water is usually released, un-
like conventional tailings, where some of the
additional water transported to the TSF is po-
tentially recoverable from the TSF. There is no
agreement on whether these potential water
savings are real or not; indeed, Lyell et al. (2008)
argued that, as long as the TSF is operated at a
high rate of rise, it acts like a very large gravity
thickener and just as much water can be re-
covered as is possible with in-plant thicken-
ers. However, data emerging from field imple-
mentation of TT, as discussed later, contradicts
this view and shows that water savings are
very real.
Some of the characteristics of thickened tail-
ings which contribute to the successes are:
1. Higher average consolidated density of
thickened tailings resulting in lower overall
volume of impoundment and related foot-
print
2. Higher angle of repose of thickened tailings,
result in lower required perimeter contain-
ment dams and smaller footprint
3. Higher % recovery of process water used
in tailings transport, with associated
reduction in fresh water needs for the
milling process
228
MPT-2013
4. Smaller space used up by ponded water in
the impoundment and reduced impacts of
seepagewater on the surrounding envi-
ronment and lower risks to the contain-
ment structures
5. Non-segregation of particle sizes upon
deposition, resulting in lower average
permeability of the tailings deposit ,
increased resistance to surface erosion and
reduced loss of tailings-contact water
through seepage
6. Higher saturation level of tailings in the
long term, post-closure scenario, which
reduces the oxidation rate and rate of acid
drainage production from acid generating
tailings
7. Easier access conditions to the deposit
surface allowing easier on-going monitor-
ing and progressive closure activities
8. Easier land reclamation and environmen-
tal restoration
The surface disposal of tailings in the form of
paste has its own advantages over the conven-
tional approach of slurried tailings disposal.
Subject to any particular case, this is likely to
afford some gains for the operation and indeed
if tailings are deposited as a paste may well
yield significant gains for the mining business
in the following aspects as summarised by
Slade et al. (2009):
1. smaller tailings disposal footprint with a
steeper beach angle
2. smaller dam engineering
3. lower water consumption
4. negligible bleed water release
5. no critical velocity required to avoid set-
tling in transportation to discharge
6. reduced closure cost depending on the
characteristics of the waste
7. reduced operating risk liability

8. reduction in contamination/leachate
potential
9. potential to not require impervious liner
and monitoring systems.
The table below elaborates the features and
benefits of both these system in an overall
manner for the industry.
Table 2: Perceived benefits of Paste &Thick-
ened Tailings, after Tacey and Ruse (2006)
Feature
1. Similar capital and reduced
operating cost to wet disposal
2. Costs accrued during
Operations
3. Increased deposit Strength
4. Decreased land footprint by at
least doubling practical stacking
height
5. Decreased demand for borrow
materials for construction
6. Reduced risk of leachate
seepage
7. Reduces or eliminates ponding
and low strength mud deposits
8. Prompt creation of firm, convex
draining surface at completion
9. Earlier, better surface leaching
and drainage
10. Potentially large reductions in
water use
11. Reduced potential for
liquefaction
12. Potentially reduced heating,
lower water demand
13. Reduced reagent requirements
7. Installations in India
The Paste-backfill technology has arrived in
India, with the first two plants being con-
Economic/Engineering Benefits
Overall economic benefit
Reduced requirement for bonds
and provisioning
Reduced risk of facility failure
Reduced land purchase cost
Less transport and construction
Better leachate and reagent
recovery
Increased surface accessibility
Early creation of trafficable
surface
Early leaching of toxicants from
surface
Reduced need for water collection
and supply facilities, pumping
energy savings
Deposit remains firm and will not
flow
Reduced energy use, cost savings
Potential operating cost savings
MPT-2013
structed in Lead Zinc mines in western India.
The major parameters of the plants are:
Parameters Plant 1 Plant 2
Yearly voids to be filled - m3 10,00,000 8,00,000
Paste Production dry t/h 400 200
Paste Production wet m3/h 240 160
Cement Consumption % 8 8 – 12%
Target strength KPa 1000 400 - 700
Mining method SLOS (sub level open stoping) LHOS (long hole open stoping)
SG of tailing sample / Solid SG 3.00 2.90
Flow Parameters:
178mm Slump 254mm Slump 178mm Slump 254mm Slump
• Paste Solid content wt % 79.12 77.34 74.1 71.8
Environmental/Social Benefits • Yield strength – static Pa 223 125 400 200
• Viscosity – Pas 0.9 0.35 0.6 0.32
Less resources applied to end of
pipe and less corrective action • Slurry bulk density – t/ m3 2.12 2.06 1.95 1.9
Costs met by operator, no long
term liability to community
Target UCS strength 1.1 MPa 0.75 MPa
Avoids offsite environmental and Thickener underflow % wt 70% 65%
safety impacts
Flocculent dosage 20 g/ t 40 g/t
Reduced sterilisation of
productive land, reduced clearing Filter cake solid % wt 83% 81%
Paste Solid content % wt 79% 75%
Reduced clearing for borrow Tailings slurry Conc. wt % 45 – 50% 58 – 65%
materials, reduced greenhouse
gas production in construction
Reduced risk of ground and
surface water contamination
8. Conclusions
Reduced fauna injury, increased
operator safety The future demands paste and thickened tail-
Progressive or more rapid
rehabilitation
ings for the sustainability for the Indian Min-
More rapid establishment of ing Industry. The technology for producing and
vegetation, reduced duration of
dust generation transporting paste is now well established
Reduced footprint from water
collection structures or impacts
worldwide and is in the process of being intro-
from diversion or abstraction
duced in a few Indian mines. Paste is being
Reduced offsite environmental
and safety impacts used as backfill and ground support at many
Lower greenhouse gas emissions underground mines around the world. The next
Reduced pollution risk
step is to apply this technology to surface dis-
posal in India and make use of the many benefi-
cial characteristics of paste.
The discussion in this paper demonstrates ar-
eas of improvement that can be achieved in an
underground mine by backfilling with paste
rather than CHF or CRF/CAF and also the ad-
vantages of tailings disposal as Paste or Thick-
ened tailings. The advantages include direct
benefits and indirect benefits to the mining op-
eration which create opportunities to improve
key aspects such as stope cycle time, produc-
tion scheduling, water consumption and re-
handling, mine environment, footprint require-
ment and many other factors. These all com-
229

bine to counter the additional capital cost as-
sociated with the design and constructionof a
paste backfill plant or a thickened tailings dis-
posal plant and lend themselves to creating a
higher NPV for the mining operation.
It is recommended to follow a systematic ap-
proach for the application of paste technology
and thickened tailings for any Indian mining
scenario beginning with material testing and
feasibility studies to investigate the potential
benefits paste and/or thickened tailings tech-
nology can successfully bring to a given project.
A case by case analysis is recommended for
every underground mine or surface disposal
application as the scale of gains may differ de-
pending on the nature and type of the mining
method.
Acknowledgements
The authors express thanks to Golder Associ-
ates for the support in developing this paper
and the opportunity to publish it at this con-
ference.
References
Ahmed, I., Francoeur, R., Anderson, J., and
Brown, R., 2010. Paste benefits and appli-
cations from the mining industry to land
reclamation. International Solidification-
Stabilization Technology Forum 2010, S/S
Tech, GPTL, Paterson & Cooke, pp. 153-
159.
Bloss, M.L., Cowling, R., and Meek, J.L. 1993. A
procedure for the design of stable cemented
fill exposures, in Proceedings Minefill 93,
South African Institute of Mining and Met-
allurgy, Johannesburg, South Africa.
Engels, J., and D. Dixon-Hardy., 2004. Tailings
disposal - Managing increasing higher vol-
umes of waste from mines. 7th Interna-
tional Symposium on Environmental
Geotechnology and Global Sustainable
230
MPT-2013
Development, Helsinki and Espoo, Finland,
June 8-10, 2004:. 13
Engels, J., and Dixon-Hardy, D., (2004). Tailings
disposal - Today’s storage of high volumes
of waste from mines. JKMRC Conference
2004, Brisbane, Australia:. 13.
Fourie, A. B., 2003. In Search of the Sustainable
Tailings Dam: Do High-Density Thickened
Tailings Provide the Solution, School of
Civil and Environmental Engineering,
University of the Witwaterstrand, South
Africa:: 12.
Grice, T., 1998. Underground Mining with Back-
fill. The 2nd Annual Summit – Mine Tail-
ings Disposal Systems, Brisbane 24-25
November 1998.
ICOLD and UNEP, 2001. Bulletin 121: Tailings
Dams - Risk of Dangerous Occurrences,
Lessons learnt from practical experiences.
Paris.144
Landriault, D., 1998. Short Course Notes: Back-
fill Technology and Practice – Paste Tech-
nology for Underground Backfill, Austra-
lian Mineral Foundation, Glenside, South
Australia, June 28–29.
Landriault, D., 2006. They Said It Will Never
Work – 25 Years of Paste Backfill 1981–
2006, 9th International Seminar on Paste
and Thickened Tailings, Limerick, Repub-
lic of Ireland, April 3–7, Australian Cen-
tre for Geomechanics.
Landriault, D., D, Welch., and Frostiak, J., 2001.
Bulyanhulu Mine: Blended Paste Backfill
and Surface Paste Deposition / The State
of the Art in Paste Technology, Minefill
2001: Proceedings of the 7th International
Symposium on Mining with Backfill, So-
ciety for Mining, Metallurgy and Explora-
tion (SME), Seattle, Washington, USA, Sept
17–19.
 MPT-2013

Lyell, K.A., Copeland, A.M., and Blight, G.E., Slade, N.M., Guilfoyle, K., and Kropp, W., 2006.
2008. Alternatives to paste disposal with Strategic and tactical mine planning in
lower water consumption. Proceedings of Enterprise Mine, Mount Isa Copper Op-
the 11th International Seminar on Paste erations, in Proceedings Strategic ver-
and Thickened Tailings (Paste08), Kasane, sus Tactical Approaches in Mining,
Botswana, 5–9 May 2008. Fourie, A.B., Australian Centre for Geomechanics,
Jewell, R.J., Slatter, P., and Paterson, A. Perth, Australia, Section 39.
(eds.). Australian Centre for TACEY, W. and RUSE, B. 2006. Making tailings
Geomechanics, Perth. pp. 171–178. disposal sustainable; a key business issue.
Li, T., Singh, U., Coxon, J., Grice, T., and Paste and Thickened Tailings – A Guide.
Sainsbury, D., 2002. Development and ap- 2nd edn. Jewell, R.J. and Fourie, A.B. (eds.).
plication of paste fill using dry tailings, in Australian Centre for Geomechanics,
Proceedings First International Seminar Perth. Ch. 2.
on Deep and High Stress Mining, Austra- Welch, D., 2003. Advantages of Tailings Thick-
lian Centre for Geomechanics, Perth, Aus- ening and Paste Technology, Responding
tralia, Section 12. to Change - Issues and Trends in Tailings
McPhail, G., Noble, A., Papageorgiou, G., and Management - Golder Associates Report:.5
Wilkinson, D., 2004. Development and Wilson, W. 2001. Co-Disposal of Tailings
implementation of thickened tailings dis- and Waste Rock, Geotechnical News: 44–
charge at Osborne Mine, Queensland, 49.
Australia. Proceedings of the International
Seminar on Paste and Thickened Tailings
(Paste 2004), Cape Town, South Africa, 31
March – 2 April 2004. Australian Centre
for Geomechanics, Perth. p. 33.
Robinsky, E.I., 1999. Tailings Dam Failures Need
Not Be Disasters – The Thickened Tailings
Disposal (TTD) System, CIM Bulletin, vol-
ume 92 (1028), 140–142.
Slade, N.M., 2010. Paste backfill — adding value
to underground mining. Paste 2010, Pro-
ceedings of the 13th International Semi-
nar on Paste and Thickened Tailings, 3–6
May 2010, Toronto, Canada, pp. 99-110.
Slade, N.M., Felipe, F., Wilson, S., and Palkovits,
F., 2009. Increasing Value in Mining Op-
erations through the Application of Paste,
in Proceedings 13th AusIMM Mill Opera-
tors Conference, Australian Institute for
Mining and Metallurgy, Adelaide, Austra-
lia.

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MODELLING & SIMULATION

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Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Model for Segregation of Binary Mixture of Solids

S. Narasimha Reddy and P.S.T. Sai*

Department of Chemical Engineering, Indian Institute of Technology-Madras,
Chennai - 600036

Abstract
The industrial applications of fluidization technology (Coal gasification, power granulation etc.)
involve solid mixtures of particles which have differed in size, density and both. The fluidization
of binary mixture of solids occurs in a definite velocity interval, which is the beginning and
complete fluidization velocity of the mixture. The beginning fluidization velocity is where pressure
drop line deviates from fixed bed behavior and the complete fluidization velocity is the ultimate
value of the bed (i.e. whole bed is at fluidization mode). The beginning fluidization velocity does
not dependent on the initial arrangement of bed, however, the complete fluidization velocity
dependent on the physical properties of solids, composition of mixture and the level of segregation.
Using the fundamental theoretical considerations and force balances between the different
segregated layers, the beginning and complete fluidization velocities of mixture are calculated.
The calculation of complete fluidization velocity is being studied because of the lack of knowledge
between particle suspension and segregation at full fluidization condition. Using the empirical
correlations available in literature, the complete fluidization velocity is found by fitting the
unknown parameters determined by experimental results. The model predicted values are
validated with experimental data.

Keywords: Fluidization; Solid mixture; Segregation; Modeling.

1. Introduction velocities are empirical and their validity limit

to specific combinations of mixtures. All the
The treatment of multi component particle beds
correlations neglecting the voidage variation
in fluidization finds large number of
with composition and do not consider the
applications. There are many correlations
actual phenomenology of the fluidization
available in literature to predict the minimum
process where axial distribution of solids varies
fluidization of binary mixtures. The common
and follows different type of patterns
approach to predict the minimum fluidization
dependence on the physical properties of solids.
of binary mixture is to modify the correlation
The aim of the present study is to modify the
used for the mono component bed to account
existing correlations proposed for particle that
for two components in the bed. The correlations
differ in size or density or both. The modified
proposed to calculate minimum fluidization
correlations are compared with experimental
* Correspending Author: P.S.T. Sai, Department of Chemical data available in literature thus testing the
Engineering, Indian Institute of Technology-Madras, Chennai model for segregating binary mixture of solids.
- 600036

235
 MPT-2013

2. Methodology
180  g ubf , m (1   m ) 2
Formisani et al., 2008 developed a model for  (    g )(1   m ) g (3)
segregating binary mixtures of solids, where d avg 2  m3
total fluidization occurs in a specific velocity
interval i.e. ubf and ucf. Here, the mixture voidage (    g ) gd 2f , p m3
is calculated from experimental results but
uf ,p  (4)
180  g (1   m )
calculation of the voidage is important at well
mixed conditions. Cheung et al., 1974 proposed (1   f ) (1   p )
the following correlation which is valid for u f hm x f 3 2
 u p ho (1  x f )
different sized particles with the limitation of ( d ) f f ( 3p d p2 )
ucf ,m 
size ratio not more than 3.. (1   m ) (1   ) (5)
3 2
hm  3 2p (ho  hm )(1  x f )
(1 x f )2
( m d avg ) ( p d p )
um  u p 
  (1) There is no relationship between progress
u f  u f  fluidization and segregation phenomena, an
After obtaining the um from the above equation, empirical correlation which is valid for specific
the mixture voidage can be obtained using mixtures only was proposed by Formisani et
Cozney-Karman equation and from this the al., 2008. This is valid for above three
beginning fluidization veloc ity c an be combinations (size or density or both).
calculated. For calc ulating the c omplete 3
fluidization velocity, the progress of component hm (1   m )  p
k x f (1  x f ) (6)
segregation and fluidization phenomena at ho (1   p )  m3
complete fluidization conditions are required.
The beginning fluidization at segregated
From the mass balance between three layers
conditions can be calculated as,
(packing layer, mixing layer, and fluidized
layer), one interaction parameter, k, which will (  g )g
u bf , s 
account for above phenomena is defined. The  x (1   ) (1  x f )(1   p ) 
 
model parameter ‘k’ is a fitting parameter and 180  g  f 3 2 f  3 2  (7)

  f d  p d 

is independent of composition and is obtained
by comparing with experimental results. In the For density segregating binary mixtures at well
present work, one k value applicable to many mixed conditions, a correlation is proposed in
literature experimental data is obtained. the present study to calculate the minimum
For different sized particles, Equation (1) fluidization of the binary mixture as shown
satisfactorily fits not only the data due to below.
Formisani et al., 2008 data but also other
experimental literature data up to diameter
    p 
xf  f  (1  x f )  

ratio of 4. For well mixed conditions, the 1
 
avg    avg  (8)
expressions for calculating the values of davg,
um uf up
ubf,m, uf,p, and ucf,m are given in the equations
2,3,4 and 5 respectively.( Formisani et al., 2012, For density segregated mixtures, ubf , ucf can be
2011, 2008), calculated by,
1 xf (1  x f )
  180g ubf ,m (1   m ) 2
d avg df dp (2)  (  f   g ) x f  (  p  g )(1  x f ) (1   m ) g (9)
d2  m3
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 MPT-2013

The comparison between experimental and

(  f , p   g ) gd 2 m3 calculated values of beginning fluidization
uf ,p  (10)
180 g (1   m ) velocities and complete fluidization velocities
at well mixed conditions are shown in Fig. 1
(1   f ) (1   ) and 2 respectively. The predictions are good
u f hm x f  u p ho (1  x f ) 3 2p
( 3f d 2 ) ( p d ) with beginning fluidization velocity when
ucf ,m 
(1   m ) (1   ) (11) compare with experimental results. Even for
hm  3 2p ( ho  hm )(1  x f )
( m3 d 2 ) ( p d ) size ratios more than 3, the values are well
fitting with experimental data in both
For density segregating mixtures at segregated
beginning and complete fluidization velocities.
condition, the beginning fluidization (ubf) can The comparison between experimental and
be calculated as calculated values of beginning fluidization
velocities at segregated conditions is shown in
ubf , s 
(  f   g ) x f  (  p   g )(1  x f ) g
Fig. 3. Here, the predictions are good with
 x (1   ) (1  x f )(1   p )  (12) experimental data
180 g  f 3 2 f  
  f d  3p d 2  0.35

3. Results and discussions

0.3

0.25

3.1. Size- segregating mixtures

Theoretical ubf,s (m/sec)

0.2

0.15
0.2
Experimental data of Rao et al., 2011
0.18
Experimental data of Rao et al., 2011
0.1
Experimental data of Nienow et al., 1978 Experimental data of Nienow et al., 1978
0.16
0.05
0.14
Theoretical u bf,m (m/sec)

0
0.12 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
Experimental ubf,s (m/sec)
0.1

0.08

0.06

0.04
Fig. 3 Comparison between experimental and
0.02
calculated values of beginning fluidization
0
0 0.02 0.04 0.06 0.08 0.1 0.12

Experimental ubf ,m (m/sec)

0.14 0.16 0.18 0.2
velocities at segregated conditions for size
segregation
Fig. 1: Comparison between experimental and
calculated values of beginning fluidization 0.35

velocities at well mixed conditions 0.3

0.25
Theoretical ubf,s (m/sec)

0.4

0.2
0.35 Experimental data of Rao et al., 2011

Experimental data of Nienow et al., 1978 0.15

0.3
Theoretical ucf,m (m/sec)

0.25 0.1
Experimental data of Rao et al., 2011
0.2
0.05 Experimental data of Nienow et al., 1978

0.15
0
0.1 0 0.05 0.1 0.15 0.2 0.25 0.3 0.35
Experimental u bf,s (m/sec)
0.05

0
0 0.05 0.1 0.15 0.2 0.25

Experimental ucf,m (m/sec)

0.3 0.35 0.4
Fig. 4 Comparison between experimental and
calculated values of beginning fluidization
Fig. 2 Comparison between experimental and velocities at segregated conditions for density
calculated values of complete fluidization ve- segregation
locities at well mixed conditions

237
 MPT-2013

3.2. Density-segregating mixtures 4. Conclusions

To calculate the minimum fluidization of binary
From this finding um and substitute in the
mixture, a model available in literature was
modified form of Kozeny-Carman equation
used. This avoids use of empirical correlations.
implemented for binary mixtures. The
For different sized particles, the empirical
predictions are good and well fit with the c orrelation and model equations are
experimental data. To find ucf, same approach
satisfac tory for c alculating u mf of binary
adopted as mentioned above. The comparison mixture. For different density particles, the
between experimental and calculated values of
model equation equations are modified by
beginning fluidization velocities and complete
knowing the phenomena at c omplete
fluidization velocities at well mixed conditions
fluidization c onditions and satisfac torily
are shown Fig. 5 & 6 respec tively. The compares with experimental data. Work is
prediction with experimental data is good. The
under progress for binary mixtures that differ
equation (12) can be used to calculate ubf,s. The both in size and density.
c omparison between experimental and
calculated values of beginning fluidization Notation
velocities at segregated conditions is shown in d particle diameter, µm
Fig. 4.The predictions are not good because d avg Sauter mean diameter,µm
density ratio more impact towards segregation dB diameter of bigger component, µm
than size segregation. dS diameter of smaller component,µm
0.3
g gravity acceleration, m.s-2
0.25
Experimental data of Rao et al., 2011

Experimental data of Nienow et al., 1978

h height of the particle layer, m
ho initial bed height, m
Theoretical u bf,m (m/sec)

0.2

0.15 k best fit parameter or interac tion

0.1 parameter, -
0.05 u superficial gas velocity, m/s
0
0 0.05 0.1 0.15 0.2 0.25 0.3 umf minimum fluidization velocity, m/s
Experimental u bf, m (m/sec)

ubf,ucf beginning and complete fluidization

Fig. 5: Comparison between experimental and velocity, m/s
calculated values of beginning fluidization umix mixture c omponent fluidization
velocities at well mixed conditions velocity, m/s
x volume fraction, -
0.6

Greek Letters
0.5

 voidage, -
Theoretical u cf,m (m/sec)

0.4

Q particle density, kg/m3

0.3

Q avg average density of mixture, kg/m3

0.2
Experimental data of Rao et al., 2011

Experimental data of Nienow et al., 1978

Qg gas density, kg/m3
0.1

µg gas viscosity, pa.sec

0
0 0.1 0.2 0.3

Experimental ucf,m (m/sec)

0.4 0.5 0.6
Subscripts
f,p of the fluidized, packed component (or
Fig. 6 Comparison between experimental and layer )
calculated values of complete fluidization ve- m,s of the homogenous mixture, segregated
locities at well mixed conditions mixture
H,L heavier component, lighter component

238
 MPT-2013

References Two-Solid Beds. International Journal of

Chemical Reactor Engineering. 10.
Cheung, L., Nienow, A.W., Rowe, P.N., 1974.
Nienow, A.W., Rowe, P.N., Cheung, L.Y.L., 1978.
Minimum fluidisation velocity of a binary
A quantitative analysis of the mixing of
mixture of different sized particles.
two segregating powders of different
Chemical Engineering science. 29, 2–4.
density in a gas-fluidised bed. Powder
Formisani, B., Girimonte, R., Longo, T., 2008. The
Technology. 20, 89–97.
fluidization process of binary mixtures of
Noda, K., Uchida, S., Makino, T., Kamo, H., 1986.
solids: Development of the approach based
Minimum fluidization velocity of binary
on the fluidization velocity interval.
mixture of particles with large size ratio.
Powder Technology. 185, 97–108.
Powder Technology. 46, 149–154.
Formisani, B., Girimonte, R., Vivacqua, V., 2011.
Rao, A., Curtis, J.S., Hancock, B.C., Wassgren, C.,
Fluidization of mixtures of two solids
2011. Classifying the fluidization and
differing in density or size. AIChE Journal.
segregation behavior of binary mixtures
57, 2325–2333.
using particle size and density ratios.
Formisani, B., Girimonte, R., Vivacqua, V., 2012.
AIChE Journal. 57, 1446–1458.
Extended Validation of a Model of
Segregating Fluidization of Homogeneous

*******

239
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Review on Simulation of Work Index Determination

Anil Pathak, Raj Kishore, U.K.Chanda, K. K.Sahu, S. Pati and N.P.H.

Padmanabhan*
Indian Institute of Technology, Bhubaneswar, 751013, Odisha, India.

Abstract
The Bond grindability test developed by F.C. Bond in the middle of twentieth century gives the
Bond’s Work Index, an important engineering parameter for design of industrial closed circuit
grinding mills. The work index is an empirical measure of the energy input required for grinding
ores from a specific particle size to the design particle size. Bond designed the work index ball mill
with strict dimensional and functional specifications and developed the experimental methodology
for determining the Work Index in a laboratory. The method has become so popular that even
today project engineers use this parameter for design of grinding circuits, even though a lot of
improvements have been reported in the literature with better understanding of the energy-size
reduction relationships.
In this paper, an effort has been carried out to present and review the literature on important
simulation models and applicability of these simulations has been proved on our ore sample.

Keywords: Bond test; work index; simulation.

1. Introduction grindability of an ore, from which the work

The experimental procedure for determination
of the Bond’s Work Index, as stipulated by Bond
(Bond, F.C., Maxson, W.L., 1943, Bond, F.C., 1949,
Bond, F.C., 1952) though being followed
internationally for designing of industrial
grinding mill circuits, is lengthy, labour-
intensive and time-consuming. In order to
ameliorate the above limitations, a lot of efforts
have been put in by many researchers all over
the globe by various methods. One of the
popular methods in this exerc ise is
experimental simulation to estimate the
* Correspending Author: N. P. H. Padmanabhan, School of
Minerals Metallurgical and Materials Eng ineering, IIT-
Bhubaneswar, Toshali Plaza, Satya Nagar, Bhubaneswar
75 100 7., Co nta ct No: +9 178 940 819 25, Email:
padmanabhan@iitbbs.ac.in
index can easily be computed. However, these
procedures require minimum experimentation
like one or two cycles of batch grinding tests in
a locked cycle manner using Bond’s method and
carry out simulation to arrive a the steady state
value of grindability of the ore. The simulations
are carried out using various types of grinding
rate equations inc luding Rosin-Rammler
grinding kinetic equation. Efforts have also been
put in to use invariant grinding time for the
experiments rather than varying grinding
times for grinding in each cycle (Kapur and
Rahman, 1971) in the Bond’s procedure. An
attempt has been made in this paper to review
a few of the simulation models that have
appeared in the literature over the years

240

2. Simulaion of Bond’s Work Index
Determination
2.1. Kapur’s algorithm
Based on the literature and grinding data
available, Bond (Bond, 1970) stated that it was
possible to estimate the Bond grindability from
batch grinding tests. He analyzed the Bond’s
test procedure and developed a stage-wise
simulation algorithm for the Bond test. He also
mentioned that the abbreviated Bond test
proposed by him was no intended to supplant
the conventional Bond’s test and that it is
possible applications lie in monitoring day-to-
day variation of the ore-grindability for control
purposes. Nevertheless, it was an attempt to
simulate the grindability estimation using
batch grinding tests and requires consideration.
Kapur (1970) derived an equation for the
grinding time or the revolutions to be given for
the (n+1)th cycle of grinding test as
1
t n 1  [U e  ( 1  r)M n 1 ]
(1)
gn
where tn+1 is the time to be given for the (n+1)th
cycle batch grinding test, gn is the rate of grind-
ing in nth cycle, U e is the total weight of under-
size product for the stipulated 250% circulat-
ing load in the Bond ball mill grinding test at
steady state conditions, r is the fraction of the
original feed retained on the mesh of grind and
Mn+1 is the weight of the feed material to the
(n+1)th cycle. He also gave an expression for the
amount retained on the mesh of grind in the
product of nthcycle as
n
R n    rM k Φ  t i 

k 1  i k   n
(2)
Where (t) is a function of grinding time,
selection and breakage parameters and initial
feed size distribution. The Eq.(2) is solvable,
provided the nature of the function (t) is
known. Kapur developed an expression for
241
MPT-2013
(t) as  (t )  exp( Gt ) where G is the
representative batch ginding parameter. One
estimate of the batch parameter, G was given
as G=G1 and G1 was given as
1  R1 
G1  ln   (3)
t1  r M1 
Another estimate for the G was given by taking
G=G2 and by numerical solution of the equation
R 2  rM1 exp(G1 t 1  G 2 t 2 )  rM 2 exp(G 2 t 2 ) (4)
Kapur developed an empirical equation for the
Bond’s work index as
Wi  2.648 [P]
0.406 0.810
[G2 ]
0.853
[r M1 ]
0.099
[1  r] (5)
Kapur used above Eq.(5) for several different
type of ores, He state that the mean square
relative difference between experimental value
of work index obtained by standard Bond test
and his value computed by using his algorithm
is 7.30%.
2.2. Karra’s modification to Kapur’s algorithm
Karra ( V.K.Karra., 1981) modified Kapur ’s
algorithm and he developed simple
mathematical algorithm for simulation of
Bond’s grindability test by using first two
grinding cycle data. Karra did not use batch
grinding parameter but used an empirical
relation for calculating the amount of product
material for subsequent c yc les whic h is
dependent on feed weight and number of
revolutions for that particular cycle, i.e.
Z n  K1Fn N n (6)
R n  K 2fn N n
where, Zn is the amount of product from fresh
(7)
feed for nth cycle, Fn is the amount of fresh feed
for nth cycle, Rn, is the amount of product from
recycle for nth cycle, fn is the amount of recycle
for n th c yc le. K 1& K 2 are c on stant of
proportionality. N n is total number of mill
revolutions for nth cycle. Karra developed his

algorithm based on consideration of the fact
that the recycle product in the Bond’s test
should be coarser than fresh feed added so that
its grinding rate will be slower therefore from
Eq. 6 and Eq.7 constant K1>K2.
Karra did not consider the batch grindability
and he used a different empirical equation to
compute work index which uses directly the
bond grindability. Karra gave an equation for
the Bond’s Work Index as
0.308 0.696
Wi  9.934 (Pi ) (G i )
Where Gi is Bond grindability, Pi is 80% passing
size of the product and F is 80% passing size of
the feed. Karra used above empirical Eq.8. for
several ores and concluded that the mean
square relative differenc e between
experimental value of work index obtained by
standard Bond test and the value computed
by using his algorithm is only 4.41 % which is
better than Kapur ’s algorithm.
2.3. Magdalinovic’s model
Magdalinovic (Magdalinovic., 1989 )derived a
simple procedure for determination of Bond’s
work index using first two grinding cycle data.
Magdalinovic developed his simulation based
on first order Grinding kinetics equation rather
than the empirical relation used in Karra’s
algorithm.
Ac cording to 1 st order Grinding kinetics
equation
R(x,t)=R(x,0) e-kt (9)
Where R(x,t) is test sieve over size material for
sieve size x at time t ; R(x,0) is oversize material
of size x in the feed; k is grinding rate constant
& t is grinding time. Grinding rate constant (k)
is calculated based on first cycle data and based
on this calculation he calculated total number
of mill revolution (Nc) which give steady state
condition with 250% re-circulating load.
ln(1  0.4r0 )
Nc  n
k better than his earlier simulation
MPT-2013
Where, n no of mill revolution per minute & r0 is
Fraction of test sieve over-size in the fresh feed.
Thus, the number of grinding cycle in standard
bond test has been reduced to two cycle.
Magdalinovic used above simulation for several
different type and size of ores, he state that the
mean square relative difference between
experimental value of work index obtained by
standard Bond test and his value computed by
0.125 using algorithm is 4.92 %. Suc h that
(F) (8)
Magdalinovic 1st order grinding kinetics model
gives reasonably good simulation result in
comparison with Kapur’s and Karra’s models.
2.4. Alternative model of Magdalinovic
Magdalinovic (Magdaliestnovic 2003) gave
another simulation based on same first order
grinding kinetics equation used earlier, but used
initial three grinding cycles instead of just two.
R(x,t)=R(x,0) e-kt (11)
Where, grinding rate constant (k1) is determined
in the first cycle from the standard Bond’s test
procedure is
ln rM1  ln R 1
k1  (12)
t
From above equation for calculating grinding
rate constant (k1) for first cycle he considered
amount of oversize material R(x,0) as equal to rM1.
i.e. it is dependent on amount of fresh feed
material of first cycle since the recycle material
for the 1st cycle is zero. The rate constant for the
first cycle k1 was found to be always slightly
greater than k 2. He recommended another
additional cycle also, which confirmed stability
of the recycle load as 250%. He used above
simulation for several different type of ores and
found that the mean square relative difference
between experimental value of work index
obtained by standard Bond test and the value
obtained by his algorithm is 2.58 % which was
(10)
242
 MPT-2013

3. Results and Discussion their encouragement. Thanks are also due to

Dr. PSR Reddy, Head, Mineral Processing
Batch grinding experiments were carried to try Division and Dr. S.K. Angadi both of Institute of
the four simulation models for the purpose of Minerals and Materials Tec hnology,
analysis. Four different ore samples were tested Bhubaneswar for their unhesitating help for the
upon and grinding tests were carried out for experimental work.
the purpose of simulation using all the four
models and the results are shown in Table 1. By
References
comparing the values of the work index
obtained by means of standard bond test and Bond, F.C., Maxson, W.L., 1943. Standard
simulated algorithm it is observed that the grindability tests and calculations, Trans.
relative percentage error of each simulation A. Instn. Min. Engrs., v-153, 362-72.
does not exceed than their mentioned all of Bond, F.C., 1949. Standard grindabiliy tests
above results. tabulated, Tans. Am. Instn. Min. Engrs., v-
Table 1: Comparative value of work indices 183, 312-329.
obtained by Bond’s procedure and Simulation Bond, F.C., 1952. The third theory of
comminution, Trans. Am. Instn. Min.
Mesh of Work Index %
Engrs., v-193, 484-494.
Material grind,
Based on Bond’s procedure
Based on simulation Relative Kapur, P.C., 1970. Analysis of the Bond
µm algorithm error
Uranium ore 1 100 10.91 11.95 (Kapur, 1970) 9.53 grindability test . rans. Inst, of Mining and
Uranium ore 2 100 10.33 10.85 (Karra 1981) 5.03 Metallurgy, 79, 103-108.
Manganese 150 14.80
15.38 (Magdalinovic,1989)
3.91 Kapur, P.C., Rahman, M., 1971. Trans. Inst. of
ore 1
Manganese 90 20.86
21.51 (Magdalinovic,2003)
3.11 Mining and Metallurgy, 80, c-74.
ore 2
Karra, V.K., 1981. Simulation of the Bond
Grindability test. CIM Bulletin , 74-19.
Acknowledgement
Magdalinovic, N., 1989. A Procedure for Rapid
The Authors would express their thanks to the determination of the Bond Work Index.
Director, IIT Bhubaneswar and Prof. Sujit Roy, Int.J.Mineral Processing, 27, 125-132
Head of School. School of Minerals, Metallurgical Magdalinovic, N., 2003. Abbreviated test for
and Materials Engineering, IIT Bhubaneswar for quick determination of Bond’s Work index.
J.Min.and Metall. 39, 1-4

*******

243
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Grinding and Classification Circuit Optimization with Modeling

and Simulation Studies at H.Z.L’s S.K. Mines

T. S. Anil Kumar Nistala, Ajit Swain and K. D. Sharma*

Central Research and Development Laboratory, Hindustan Zinc Ltd, Udaipur 313024,
Rajasthan, India.
Abstract
Size reduction operation in a mineral beneficiation circuit is an extremely energy inefficient. The
process of developing a model for the circuit and simulating it regularly will be a Hawkeye on the
external parameters effecting circuit’s performance and it will be useful in predicting the optimum
operating conditions of the circuit and therefore retrofitting the circuit.
A grinding and classification model was developed using JKSimMet (Version 5.2) and used to
simulate at two different throughputs to the grinding circuit. The objectives are development of
model, Validation of model and finally circuit simulation for estimation of the circuit’s performance
at increased throughput to the circuit.
This paper engages thoroughly in the development and validation of the grinding circuit’s model,
grinding circuit’s simulation and its outcome.

Keywords: Modeling; simulation; grinding; classification

1. Introduction industry. The optimization of the beneficiation

Optimizing the grinding circuit the advantages
will be decreased unit operation costs, increased
c apac ity and improved performanc e of
downstream processes due to improved feed
size distribution. In most plants, optimization
criteria are defined based on the following
purposes, a) Capacity improvement while
maintaining current final product specification,
b) Finer final product size while maintaining
current capacity and c) Minimizing operation
costs while maintaining both current capacity
and product size.
Nowadays, process modeling and simulation
is one of the main optimization tools used in
* Correspending Author: Dr. K. D. Sharma, Head-C.R.D.L,
Central R&D Laboratory, Hindustan Zinc Ltd, Udaipur
313024, Rajasthan, India. E-mail: kd.sharma@vedanta.co.in
plant using simulation consists of several stages,
a) characterize operation parameters of feed in
laboratory tests, b) estimate mac hine
parameters, using plant survey (model
calibration), c) performing simulations to
explore possible optimization solutions by
c hanging c irc uit flow sheet or proc ess
equipment or operating conditions, and d)
evaluation of solutions found through
simulation studies by running plant tests under
proposed flow sheet modifications or operating
conditions (Napier-Munn et al.1996).
Sindesar Khurd Mine is located near Dariba
village in Rajsamand district of Rajasthan,
India. The mine is a lead - zinc mine which
contains sulphides of lead, zinc, and iron. The
sulphide mineral of iron in the run of mine is

244
 MPT-2013

pyrite. This is the major gangue mineral in the stopped and a sample was taken by removing
ore. The optimum P80 maintained is 80% material over a two-meter length. Operating
passing 63microns. conditions during sampling was recorded. Steps
The ROM is initially crushed and the product involved in the present study are:
is sent to a grinding circuit which consists of a 1. Sampling through the circuit survey,
combination of rod mill operating in open 2. Sizing analysis of the samples
circuit and a ball mill operating in a closed 3. Mass Balance.
circuit milling processes. The combined mill 4. Model Development
discharges were sent to the hydro cyclone 5. Model Validation
classification whose over flow is a feed to the 6. Simulation studies.
downstream differential froth flotation process. The sampling was done at the six points of the
In this scenario, grinding optimization studies circuit. The sampling points are
were done with the objective of increasing the 1. Rod Mill Feed (P80:20mm)
throughput to the rod mill of grinding circuit 2. Rod Mill Discharge (P80:1mm)
under the same current capacity. Process 3. Cyclone Feed
modeling and simulation approach was used 4. Cyclone Underflow
to find optimization solutions considering the 5. Cyclone Overflow
requirements of downstream Flotation process. 6. Ball Mill discharge
The aim of the study was to develop 3. Mass Balance Studies
mathematical models of rod mills, ball mills and
classifiers used in the grinding circuit and to The samples thus collected were dried for the
investigate the effec ts of the proposed pulp density calculations. Thus obtained
modifications on the circuit performance using samples were wet sieved for the size analysis
simulation. of samples. The sizing data and the pulp density
data were used in the mass balance studies on
2. Sampling Campaign of the Circuit the circuit with the JK SimMet 5.1 software.
Sampling campaign from grinding circuit was Mass balancing includes reconciliation of
planned to assess its performance under the survey data to minimize sampling & sizing
current operating conditions. errors; also provides missing stream data.
Table 1: Mass balance Studies results
Liqui Pulp Vol. 80%
Solid %
d SG Flow passes
Equipment Port s (t/h) Solids
(t/h) (t/m³) (m³/h) (mm)

Bal Bal Bal Bal Bal Bal

Combin
Feeder 142 1.46 98.98 2.845 50.43 17.9
er

Rod Mill Combin

142 32.49 81.38 2.142 81.45 17.9
er

Prod 142 32.49 81.38 2.142 81.45 0.936

Combin
345.6 119.8 74.26 1.947 239 0.363
Ball Mill er

Prod 345.6 119.8 74.26 1.947 239 0.121

Combin
487.6 302.3 61.73 1.679 470.4 0.206
er
Figure 1: Flow sheet of the mineral grinding Hydro-cyclone
U/F 345.6 119.8 74.26 1.947 239 0.363

and classification circuit of S. K. Mines O/F 142 182.5 43.76 1.402 231.5 0.0607

Samples collected over a period of 3hrs a cut at cyclone feed

Combin
er
487.6 302.3 61.73 1.679 470.4 0.206
sump
every half an hour. The samples collected were Prod 487.6 302.3 61.73 1.679 470.4 0.206

then dried for the % solids calculations. To *Estimated SSQ: 12.5 (lower the value indicates better
the data quality)
sample Rod mill fresh feed, belt conveyor was

245
 MPT-2013

Thus the obtained reconciled data was used in the
development of the models for the individual equipments
in the grinding & classification circuit. The specifications
& details of the equipments that were used in the
development of the models are as follows.
Table 2: The details of the equipments that were used in
the development of the models
Rod mill Ball mill
4.3. Model validation
The obtained fitted model parameters thus
make the model development of the individual
equipments. The developed models are to be
validated with another set of the process data
for getting acquainted with the precision of
prediction of the developed models. Validation
Hydro cyclone

Internal Diame Cyclone - Dc 0.55

involves comparing process response after a
Internal Diameter (m) 3.2 4.4
diameter (m) ter (m) 2
step-change in any process variable with the
Fraction
Internal Length (m) 4.8 Critical
Speed
0.74 Inlet - Di (m)
0.11
1 model response after simulation for the same
Fraction Critical Speed
0.6 Load
0.4
Vortex - Do
0.15
step-change in the same process variable. For
5 Fraction (m)

Ore Work
this purpose, a circuit survey campaign was
Spigot - Du
Load Fraction 0.3 Index
(kWh/t)
9.5
(m)
0.09
conducted on the same grinding & classification
Ore Work Index (kWh/t) 9.5
Original Mill
Ball Top Size 40
Cylinder Length - Lc (m)
0.59 circuit whose throughput was step increased
4
(mm)
to 150 tph from 140 tph. The corresponding
Cone Angle - Theta (deg) 10
Feed 90% Passing Size
(mm)
20
No of cyclones
water addition to the circuit was also increased
4
to maintain the desired pulp density of the
slurry at the respec tive points. Proc ess
4. Model Development variables subjec ted to step-c hange for
The empirical models that were used in the validation are as follows.
development of the individual quipments of Table 4: Process variables subjected to step-
this case study were as follows. change for validation
1. Rod Mill (Lynch – Kavetsky Model) Process variable Model
Development
Model Validation

2. Ball Mill (perfect mixed ball mill model) Circuit Feed rate (TPH)

Water Rod Mil

140

32
150

38

3. Hydro Cyclone (Nageswararao fine Addition

Ball
Mill
140 148

cyclones)
Thus using the software, the models (model The process data after getting reconciled
(through mass balance studies) was used for
parameters) were developed by fitting the
the validation. The validation is, using the
reconciled data obtained from the mass balance developed model for simulating the equipment
studies. to get its virtual response for the given step
Table 3: The fitted model parameters which change in the process variable. The models were
were used in the development of the models validated at the given step change in the process
Model Guessed Fitted Fit
variable. The validation results at increased
Equipment
Parameter Value Value SD
throughput were as follows.
Mill Const 1500 983.1 34.52

SL 1.8 1.821 0.833

Rod Mill Vol. Flow 80% passes
Solids (t/h) Liquid (t/h) % Solid s
IN -6.2 -6.123 2.986 (m³/h) (mm)
Equipment Port
XC 3.5 3.574 0 Si Si Si Si
Bal. Bal. Bal. Bal. Sim. Bal.
m. m. m. m.
ln R/D1 2.453 2.02 0.126 Combine 79.7 79.7 89.8 19.3 19.2
150 150 38.1 38 89.72
r 4 9 3 3 8
Ball Mill ln R/D2 5.193 5.115 0.102 Rod Mill
79.7 79.7 89.8 1.41 1.43
Product 150 150 38.1 38 89.72
ln R/D3 6.306 5.77 0.657 4 9 3 8 3

Cyclone 567. 319. 63.9 62.3 515. 0.34 0.33

KQ0 548.6 523.2 36.08 sump
Product
2
514
9
310
4 8 5
487.2
9 6

KD0 2.57E-05 2.30E-05 0 Combine 417. 131. 275. 0.55 0.59

364 122 76 74.9 247.5
r 2 8 6 3 8
0.046 Ball Mill
Hydrocyclo 417. 131. 275. 0.17 0.14
Eff @ 0.33 0.9 0.979 2 Product 364 122 76 74.9 247.5
ne 2 8 6 3 4

0.013 Combine 567. 319. 63.9 62.3 515. 0.34 0.33

514 310 487.2
Eff @ 0.66 0.8 0.72 8 r 2 9 4 8 5 9 6

Hydro 417. 131. 275. 0.55 0.59

Cal WS 59.62 59.62 1.523 U/F 364 122 76 74.9 247.5
cyclone 2 8 6 3 8
Liquid 188. 44.3 44.3 239. 0.06 0.06
O/F 150 150 188 239.7
Feeder Exp Liq 31.88 31.88 1.876 1 6 8 8 41 42

246
 MPT-2013

Table 5: The comparison of the results obtained result in serious problems in the recoveries of
after the simulation studies (model validation) the metals. In order to maintain the same cut
with the results obtained with the data size of the hydro cyclone and increasing the
reconciliation (mass balance studies) recirculation load, the only way is to increase
the throughput and by maintaining same pulp
density of the slurry (feed to cyclone). So, in order
to see its feasibility the circuit was simulated
at increased throughput i.e. @ 160 TPH to the
rod mill with appropriate increase in the water
addition to the circuit. The results are tabulated
below.
Table 6: The results obtained after the
Figure 2: Size analysis comparison of the simulation studies at increased throughput to
various points in both the data reconciled case the grinding circuit @ 160 TPH.
and the simulated case
From the above results it is quite evident that Sol
ids Liqui
%
Pulp Vol.
%Pass
es 80 %
Equipment Port d SG Flow
Solids 1.00 passes
the response of the models for a given step (t/h
)
(t/h) (t/m³) (m³/h)
mm

change in the process variable is very close with Rod Mill

Combine
r
160 38 80.81 2.125 93.17 14.58 19.28

the actual response of the circuit. The hydro Prod 160 38 80.81 2.125 93.17 70.4 1.5

First stage
Prod 537 308.8 63.49 1.712 494 90.03 0.362
cyclone over flow which is nothing but the feed sump

Combine
377 120.8 75.73 1.985 250.9 85.8 0.657
to flotation was very same in both the cases Ball Mill r

Prod 377 120.8 75.73 1.985 250.9 98.3 0.15

with neglisable difference. The recirculation Combine
537 308.8 63.49 1.712 494 90.03 0.362
r
load is also healthy in both the cases with slight Hydro cyclone
U/F 377 120.8 75.73 1.985 250.9 85.8 0.657

difference between the two cases. Also the O/F 160 188 45.98 1.431 243.2 99.95 0.0671

product sizes of the rod mill in both the cases

are found to be very identical. The difference
was found in the ball mill product, which is
not significantly varied.
Thus the developed models were successfully
validated. So, they c an be used for the
simulation studies. Though they must be
validated at regular time intervals using the
data obtained from the mass balance studies,
obtained from the circuit survey data.
5. Simulation studies on the grinding circuit @
increased throughput
But the scope of increasing the recirculation
load (which is ~240%) was seen in the validation
studies. As the cyclone over flow size must be
the same as the finer cut size of the cyclone may
6. Conclusions
The conclusions that were drawn from the
results of the simulation studies are as follows.
 Grinding Circuit Output which is feed to
Flotation size is not disturbed i.e. the size
which was required is maintained.
 The recirculation load on ball mill got
increased from 364 TPH to 377 TPH with
neglisable change in the product size which
is P80:150 Microns.
 The reduction ratio of the rod mill was
almost remained constant (13.43 @ 145 TPH
& 12.83 @ 160 TPH) with a very slight
decrease.
 The % water reporting to the underflow in
the increased throughput case was 39.1%
and at 145 TPH it was 41.2%. This indicates
betterment in the cyclone performance.

247

Through reducing the fines recycling to the
ball mill, which is an unnecessary load on
the ball mill causing increment in COP and
recovery losses.
Thus The Grinding Circuit is able to handle
increased throughput. However aspects like
pumping capacities / limitations, electric drive
capacities of the mills need to be verified.
Acknowledgment
*******
248
MPT-2013
The authors would like to thank Hindustan Zinc
Limited – S. K. Mines proc essing plant
administration for supporting this research
and sincere cooperation of plant personnel for
making this happen.
References
Napier–Munn, T. J., Morrell, S., Morrison, R. D.
and Kojovic, T., 1996, “Mineral Comminution
Circuits”, JKMRC, Australia, pp. 318-320, 332.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

A Fixed-Grid Model of Solidification of Semitransparent

Materials

S. P. Kar and P. Rath

School of Mechanical Sciences, Indian Institute of Technology Bhubaneswar, Odisha,
751 013, India

Abstract
This article presents a mathematical model for solidification of two-dimensional semitransparent
material. The medium is considered absorbing, emitting and scattering. The radiation field is
obtained by solving the equation of transfer. The temperature field is predicted by solving the
energy equation with a volumetric radiation source. The finite volume method is adopted to
discretize both the equations: the equation of transfer and the energy equation. The enthalpy
formulation is used to capture the continuously evolving solid-liquid interface during phase
change. The thermo physical properties are taken different for different phases. The results are
validated with those available in the literature. The effect of important parameters such as the
scattering albedo and the conduction-radiation parameter on the liquid fractions and the
temperature distributions in the medium are studied. It is observed that with lower value of the
scattering albedo and lower value of conduction-radiation parameter, the solidified region is
more. It is also found that the mushy-zone thickness becomes less with radiation dominated
phase change process.

Keywords: semitransparent, finite volume method, enthalpy formulation, volumetric radiation

1. Introduction
Phase change process of semitransparent
materials finds wide applications in industry
that includes crystal growth (Voller, 2008), laser
material processing (Sarkar et al., 2002) etc. Due
to the complex mechanism of heat transfer
process involved in the evolution of the phase
front, numerical modeling of such process
becomes a challenging task. Nonlinear effect of
the thermal radiation on the prediction of the
* Correspending Author: : P. Rath, Asst. Professor, School
of Mechanical Sciences, Indian Institute of Technology
Bhubaneswar, Odisha, 751 013, India
temperature field further make the process more
complicated. So, an appropriate numerical
model is essential to get an insight into such a
complex phenomena.
All these above applications involving the
phase change process are analyzed by solving
coupled conduction-radiation energy equation
using different methods such as finite difference
method (FDM), finite element method (FEM),
finite volume method (FVM). The radiation
information is obtained by solving the
radiation transfer equation using different
methods such as the Monte Carlo method (MC)
(Guo et al., 2000), the discrete ordinates method
(DOM) (Guo and Kumar, 2001), P1
approximation

249

method (Mitra et al., 1997), the integral equation
solution (Tan and Hsu, 2001), the finite volume
method (FVM) (Chai et al., 1994), the radiation
element method (REM) (Guo et al., 2001) and
the lattice Boltzmann method (LBM) (Mishra
and Roy, 2007).
Chan et al., (1983) suggested a model of melting
and solidification of semitransparent material
involving internal thermal radiation. They
concluded that radiative heating or cooling
causes internal melting and solidification. They
presented an exact and two approximate
solutions to three simple solidific ation
problems and discussed the effect of the two-
phase zone on the solidification of semi-
transparent materials. Lapka and Furmanski,
(2008) proposed a numeric al model of
solidification of a semitransparent material and
discussed the effect of different parameters such
as conduction-radiation parameter, scattering
albedo, optical thickness on the temperature
distribution in the medium. They investigated
different cases taking different relationships
between liquid fraction and temperature
during the solidification processes. Yi et al.,
(2011) analyzed a numeric al model of
solidification of semitransparent material
having graded index. They used Galerkin finite
element method to solve the energy equation of
coupled conduction-radiation phase change
process. They concluded that refractive index
gradient can speed up the phase change process.
Maroufi and Aghanajafi, (2013) analyzed the
solidification of semitransparent material using
the LBM. They discussed the temperature
distribution inside the medium taking into
account the volumetric radiation.
Recently, Mishra et al., (2008) has analyzed the
solidification of a 2-D semitransparent material
using the LBM method. Raj et al., (2006) and
Parida et al., (2007) investigated the 1-D
solidification of semitransparent material using
the LBM method. They c onsidered the
volumetric radiation which was found to have
250
MPT-2013
signific ant effec t on the predic tion of
temperature distribution and liquid fraction in
the medium. They used the FVM method to
obtain the radiative information. Most of the
authors have used two different methods to
solve the energy equation and radiative
transfer equation. So, the present paper focuses
on solving both the energy equation and the
radiative transfer equation using one method
i.e. FVM to perform a parametric study for two-
dimensional transient solidific ation of
semitransparent binary materials.
This article is divided into five sections. In the
next section, the physical problem is defined
followed by formulation of the phase change
process. The overall solution procedure is
discussed next. The results of the chosen
problem are discussed in the results and
discussion section followed by conclusion.
2. Physical Model
500 K
1000 K 1000 K
Y
y
x
1000 K
X
Fig. 1: Schematic and Computational domain
A two-dimensional cavity, with a height and
width equal to unity filled with solid
semitransparent material is considered (Fig. 1).
The medium is assumed to be absorbing,
emitting and scattering. Initially the material
is at temperature T 0 which is more than its
liquidus temperature, TL. At time t > 0, the north
boundary is maintained at a temperature
below the solidus temperature, TS. All other
boundaries are maintained at the initial
temperature. So, solidification starts from the
 MPT-2013

north boundary and the solid-liquid interface The radiation information can be obtained by
is captured by enthalpy based approach (Voller solving the radiative transfer equation given
et al., 1988). The enthalpy based energy equation as
taking into consideration the volumetric l M
radiation can be written as 1 I  l ll l
  I  1    I b  I 
l
 (7)
  s 4 l  l
Energy Equation
   T    T  3. Formulation
  H     q    qr   k    k     qr (1)
t
c
x  x  y  y  3.1. Radiative transfer equation
  The inscattering term in Eq. (7) is summed over
H    g S
H S  gL H L  all the control angles used to discretize the
t t
domain under construction. For the present
 case, an isotropic scattering is considered for

t
g C S PS
T  g L  C PLT  L f  which the phase function  l’l = 1. Under this
assumption Eq. (7), the linearized RTE can be
 g L written as
 C pmix
T    Lf (2)
t t l
1 I l l l
  qr    4 I b  G   m I  Sm (8)
  s
 1    4 T  G  4
 (3a)
where,  lm and Slm are the modified extinction
ˆ )d  coefficient and the modified source term
where G( r ,t )   I( r ,s,t (3b)
respectively which can be represented as
4

  
T 4 l
m   1  
l
 (9a)
and I b  (3c)  4 

The energy equation (Eq. (1)) can be written in  M
l l
Sm  1    I b 
l
dimensionless spatial coordinates as
4
 I  (9b)
l 1
l  l
C pmix
T
 2
 k T   1   k T 
1 
  mix   2   mix  
t X x  x  Y y  y  Integrating Eq. (8) over a typical 2-D control
g L volume and a control angle within a specified
 1   4T 4  G  Lf   t
(4) time step, the RTE becomes
where, x*= x/X, y* = y/Y 1 I
l

     
l l l
Initial Condition  
  V t s
dvd  m
I  Sm dvd (10)
 V t
 
T(x , y , 0)  T0 (5)
Applying divergence theorem to the 2nd term of
Boundary Conditions Eq. (10), assuming the magnitude of intensity

T(x , 0, t)  T0 (6) to be constant over the control volume and a
control angle, Eq. (10) can be written as

T(0, y , t)  T0 n
1 l
i
ˆ ˆ  d   
 I A   s.n i
l l
m P
l
I  Sm V (11)
l
 l

T(X, y , t)  T0  i 1 

* On further simplification, for a control volume

T(x , Y, t)  TN  TS and a control angle, Eq. (11) becomes
251
 MPT-2013

3.2. Liquid fraction update procedure

1 1

I l
e
l

 I w A x Dcx 
l


I l
n
l

 I s A y D cy
l
(12) In the present method, an iterarive update
procedure is developed to update the liquid
 l
 m ,P I P  Sm ,P
l l
 V
l
fraction in each control volume. The iterative
update relation is given as
where D cxe    sˆ  nˆ x  d   D cxw
l l l
a p t
g Ln 1  g Ln  
L f V P
T p
n

 g Ln T L  T s   T s  (16)
  sˆ  nˆ  d
l l l
D cyn  y
  D cys
To avoid overshooting and undershooting
l
   d , A x
 A y problem during computation, following
  conditions are set.
To relate the boundary intensities to the nodal
(a) If g L < 0, then g L is set to zero.
intensities, the STEP spatial difference scheme
(b) If g L > 1, then g L is set to 1.
(Chai et al., 1994) is used. In the step or upwind
A control volume can be said to solidify
scheme the downstream boundary intensities
completely when, g L = 0. Thus it can implicitly
are set equal to the upstream nodal intensities
capture the solid-liquid front in the domain at
as follows.
any time instant. The tolerance limit for
convergence of the iterative solution is set to
I1e  I1p , I1w  I1W , I1n  I1p , I1s  I1S (13)
10-7 in the present simulation.
Applying the STEP scheme, Eq. (12) becomes. 3.3. Overall solution procedure
l
 Ax D l
Ay D cy
 Ax D I l l
The Overall solution procedure for the present

cx
   ml , P Vl  I Pl  cx W

     problem can be summarized below.

l l
Ay Dcy I S (14) (i) Discretize the domain.
  S ml , P V l
 (ii) Set the initial temperature in the domain
So, the final discretization equation for the nodal as T0.
intensities for D  0 and D  0 conditions can
l
cx
l
cy
(iii) Set the initial intensity field to be zero and
be written as the liquid fraction () to be unity.
(iv) A time step loop is started. Advance the
a Pl I Pl  aWl I Wl  a Sl I Sl  b l (15) time step to.
where, the coefficients are given as (v) The RTE (Eq. 7) is solved using the guess
source term based on the guess temperature
A y Dcyl Ax Dcxl
a Sl  l
, aw  field to get the intensity distribution in all
  the directions and at all locations inside
the medium.

a P   A x D cxl   A y D cyl   mP
l
 V  l  (vi) is found from the intensity field using Eq. 3
l
b  S mP  V  l
as discussed in the formulation section.
Once the intensity field is known,   q r can be (vii) The temperature field is solved from the
obtained from Eq. 3. Then the temperature is energy equation (4).
calculated from the energy equation (4) and the (viii) Update the in the current iteration using
liquid fraction of each control volume is the liquid fraction update Eq.(16)
(ix) The convergence for IP , TP and are checked
updated according to the following fraction
using the tolerance limit between two
update procedure.
consecutive iterations.

252
 MPT-2013

· If the solution converges, steps (iv) – (viii) 1

are repeated till the desired time step is 0.9

Temperature (K)
reached. 0.8

· If the solution does not converge, steps (v) 0.7

21 X 21
– (viii) are repeated. 0.6 11 X 11
31 X 31
0.5
4. Results and Discussions 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Distance, y/Y

In order to check the grid independence of the 1

numerical results, a grid refinement test is done 0.9

using various control angles and control

Temperature (K)
0.8
volume sizes. Fig. 2a shows the effect of control
0.7
volume size and Figure 2b shows the effect of 6x3
0.6 8x4
control angle size on temperature distribution 12 x 6
0.5
at the centre line at t = 5 secs. It is found that the 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Distance, y/Y
control angle size of 8 ´ 4 (8 divisions of
azimuthal angle and 4 divisions of polar angle) Fig. 2: Grid independence test: (a) effect of
and control volume size of 21 ´ 21 gives the grid control angle size and (b) effect of control
independent results. Although not shown, it is volume size on centerline temperature
distribution
found that beyond a time step size Dt = 0.001,
there is no change in the results. Hence, the 1

above grid (angular and spatial) and time step 0.9

size are chosen for further presentation of

Temperature

0.8

results. The material properties are taken as 0.7

given in the Table 1. Present

0.6
Table 1: Material Properties used in the Mishra et al. (2008)
Parameter Value Unit 0.5
simulation 0 0.2 0.4 0.6 0.8 1

ks 2.268 W/m-K Distance, y/Y

1.72368 W/m-K
k mz Fig. 3: Validation with available results at t =
kL 1.3608 W/m-K 5 secs
1.0 J/Kg-K
Fig. 3 shows the temperature distribution at
C ps the centerline (x/X = 0.5) of the medium at t = 5
C mz 1.12 J/Kg-K secs. It is observed that the present results agree
1.2 J/Kg-K well with the available result from the
C pL
literature.
s = L 1000 Kg/m3
1

Lf 1000 J/kg
0.9

600 K
TS
Temperature

0.8

800 K 0.7
TL N = 0.01
0.6 N = 0.1
2793 K
Tb N=1
0.5
To 300 K 0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Distance (y/Y)
 5.67  10-8 Wm?2 K-4
Fig. 4a :Centre line temperature distribution
(T/Tref) at t = 5secs for different conduction-
radiation parameters

253
 MPT-2013

line for different values of scattering albedo at t

1.2 = 5 secs. It is found that as the value of scattering
1
albedo increases, the thickness of mushy zone
increases. This is because, the medium scatters
Liquid fraction

0.8

0.6
more energy as the value of the scattering albedo
0.4
N = 0.01 increases and the effect of radiation on the phase
0.2 N = 0.1
N=1 change process decreases.
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Distance, y/Y

Fig. 4b: Centre line liquid fraction distribution

at t = 5secs for different conduction-radiation
parameters
Fig. 4a shows the temperature distribution
along the centre line for different conduction-
radiation parameters at t = 5secs. It is observed
that for radiation dominated phase change
process i. e. N = 0.01, the thickness of mushy
zone decreases. The temperature gradient is
more in the mushy zone region. Fig. 4b shows
the variation of liquid fraction in the center line Fig. 6a: Temperature contour at t = 5 secs
with the different c onduc tion-radiation
parameters at time, t = 5 secs. Near to the cold
boundary, the solidified region is more in the
conduction dominated phase change process (N
= 0.1) where as it is found less in the radiation
dominated phase change process (N = 0.01).
1

0.9
Temperature

0.8

? = 0.0
0.7 ? = 0.4
? = 0.8
0.6

0.5
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
Distance, y/Y

Fig. 5a: Centre line temperature distribution at

t = 5secs for different scattering-albedos Fig. 6b: Liquid fraction contour at t = 5 secs
1.2
Fig. 6a and 6b show the temperature
1
distribution and liquid fraction distribution in
Liquid fraction

0.8

0.6
the medium at t= 5sec s. It is seen that
0.4
? = 0.0
? = 0.4
solidification starts from the north boundary.
0.2
? = 0.8
It is found that the temperature gradient
0
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
decreases from the solid-mushy interface to
Distance, y/Y
mushy-liquid interface.
Fig. 5b: Centre line liquid fraction distribution
5. Conclusion
at t = 5secs for different scattering-albedos
Fig. 5a and 5b shows the variation in A numerical model of solidification of 2-D square
temperature and liquid fraction along the center semitransparent medium was discussed. The

254
 MPT-2013

medium was considered to be absorbing,  = under relaxation factor

emitting and scattering. The equation of transfer Superscripts
and energy equation were solved using FVM l = index for the discrete direction
approach. Enthalpy method was employed to * = non-dimensional parameter
capture the evolving solid-liquid interface. The PI = previous iteration value
distribution of liquid fraction and temperature o = value from previous time step
were predicted for different parameters such Subscripts
as scattering albedo, conduction-radiation b = black body
parameter. It was observed that for radiation D = downstream
dominated phase change with lower value of m = modified
conduction-radiation parameter; the thickness mix = mixture
of mushy zone was less. The amount of solidified mz = mushy zone
region is found to be more for lower value of P = node
the scattering albedo and conduction-radiation P* = value from previous iteration
parameter. U = upstream
Nomenclature Abbreviations
RTE = Radiative Transfer Equation
Dcz = direction cosine
FVM = Finite Volume Method
gL = liquid volume fraction
MC = Monte Carlo method
HS = solid enthalpy
DOM = Discrete Ordinate Method
HS = Liquid enthalpy
REM = Radiation Element Method
H = nodal latent heat
I = intensity
References
k = thermal conductivity
n̂ = the unit outward normal vector
Brent, W. D., Voller, V. R. and Reid, K. J., 1988.
qr = radiative heat flux
The enthalpy porosity technique for
s = distance
modeling convection- diffusion phase
t = time
change: Application to the melting of a
TS = solidus temperature
pure metal. Numerical Heat Transfer. 13,
TL = Liquidus temperature
297-318.
V = volume
Chai, J. C., Lee, H. S., and Patankar, S. V., 1994.
x* = dimensionless axial distance
Finite volume method for radiation heat
y* = dimensionless vertical distance
transfer. J. Thermophysics Heat Transfer.
Greek symbols
8, 419-425.
 = scattering albedo
Chan, S. H., Cho, D. H. and Kocamustafaogullari,
 = extinction coefficient G., 1983. Melting and solidification with
 = polar angle internal radiative transfer-a generalized
phase change model. International Journal
 = azimuthal angle
of Heat and MassTransfer. 26, 621-633.
 = solid angle Guo, Z., Kumar, S., and San, K-C., 2000.
 = optical thickness Multidimensional monte carlo simulation
 = scattering phase function of short pulse transport in scattering
s = scattering coefficient media. J. Thermophysics Heat Transfer. 14,
504-511.
255

Guo, Z., and Kumar, S., 2001. Discrete-ordinates
solution of short-pulsed laser transport in
two-dimensional turbid media. A p p l
Optics. 40, 3156-3163.
Guo, Z., Kumar, S., and Maruyama, S., 2001.
Transient radiation element method for
three-dimensional scattering, absorbing
and emitting medium. Num. Heat
Transfer: PART B. 39, 371- 387.
Lapka. P. and Furmanski, P., 2008. Numerical
modelling of solidification processes of
semitransparent materials using the
enthalpy and the finite volume methods.
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of conduction-radiation heat transfer
during phase c hange proc ess of
semitransparent materials using lattice
Boltzmann method. J. Quant. Spectros.
Radiative Transfer. 116, 145-155.
Mishra, S. C., Behera, N. C., Garg, A. K. and
Mishra, A., 2008. Solidification of a 2-D
semitransparent medium using the lattice
Boltzmann method and the finite volume
method. International Journal of Heat and
MassTransfer. 51, 4447- 4460.
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transient conduction-radiation problems
using the lattice Boltzmann method and
the finite volume method. J.
Computational Phys. 233, 89- 107.
Mitra, K, Lai, M. S., and Kumar, S., 1997.
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participating media within a rectangular
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Parida P. R., Raj. R., Prasad A. and Mishra, S. C.,
2007. Solidification of a semitransparent
planar layer subjected to radiative and
convective cooling. J. Quant. Spectros.
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2006. Analysis of solidific ation of a
semitransparent planar layer using the
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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

CFD modelling of column flotation: Predicting two phase flow

hydrodynamics

Balraju Vadlakonda* and Narasimha Mangadoddy

Department of Chemical Engineering, Indian Institute of Technology, Hyderabad,
Ordnance Factory Estate, Andhra Pradesh, India-502205

Abstract
Column flotation (CF) is versatile equipment and is being practiced for significant growth in
mineral processing since many years. The flow in column flotation is multiphase transitional/
evolving turbulent flow. The complex multi-phase flow in these columns is far from complete
understanding. The complete understanding of hydrodynamics of column flotation (CF) is essential
to model and develop design criteria. However, its similarity to the bubble columns provides a
basis for improved understanding of fluid flow in CF using the multi-phase CFD methods. This
paper presents a three-dimensional, two-phase, CFD model for numerical simulation of water-air
dispersive flow in column flotation. Eulerian-Eulerian multi-phase (Two-fluid) model with standard
k-å turbulence model has been employed in these simulations. Simulations had been carried out to
predict the time averaged gas hold-up, liquid velocity and turbulence quantities for various gas
superficial velocities. The CFD model was extensively validated against the literature based rectangular
bubble columns in terms of gas-holdup and liquid velocities. The model was also validated against the
4 inch laboratory circular column flotation gas-holdup data.

Keywords: Eulerian-Eulerian models, Column Flotation, Computational fluid dynamics, Turbulence,

Gas hold-up, Liquid velocity.

1. Introduction
Column flotation has been using enormously
in mineral process industries to separate many
minerals. Due to its better yield performance
compare (Jena et al., 2008) with conventional
flotation cells, it has been attracting academics
and mineral separation process industries.
Performance of Column flotation depends on
bubble-particle interac tions, removal of
particle –bubble aggregates and break-up and
* Correspending Author: Balraju Vadlakonda, Department
of Chemical Engineering, Indian Institute of
Technology, H yderabad, Ordnance Factory Estate,
Andhra Pradesh, India-502205, Ph : +91-40-23026086,
ch10p005@iith.ac.in
coalescence of bubbles, which are mainly
driven by physic-chemical interactions. All
these interac tions well explained by
hydrodynamics of the process. For the study of
hydrodynamics of Column Flotation, Bergh and
Yianatos (1995) built an empirical model. A
number of (Sastry and Lofftus, 1988, Cruz, 1997)
phenomenological models have been developed
for analyse the hydrodynamics of Column
Flotation.
To understand the c omplexity of
hydrodynamics in column flotation, advance
tools such as computational fluid dynamics
(CFD) elucidate clearly. It is very helpful to

257

develop the design criteria (Chakraborty et al.,
2009). Initially two phase flow of
hydrodynamic s had studied in c olumn
flotation. To analyse the hydrodynamics in
column flotation, we considered bubble column
CFD methods as basis.
Many researc hers had c arried out CFD
simulations to analyse the hydrodynamics of
bubble column. Dispersed gas–liquid ûows in
bubble columns had simulated using volume
of fluid (VOF), Eulerian–Eulerian and Eulerian–
Lagrangian approaches. Eulerian–Eulerian
simulations can predict the low-frequency
oscillations of the meandering bubble plume
and time-averaged ûow properties in
reasonably good agreement with experiments
(Buwa and Ranade, 2002, Rampure et al., 2003).
Eulerian–Lagrangian approach could predict
the time-averaged properties (Delnoij et al.,
1999, Lain et al., 2002)
Two phase CFD simulations had carried out
using mixture model previously in column
flotation. In this present work, CFD simulations
had carried out to explain the time averaged
gas hold-up, liquid velocity and turbulence
characteristics of column flotation. The effect of
gas superficial velocities had tested in flow
c haracteristic s of c olumn flotation. CFD
simulations had tested with experimental data
(Shukla et al, 2010).
2. CFD Model
The Eulerian-Eulerian two phase fluid model
had been used in simulations of Column
Flotation. All simulations had carried out with
the help of commercial software FLUENT
version 13.Simulations had carried out based
on finite volume method. Appropriate user
defined func tions had used in FLUENT
software.
Eulerian-Eulerian CFD model was well adopted
in bubble column simulations. Both phases are
treated as interpenetrating fluids. The
258
MPT-2013
collectively averaging the mass and momentum
conservation equations describes the time
dependent motion of both phases. Eulerian two
fluid model is able to accounts the gas-liquid
interactions in the terms of drag, lift, virtual
mass and induced turbulence etc. The CFD
model had validated with literature based
rectangular bubble column (Buwa, 2006).The
resulting set of equations solved by using finite
volume method and applying pressure-velocity
coupling scheme based on SIMPLE algorithm.
In churn turbulent flows Euler-Euler method
usually preferred.
k-  turbulence model had used in most of
bubble column simulations. It is a two equation
model, which include two extra transport
equations to characterize the turbulent flow.
Turbulent kinetic energy (k) decides the energy
in the turbulence and turbulent dissipation (  )
defines the scale of the turbulence.
2.1 Basic model equations
Mass conservation equation
The mass conservation equation for the phase
q can be written as
Where the velocity of phase q and mass
transfer between phases is not considered and
therefore source term ( ) was set to zero.
Momentum conservation equation
The momentum balance for phase q can be
written as

Where is the qth phase stress-strain tensor
Here and are the shear and bulk viscosity
of phase q, is an external body force, is
a lift force, is a virtual mass force, is
an interaction force between phases, is the
interphase velocity and p is the pressure shared
by all phases.
Where, is the interphase momentum ex-
change coefficient. The schiller Naumann drag
law had used in the simulations.
Lift force and virtual mass force didn’t consider
in simulations.
Turbulence equation
Turbulence can be taken into consideration for
both phases. k-å turbulence model has been
used in these simulations. The reference has
taken from ANSYS FLUENT 13.0 theory guide
(Fluent (2010)).
The governing equation for the turbulent kinetic
energy (k) and the turbulent energy dissipation
rate ([) are given below.
The turbulent visc osity c omputed by
In this, represents generation of turbulent
kinetic energy due to the mean veloc ity
259
MPT-2013
gradients. =1.44, =1.92, =0.09,
=1.0, =1.3 are constants.
3. Numerical Simulation
3.1. Geometry and grid considerations
Fig. 1 shows the schematic diagram of column
flotation with dimensions of 1.68m height and
0.1m diameter (Satish et al., 2010). Feed pipe is
located at 1.3m height of column from base. Air
flow comes through sparger from bottom of
column. Air was supplied at a known velocity
(Ug =1.30, 3.29, and 5.01 cm/s). This prepared
feed water was fed to the flotation column at
desired feed velocity 2.76 cm/s.
The two fluid Eulerian-Eulerian model was ap-
plied for the gas-liquid dispersive flow in column
flotation. This basic CFD model was used to simu-
late the dynamic flow behaviour in column flota-
tion. The k-å turbulence model had been used in
these simulations. Turbulence was considered for
both phases. Unstructured computational grid
had used.
Column Flotation has divided into 1, 51,090 cells.
The transient simulations were performed and
the time step 0.001 s was used for column flota-
tion. The velocity–pressure linkage was handled
through the Phase coupled SIMPLE procedure
in column flotation. Mass and momentum equa-
tions were solved using higher-order
discretization schemes, like QUICK. The gas inlet
was taken as a velocity inlet, with a volume frac-
tion one. The average bubble size used is 5 mm.
At the column outlet, a degassing boundary con-
dition was speciûed as described by Ranade
(1997).
4. Results and Discussion
Column flotation simulations had carried in
transient manner. Simulations results were
analysed at three different heights of column
from bottom i.e. 0.42m, 0.84m and 1.26
m.Numerical simulations had carried out with
 MPT-2013
0.1m
4.1. Gas hold-up
Fe e d The effect of air superficial velocity on gas hold-
1.68m up had analysed in Fig 3. The time averaged
gas hold-up values had increased with air
1.3 m superficial velocity. Simulations values had
matched with experimental results (Shukla et
Air
al., 2010).
(a) Ta ilings (b)
Fig. 1: Schematic diagram of Column
Flotation (a) Geometry (b) CFD grid
three air superficial velocities 1.3,3.29,5.01cm/s
and water flow rate 2.76 cm/s. Water had
entered to the column at 1.3m height above the
base. Time averaged flow properties had
analysed through CFD simulations. Simulations
had been carried out to analyse the time averaged
gas hold-up, liquid velocity and turbulence
quantities.
The CFD model had validated with literature
based rectangular bubble column (Buwa, Fig. 3: Effect of air superficial velocity on gas
2006).In rectangular bubble column time hold-up
averaged gas hold-up and time averaged axial 4.2. Liquid velocity
liquid veloc ity had validated with
experimental results. CFD simulations had The liquid velocity has transitional/turbulent
carried out for air superficial velocity 0.14cm/s nature in column flotation.
with 2.25 aspect ratio. The results had shown
in Fig. 2(a) and 2(b).

Fig. 2(a): Time averaged gas hold-up profile

for column with H/W=2.25 at gas superficial
velocity 0.14 m/s

Fig. 2(b): Time averaged axial liquid velocity (a) Velocity vectors of water (b) Velocity vectors
for column with H/W=2.25 at gas superficial of air
velocity 0.14 m/s
260
 MPT-2013

Zone-1 From Figs. 4(a)-(c) it can be observe that liquid

moves upwards at the column centre while
negative velocity at the wall side. Due to velocity
differences in centre and walls, liquid flow
Zone-2 recirculation pattern was observed in column
flotation. Liquid recirculation is the major
reason for mixing in column flotation. Axial air
Zone-3 superficial velocity has always in positive
direction. Liquid velocity had analysed in zone
wise. Zones had created at heights of 0.22m,
Zone-4 0.47m, 0.75m, 0.995m and 1.5m from base of
column.Zone-1 had is region of above the height
Zone-5 of 1.50m,Zone-2 is region between the height of
0.995m to 1.5m, zone-3 had the region between
Zone-6 the height of 0.75m to 0.995m, zone-4 is region
between the height of 0.47m to 0.75m and zone-
(c1) Velocity vectors of water zone wise
5 had the region between the height of 0.22m to
0.47m and zone-6 is below the region of 0.22m
from base of the column. In zone-2 liquid above
the feed pipe had the downward velocity and
below the feed pipe it had upward velocity at
centre of the column. In this zone liquid had
swirling motion near the feed inlet position. In
remaining zones liquid had upward motion in
middle of the column while it had negative
velocity at walls of the column. However more
mixing will takes place below the feed inlet of
the column due to recirculation of liquid.
(i) zone-6 (ii) zone-5 (iii) zone-4 (iv)zone-3 The comparison of time averaged axial liquid
velocity had analysed at three positions from
bottom of the c olumn with 1.3 c m/s air
superficial velocity. It had explained in Fig. 5.
Numerical simulations had carried out with
different air superficial velocities. Liquid
velocity had attained maximum at the centre
of the column. Unfortunately, experimental
data on the time-averaged liquid velocity were
not available. Effect of air superficial velocities
on time averaged axial liquid velocity had
analysed (Fig. 6). Air superficial velocity
(v) zone-2 (vi) zone-1 influences the positive and negative velocity of
(c2)Velocity vectors of water zone wise. the liquid in the column. Both positive and
Fig.4:Velocity vectors of water and air in negative veloc ities will inc rease with air
column flotation superficial velocity. Liquid circulation had been
261
 MPT-2013

caused by increase the air superficial velocity,
and then as a result more mixing will takes
place in column flotation.
kinetic energy and turbulent intensity at
different heights of column. Due to bubble
interactions with liquid at the above of sparger
the turbulent kinetic energy and intensity
gained maximum. Bubble interaction with
liquid and mixing phenomena leads to change
in the values of turbulent kinetic energy and
intensity.

Fig. 5: Time averaged axial liquid velocity at

different heights of column for air superficial
velocity 1.3cm/s

Fig. 7: Turbulent kinetic energy at different

heights of column for air superficial velocity
1.3 cm/s
Fig. 6: Effect of different air superficial veloci-
ties on time averaged axial liquid velocity at
0.42m height of column

4.3. Turbulence parameters

Turbulent kinetic energy, turbulence intensity

and turbulent dissipation rate of column had
analysed through numerical simulations.
Turbulence properties had analysed at different Fig. 8:Effect of different air superficial
heights of column from bottom with using velocities on turbulent kinetic energy at 0.42m
1.3cm/s air superficial velocity. Turbulent height of column
kinetic energy and intensity had reached
maximum value at centre of the column and in
walls had reached minimum values.
Turbulent kinetic energy and turbulent
intensity had increased with air superficial
velocity because of great amount of bubbles
into flow (Broder and Sommerfeld, 2009). Fig. 8
and 10 had explained the effect of air superficial Fig.9: Turbulent intensity at different
velocity on turbulent kinetic energy and heights of column for air superficial velocity
turbulent intensity. The turbulent kinetic 1.3 cm/s
energy and turbulent intensity got maximum
at below the feed inlet of column. Froth zone
had less value of turbulent kinetic energy and
turbulent intensity compare to pulp zone. Fig.
7 and 9 had explained the changes in turbulent
262

Fig.10: Effect of different air superficial
velocities on turbulent intensity at 0.42m height
of column
The turbulent dissipation rate attained
maximum at walls of the column and minimum
at centre of the column (Fig. 11). Bubble break-
up and coalesc ence had increase due to
collisions among the bubbles. So collisions
among the bubbles lead to create smaller eddies
in the bubbly flow. The bubbles radial
fluctuating velocity had been significant and
bubbles moves to towards to the wall. This may
be significant in turbulent dissipation rate. It
had increased with air superficial velocity (Fig.
12).
Fig. 11: Turbulent dissipation rate at different
heights of column for air superficial velocity
1.3 cm/s
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MPT-2013
Fig. 12: Effect of different air superficial
velocities on turbulent dissipation rate at 0.42m
height of column
5. Conclusions
Three-dimensional, two-phase, CFD simulations
had c arried out to analyse the water-air
dispersive flow in column flotation. Eulerian-
Eulerian multi-phase model with k-å turbulence
model had used in simulation. Time averaged gas
hold-up and liquid velocity had analysed in
column flotation. Gas hold-up had increased with
superficial air velocity. Liquid recirculation and
mixing will change with air superficial velocity.
Turbulent kinetic energy, intensity and turbulent
dissipation rate had analysed in column. It had
increased with air superficial velocity.
6. References
AnsysFluentTM 13.0 Theory guide, 2010.
BalrajuVadlakonda, Narasimha, M., 2011. Two
phase CFD simulation of column flotation,
International conference on Mineral
Processing Technology, 2011, Oct 20-22,
Udaypur, India.
Bergh, L. G. and Yianatos, J. B., 1995. Dynamic
Simulation of Operating Variables in
Flotation Columns. Minerals Engineering.
8 (6), 603-613.
Bröder, D., Sommerfeld M. 2009. Analysis of
hydrodynamics and microstructure in a
bubble column byplanar shadow image
velocimetry. Ind, Eng. Chem. 48, 330-340.
Buwa, V.V., Ranade, V.V., 2002. Dynamics of
gas–liquid ûow in a rectangular bubble
column: experiments and single/multi-
group c fd simulations. Chemic al
Engineering Science. 57, 4715–4736.
Cruz, E. B., 1997. A Comprehensive Dynamic
Model of the Column Flotation Unit
Operation. PhDThesis. Department of
Mining and Minerals Engineering, Virginia
Polytechnic Institute and State University.
Chakrabortyet, D., Guha, M., Banerjee, M., 2009.
CFD Simulation on influence of superficial
gas veloc ity, c olumn size, sparger
arrangement, and taper angle on

hydrodynamics of the Column flotation cell.
Chemical Engineering Communications.
196 (9), 1102-1116.
Deng, H., Mehta, R. K., Warren, G. W., 1996.
Nuemerical modelling of flows in flotation
columns. IntJ.Mineral processing. 48, 61-
72.
Delnoij, E., Kuipers, J. A. M., van Swaaij, W. P.
M., 1999. A three-dimensional CFD model
for gas–liquid bubble columns. Chem. Eng.
Sci. 54, 2217-2226.
Lain, S., Broder, D., Sommerfeld, M., Goz, M. F.,
2002. Modelling hydrodynamics and
turbulence in a bubble column using the
Euler–Lagrange proc edure. Int. J.
Multiphase Flow. 28, 1381-1407.
Jena, M. S., Biswal, S. K., Das, S. P., Reddy, P. S. R.,
2008. Comparative study of the
*******
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MPT-2013
performance of conventional and column
flotation when treating coking coal fines.
Fuel Processing Technology. 89, 1409-1415.
Ranade, V. V., 1997. Modelling of turbulence flow
in a bubble column reactor. Chemical
Engineering Research Design. 75, 14–23.
Rampure et.al, 2003. Modelling of gas–liquid/
gas–liquid–solid ûows in bubble column
reactors. Canad.J.Chem. Eng. 81, 692-706.
Sastry, K. V. S., Lofftus, K. D., 1998. Mathematical
Modeling and Computer Simulation of
Column Flotation. Column Flotation ’88,
ed, SME Annual Meeting, Arizona, USA.
57-68.
Shukla, S. C, Kundu, G., Mukherjee, D., 2010.
Study of gas holdup andpressure
characteristics in a column ûotation cell
using coal. Minerals Engineering. 23, 636–
642.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Computational and Experimental Study of the Effect of Inclination

on Hydrocyclone Performance

V.T.S.R. Kumar Reddy, Kedar S. Kumbhar and Narasimha Mangadoddy*

Department of Chemical Engineering, Indian Institute of Technology Hyderabad,
Ordinance Factory Estate, Yeddumailaram, 502205, India

Abstract
In this paper, the effect of inclination on hydrocyclone performance is studied using computational
fluid dynamics technique and experimental methods. Water only experiments and the
corresponding two-phase CFD simulations in 3" and 4" diameter cyclones are carried out at 0, 30,
45, and 60 degrees inclined positions to the vertical plane. The two-phase CFD flow analysis
shows that the water split to underflow decreases as the inclination increases which are consistent
to the experiments. The predicted tangential velocity profiles show mixed behaviour, 45 0
inclinations with high tangential velocity. An increased pressure drop is also observed with the
inclination. The effect of inclination on air-core profiles is minimal. An increase in the inclination
shows an air-core size reduction trend. Experiments at various inclinations on flow split and
classification performance of 3 inch hydrocyclone performed using the silica slurry. The analysis
shows the increased cut-size and the reduced water split with the inclination. Cross validation of
inclined cyclone’s CFD data is attempted with ERT and High speed video imaging experiments.

Keywords: Hydrocyclone, multi-phase CFD, turbulence, particle classification, air-core,

inclination

1. Introduction of contents during shutdown. In the phosphate

Vertical cyclones are common in practice in
most of the comminution circuits. Horizontal
cyclones can be found in extreme cases which
are for installation convenience rather than for
process reasons. Inclined cyclones are also
present for spec ific mineral proc essing
applications. In coal preparation plants, dense
medium c yc lones are operated near to
horizontal inclination of 20 degrees to allow
large spigot sizes for sinks removal, self-drain
* Correspending Author: Narasimha Mangadoddy, Email:
narasimha@iith.ac.in; Fax: +91 40 23016032
removal, dense medium cyclones are inclined
with an angle between 0-90 degrees for better
separation of ore and tailings (Liu Feng et al.,
2006). Even in the clusters, hydrocyclones are
mounted with an inclination around the feed
distributor for uniform distribution of slurry
and under flow collection. It is believed in
mineral processing industry that inclined
cyclones would fetch the benefit in number of
ways while classifying the material by size.
Gravity influences the cyclone performance
through the air core size and position variations
in large cyclones. It also favours the cyclone

265

operation at coarser cut points without varying
any other design and operating parameters.
Minimizing fines misplacement to underflow
can be achieved with inclination.
2. Literature Review
Usage of horizontal cyclones in place of vertical
cyclones increased the efficiency by reducing
short circuit flow of fines to underflow hence
dec reases c irc ulating loads on ball mill
(Hochsheid, 1987, Orwe and Noreen, 1988).
Similar observation was found with 45 degree
inclined cyclones (Johnstone and Rais, 1988).
There was an improvement in the efficiency of
hydrocyclones when they were operated at low
pressures in horizontal direction (Bradley,
1960) due to reduction of water recovery to
underflow. Asomah and Napier-Munn
(Asomah and Napier-Munn, 1997) conducted
experiments on various hydrocyclones with
different inclinations (0-120), diameters (102-
508mm). Their results show inclination of 45
degrees or greater has a significant effect on the
performance of large diameter hydrocyclones
in low pressure operations. Their observations
include the increase of cut size with increase in
inclination. They also developed an empirical
model for hydrocyclones with the inclusion of
feed size, viscosity and inclination. Rong and
Napier-Munn (Rong and Napier-Munn, 2003)
inclination investigations (0-180 degrees) on
200mm JK classifying cyclone reveals, there was
an improvement in sharpness of separation
from vertical to horizontal position; thereafter
it decreases significantly to a low value. Their
inclination results on flow ratio decrement and
improvement of solids percentage in the
underflow were similar to the literature
(Asomah and Napier-Munn, 1996). Inclination
effect on 75mm hydrocyclone has been studied
by Banisi and Deghan (Banisi and Deghan-
Nayeri, 2005). They concluded that there won’t
be considerable change in the performance of
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MPT-2013
hydrocyclone for low solids concentration (10%
wt). Thereafter there was significant increase
in the cut size when cyclone operated beyond
45 degrees inclinations for c oncentrated
slurries. Data was tested with the empirical
model proposed by Asomah and Napier-Munn
and got an error of 6.6% in the predicted cut
size. Either of these studies was not
concentrated on high pressures and high
perc entage of feed solids effec t on the
performance of hydrocyclone.
In this paper, the effect of inclination on
hydrocyclone performance is studied using
computational fluid dynamics technique and
experimental methods. Water only and slurry
based classification experiments and the
corresponding two-phase CFD simulations in
3" and 4" diameter cyclones are carried out at
different inclined positions to the vertical plane.
Inc lination effec t on flow analysis of
hydrocyclone w.r.t. mean and turbulent flow
field, water split, LZVV, air-core size and
position, and particle turbulent dispersion is
attempted. Basic reasons behind the cyclone
inclination effect on particle classification
mechanism have been eluded.
Fig.1:Schematic of test rig used for experiments
3. Methodology
To find out the inc lination effec t on the
performance of hydrocyclone, a test rig with
75 mm and 100 mm c onventional
hydrocyclones was designed and
 MPT-2013

commissioned. Schematic of the test rig and 4. Result and Discussion

conditions used is shown in figure 1.Variables
used in the experiments and their range were
given in table 1. Silica feed, 90% passing through
200 µm is used for testing. At particular feed
concentration hydrocyclone is rotated with an
increment of 150 over the range 0 – 600 from
vertical position. At each inclination the
pressure is varied in the range of 5-25 psi by
regulating bypass valve and inspecting through
pressure gauge. 3 sets of steady state over flow
and under flow samples are collected for 10
seconds and average flow rates are calculated.
Collected samples were dried in an oven and
particle size distribution is measured by
analyzing through Microtrac particle size
analyzer S 3500. Tests are further continued
with variation in spigot diameter also.
Corrected cut size (d50c) using fraction of feed
water to underflow (Rf) is the main criteria for
comparison of hydrocyclone performance.
Experimental data is analyzed for both water
only and silica slurry systems. Using the water
only experiments, the inclination effect on water
split ratio & volumetric flow rate at different
pressures & spigot diameters is also analyzed.
Using silic a slurry based c lassific ation
experiments additional analysis is attempted
to quantify the effec t of inc lination on
hydrocyclone performance indices; water split
ratio (Rf), slurry volumetric flow rate (Q), cut
size (d50) & sharpness of separation (á) operating
under different design and operating
conditions.
(a) (b)

Fig. 3: Variation of volumetric flow rate at

different Pressures for (a) 3" and (b) 4"
hydrocyclone with 12.5mm spigot

a. Water only experiments

(a) (b)
Fig. 2: 3" Hydrocyclone (a) Schematic diagram
(b) Mesh used for simulation (c) 4"
Hydrocyclone
Table 1: Range of variable conditions used to
study the inclination effect
Variable
Inclination (degree)
Pressure (psi)
Concentration (wt % of feed solids)
Vortex finder diameter (mm)
Inlet diameter (mm)
Spigot diameter (mm)
Cyclone diameter (mm)
i. Volumetric Flow rate Vs. Inclination
Using the water only experimental data on 3
inch and 4 inch hydrocyclones, the volumetric
flow rate, Q is calculated by adding the steady
(c) state overflow and underflow rates and
presented in Fig. 3 a&b. Fig. 3 a&b also shows
the inclination effect on volumetric flow rate of
water for different inlet pressures and spigot
diameters. It is observed that an increase in the
inc lination leads to an inc rease in the
volumetric flow rate of water. As expected for
Variation Range every inclination position the volumetric flow
0, 30, 45, 60
5, 10, 15, 20, 25 rate is directly proportional to the pressure.
0, 10, 28.76, 50
ii. Slurry experiments
25 & 38
45 & 52x20 The inclination effect on volumetric flow rate
12.5, 15
75 & 100
of different solid concentrations operating at
constant pressure (10 psi) and spigot diameter
267
 MPT-2013

(12.5 mm) is shown in Figure 4 (a) and (b) for 3

inch hydrocyclone.

(a) (b)

Fig. 6: Variation of Water split ratio (water) with

(a) (b) respect to inclination for 4 inch Hydrocyclone
with (a) 12.5mm (b) 15mm spigot
Fig. 4: Variation of slurry volumetric flow rate It is also observed that at high pressure (25psi)
for 3" Hydrocyclone at (a) different feed the water recovery to underflow is very less
concentrations and (b) different pressures for compare to pressure at (5 psi). At low pressure
50% concentration. (5psi) water rec overy to underflow is
significantly reducing with inclination, but at
At low solids concentrations (as shown in Fig.
high pressure (15, 20 & 25 psi) there is no effect
4 a) the slurry volumetric flow rate is slightly
of inclination on water recovery as observed in
dec reased by inc lination of c yc lone. As
Fig. 5 & 6. The inclination has strong effect on
observed in Fig. 4 a, at high feed solids
centrifugal force, which leads to develop more
concentrations the slurry volumetric flow rate
pressure drop in cyclone. Increasing pressure
slightly increases with the angle of inclination.
drop leads to reduc e water rec overy to
Further the effect of inclination on flow rate for
underflow by increasing upward axial velocity.
50% solid concentration at low inlet pressure
From Fig. 5 b, 6 b, it is observed that increasing
(say 5 psi) is seems more pronounced compared
spigot diameter reduces the pressure drop in
to that of the high inlet pressures (see Fig. 4 b).
cyclone as a result increasing water recovery
b.Water split ratio (Rf) Vs. Inclination (i)
to underflow. From Fig. 5 a, 6 a, it is observed
i. Water only experiments
that for 15 psi water split ratio in 3" cyclone is
The inclination effect on water recovery to
12% while in 4" cyclone for same pressure it is
underflow for different pressures and spigot
15%. It implies that in 4" cyclone pressure drop
diameters is shown in Fig. 5 a & b. Using
is less compare to 3" cyclone.
experimental analysis it is observed that, an
ii. Slurry experiments
increasing angle of inclination leads to a
The effect of inclination on water split ratio for
reduction in water split to underflow.
10%, 28.76% & 50% solid concentration is shown
in Fig. 7. From Fig. 7 it is observed that the
change in recovery of water for 10% solid
concentration is not significant. For 28.76% solid
concentration the water recovery for the
vertically mounted cyclone is 20%, whereas it
(a) (b)
decreased to 13% when it operated at 600. Fig. 7
also represent the effec t of high solid
Fig. 5: Variation of Water split ratio (water)
concentration on water recovery to underflow.
with respect to inclination for 3 inch
It is observed that an increase in slurry
Hydrocyclone with (a) 12.5mm (b) 15mm spigot
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 MPT-2013

viscosity leading to decreasing pressure drop

inside the cyclone which leads to increase in
water recovery to underflow, whereas
increasing angle of inclination increases the
pressure drop which lead to decreasing water
recovery to underflow. From Fig. 7 b, it is
observed that at high pressure water recovery (a) (b)
to underflow decreasing because of high
pressure drop. Fig. 8: Cut-size (d50) variation with respect to
inclination for different feed concentration
with 12.5 mm spigot for (a) 10 psi (b) 25 psi
b. Sharpness of Separation (á) Vs. Inclination
The effect of inclination on sharpness of
separation for 10%, 28.76% solid concentration
is shown in Fig. 9. From Fig. 9 it is observed
(a) (b) that, increasing angle of inclination leads to
slight increase in sharpness of separation (á)
Fig. 7 :Variation of Water split ratio (solid conc.) for 10%, 28.76% solid concentration at constant
with respect to inclination for 3 inch pressure (15 psi), & constant spigot diameter
hydrocyclone with 12.5 mm spigot for (a) 10 (12.5mm). Fig. 9 also represent the high solid
psi (b) 25 psi concentration effect on sharpness of separation.
c. Cut- size (d50) vs. Inclination
The effect of inclination on cut size for 10%,
28.76% & 50% solid concentration is shown in
Fig. 8. From Fig. 8 it is observed that, the cut
size increases with cyclone inclination. For 10%
solid concentration the inclination effect on cut
size is not significant. But in 28.76% & 50% solid
concentration case inclination has a strong
effect on cut size. The cut size is increasing
above 300 inclinations as observed in 28.76% & Fig.9: Sharpness of separation (á) Vs.
50% solid concentration case. Fig. 9 also Inclination (i)
represent the high solid concentration effect on For high solid concentration 28.76% the alpha
cut size. Higher solid concentration decreasing is increasing, it means particle size less than
the partic le settling rate whic h leads to cut size escaping as underflow & greater size
increases the cut-size. At high pressure (25 psi) esc aping as overflow. In c ase of dilute
cut size is reducing compare to low pressure suspension every particle move independently,
(10 psi). For 28.76% solid concentration case cut while in the case of dense flow the particles
size is significantly increasing with inclination interact, which leads to increased suspension
at high pressure (25 psi).

269
 MPT-2013

viscosity. As result, fine particles can’t be
effectively transported to the overflow.
5. Numerical Simulations
3 inc h c yc lone whic h is used for the
experimental studies is considered for the
simulation studies. Sc hematic of the
hydroc yc lone and mesh used for the
simulations is shown in Fig. 2. Grid with
1,56,060 nodes used in the simulations. Air core
at low pressure centre region is resolved by
volume of fluid (VOF). Turbulence is modelled
using large eddy simulation (LES). The model
equations and strategy for simulating air-core
and flow field are similar to Narasimha et al
2006. Inlet is set to velocity and outlet has been
set to pressure boundary condition. A bounded
central differencing scheme is used to discretize
momentum equations. Pressure is solved by
using PRESTO. Quick is used to solve dispersed
phase transport equations. Fixed time step of
compensating by radial velocities. Which can
be seen as sum of the forces is equal. Lower
values of RMS radial velocity refers to minimal
radial particle dispersion compared to higher
RMS radial velocity. This results to an increased
cut-size at increased inclination positions,
which inherently have higher RMS radial
velocity values. The 450 inclination consistently
have higher tangential velocities and lower
RMS radial component, indicating the better
performance of cyclone compared any other
inclined positions. The basic reason beyond
this peculiar behaviour at 450 inclination yet to
be resolved.
(a) (b)

5.0x10-5s is used. Different inclinations are

Fig. 10: CFD predicted (a) Centrifugal to
maintained in the simulation by changing the
Gravitational forces (b) RMS radial velocity at
gravity direction values.
different inclinations along the radial positions
a. CFD predictions ii. Air-core predictions
i. Velocity predictions
Tangential, RMS radial velocities predicted by
CFD model at different inclinations has shown
in Fig. 10 a & b. From the figure 10a, it can be
noticed that, there is a mixed behavior in the
tangential velocity predictions. A decreasing
trend in the tangential velocity can be observed
from 00 to 300 inclinations. From 300 to 450 there
is an increase in the velocity and there after
velocity decrease at 600. Predicted RMS Radial
velocities also shown similar mixed behaviour
as predicted tangential velocities. There is an
improvement in the velocities from 00 to 300 (a) (b) (c) (d)
inclinations and decreased at 450, there after it
is showing increment up to 600. This can be true; Fig. 11: Contours of CFD predicted air-core at
as the inclination with respect to vertical (a) 00 (b) 300 (C) 450 (d) 600 inclinations
position is increasing the variations with CFD predicted air-core shape and position at
tangential veloc ity predic tions are different inclinations are shown in Fig. 11. From

270

the figure, it can be noted that the air-core size
is reducing with respect to inclination. From 0
to 45 degree inclination, air core size is reduced
and slight improvement at 60 degree. Air-core
position near the vortex finder and spigot
section is almost constant in all the inclinations.
iii. Axial velocity and LZVV predictions
(a) (b) (c) (d)
Fig.12:CFD predicted (a) Axial velocities; LZVV
contours at (b) 00 (c) 300 (d) 450 (e) 600 inclinations
Axial velocities, LZVV contours predicted by
CFD are shown in figure 12. From fig 12 (a) one
can observe that axial velocities predicted by
LES-VOF model at 0 0 inclination is having
higher veloc ities c ompared to other
inclinations. Sudden decrement is observed at
300 and further increment up to 600 inclination.
From Fig. 12 (b, c, d, e) peculiar behaviour is
observed at 450 i.e. from 0 degree inclination
there is a lateral shift towards the centre. At
450 inclination the shift is towards the wall.
(a) (b) (c)
Fig. 13: Conductivity profiles of reconstructive
images (Total Variation algorithm) at (a) 0 (b)
30 (c) 45 (d) 60 degrees
6. Cross Validation
The simulation studies are validated against
Electrical Resistance Tomography (ERT) data,
High speed image analysis data. ITOMS ERT
MPT-2013
acrylic conical section with 16 electrodes
around the periphery used for the
measurements two-phase concentrations, thus
estimating the air core profiles and the effect of
inclination on the air core diameter. Qualitative
prediction of air-core shape by ERT at different
inclinations is shown in Fig. 13.
(a) (b)
Fig. 14 (a): Air core diameters measured by
CFD validated against ERT and Experimental
video data (b) CFD predicted water split ratio
compared to experimental data at different
inclinations
Alternative technique used for the air core
diameter measurement is capturing a video and
analysis through images. A digital camera,
having 14.1 mega pixel resolutions with 10X
optical zoom (a Sony-G lens) at 30 fps at
1280x720 pixels, is used for air-c ore
visualization. A total of minimum 10 seconds
(nearly 300 frames) air-core recorded video is
converted into a number of images. Nearly 30
images are averaged (per sec basis) then
analyzed for air-core occupied diameters. The
averaged air-core diameter and its associated
(d)
standard deviations are reported in Fig. 14 a.
Another validation is with respect to water
split to underflow (Rf) is given in Fig. 14 b. From
the figure it can be observed that CFD predicted
water split is following experimental trend
with small deviation.
a. Radial dispersion Vs inclination
Roco demonstrated the significance of turbulent
dispersion force in turbulent transportation of
particles (Roco, 1996). This technique quantifies
271
 MPT-2013

the importance of turbulent dispersion force of From the Fig. 15 a, it can be noted that fine
particles to motion of particles by gravitational particles (4m) are dominated by dispersion
force. He also defined dispersion index which is force. Therefore, the dispersion index of the fine
the ratio of dispersion to agglomeration energy particles is above 1 at all inclinations. As the
per unit time. In the hydrocyclone perspective particle size increases, separation is dominated
agglomeration energy c an be taken as by centrifugal forces (Fig. 13 b, c). Inclination
c lassification energy per unit time. 450 has peculiar effect i.e. dispersion is very low
Classification energy further can be expressed for all the particle sizes from fine to coarse. This
as classification force multiplied by particle is due to low RMS radial velocities (10 b).
diameter. Dispersion index can be defined as
7. Conclusions
2
 u*  r The effect of inclination on hydrocyclone
 v i
I dis   i performance is studied using CFD technique
d p (   m ) and experimental methods. Water only and
slurry based classification experiments and the
Where u* is RMS radial velocity, v i is mean
corresponding two-phase CFD simulations in
tangential velocity at a radius r­i, dp is particle
3" and 4" diameter cyclones are carried out at
diameter, r, rm is particle and mixture density.
different inclined positions to the vertical plane.
Inc lination effec t on flow analysis of
Dispersion index hydrocyclone w.r.to mean and turbulent flow
S.No Remarks
value (Idis)
Separation is dominated field, water split, LZVV, air-core size and
1 Idis  1
by centrifugal forces position, and particle turbulent dispersion is
Particles are dispersed in made in detail. Water only, slurry volumetric
2 1  Idis  10
fluid
flow rates variation with inclination presented.
3 Idis > 10 Dispersion is main force
An improvement in the cut size with inclination
is observed at high feed solid concentrations
Dispersion index calculated for 4m, 28.29m, (28.76%, 50%). Enhancement of cut size is higher
63m particles is given in Fig. 13. From the Fig. with high pressures c ompared to low
15 a, b, c, it can infer that, separation is pressures. Inclination has very minimal effect
dominated by centrifugal forces towards the on the cut size at low concentrations. Dispersion
wall. Hence, there is reduction in the dispersion index is defined and the effect of inclination is
index.

(a) (b) (c )

Fig. 15: Dispersion index variation with inclinations for (a) 4m (b) 28.29m (c) 63m particles

272

explained for fine to coarse particles. Peculiar
effect of 450 inclinations due to the low predicted
radial RMS veloc ities is responsible for
improved performance and lower cut-size
compared any other inclined cyclone positions.
Air core size predic ted by CFD is cross-
validated against image analysis data with a
recorded video through plexiglass and ERT
data.
Reference
Asomah, A. K., Napier-Munn, T. J., 1997. An
Empiric al Model of Hydroc yc olnes,
Inc orporating Angle of Cyc lone
Inclination. Minerals Engineering. 10(3),
339-347.
Asomah, A.K., Napier-Munn, T. J., 1996. The
Performance of Inclined Hydrocyclones in
Mineral Proc essing. In Proc .
Hydrocycolnes ’96, ed. Claxton, S.a.T., eds.
Mech. Eng. Pubs., Cambridge, London. 273-
287.
Banisi, S., Deghan-Nayeri, H., 2005. Effect of
angle of hydrocyclone inclination on cut
size. Canadian Metallurgical Quarterly.
44(1), 79-84.
*******
273
MPT-2013
Bradley, D., 1960. The Hydroc yc lones.
Pergamon Press.
Hochsheid, R. E., 1987. Horizontal Cyclone in
Closed-Circ uit Grinding. Mining
Engineering. 262-266.
Johnstone, R. H., Rais, S. A., 1988. Increased
Performance Through Flash Flotation and
Cyclone Optimization, In 3rd Mill Ops.
Conf. Aus. Inst. Min. Met., Cobar. 79-84.
Narasimha, M., Brennan, M., Holtham, P. N.,
2006. Large eddy simulation of
hydrocyclone - prediction of air-core
diameter and shape. International Journal
of Mineral Processing. 80 (1), 1-14.
Orwe, D., Noreen, D., 1988. Horizontal Cyclone
Plant Trials at Bougainville, In 3rd Mill
Ops. Conf., Cobar, Aus. Inst. Min. Met. 71-
77.
Roco, M. C., 1996. One equation turbulence
modelling of incompressible mixtures. N.P.
Cheremisinoff (Ed.), Encyclopedia of Fluid
Mechanics. 10, 1-68.
Rong, R., Napier-Munn, T. J., 2003. Development
of a More Efficient Classifying Cyclone.
Coal Preparation. 23(4), 149-165.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Modeling of Oil-Agglomeration Process for Beneficiation of Coal

Fines Using Artificial Neural Networks

Sweta Kumari, V.K. Kalyani*, T. Gouri Charan, G.S. Jha and Amalendu Sinha
Central Institute of Mining & Fuel Research, Dhanbad – 826015, Jharkhand, INDIA

Abstract
In India, coal will continue to be the primary energy resource. Coal, the abundant fossil fuel, met
nearly the sixty percent of India’s total energy requirements. Because of high ash contained, Indian
coal reserved is mostly low quality with less calorific value and hence these coals are not much
suitable for utilization in steel industries. Due to mechanization of coalmines, the quantity of fine
coal generated has increased exponentially. Most effective method of removing inorganic impurities
from fine coals based on the concept of difference between the surface property of organic and
inorganic particles is oil agglomeration
Reported in the present paper are the results of the tests performed on finely ground middling’s of
coking coal using oil-agglomeration process in respect of the quantity and quality of the
agglomerates. The effects of important process variables of conditioning viz., conditioning time,
pH of pulp during conditioning and percent solids by weight in the pulp on the yield percent of
agglomerates were investigated in detail. On the basis of experimental data generated in respect
of all the above parameters, an attempt has been made to implement a three layer feed forward
artificial neural network (ANN) technique to simulate the process. The results indicate that
prediction from ANN model are in good qualitative and quantitative agreement with the
experimental results, thereby validating the accuracy of the developed model.

Keywords: Coal fines, Beneficiation, Oil agglomeration, Neural network, Back propagation
algorithm
1. Introduction promising method of “oil-agglomeration” has
been touted as a potentially effective method
Of the known processes for beneficiation of fine for agglomerating the coal fines, which is
coals below 500 microns is froth flotation. finding much wider applications now. In oil-
However, it suffers from some basic short agglomeration method, inorganic impurities
comings also, most important ones among are removed from fine coals based on the
which are comparatively lower yield and high concept of difference between the surface
moisture content of the beneficiated product property of organic and inorganic particles.
when most of the fines treated are below 76 Since the process of oil-agglomeration came
microns with high ash. Furthermore, the lower into the commerc ial applications, many
rank coal and also oxidized coal surfaces are improvements have been made to optimize the
unsuitable for flotation. In such cases, a very process parameters. Recently, Aslan ( 2009 ) has
improved the process by optimizing the
* Correspending Author:vkkalyani@yahoo.com
parameters that affect the agglomeration

274

performance in the oil agglomeration process
for whic h he used response surfac e
methodology and quadratic programming and
Kalyani, V.K.,et. al.,(2005) have reported the
Optimization of a laboratory sc ale froth
flotation proc ess using response surface
methodology.
In yet another study, Aktas (2002) has studied
different fac tors effec ting spheric al
agglomeration performance of coal fines and
Chary et al. (2010) have reported their findings
based on experimental conditions for recovery
of coking coal fines by oil agglomeration
method. However, Valdes et al. (2007) have
proposed a method for prediction of the
agglomeration capability of waste vegetable
oils in relation to the recovery of coal from coal
fines cleaning waste. In recent years, Cebeci and
Sonmez (2006) employed Box-Wilson
experimental design method to evaluate the
effec ts of proc ess parameters on the
agglomeration of bituminous coal. Panda et al.,
(2012) successfully applied ANN technique to
study the performance of jig for beneficiation
of non-coking coal. The recent trend in the study
of oil agglomeration technique is to model and
optimize process and design parameters of the
agglomeration method. Of late, a powerful
tec hnique used for modeling of oil
agglomeration process is artificial neural
network (ANN).
ANN has been used widely for dynamic process
modeling where the development of
phenomenological or the empirical models
either becomes impractical or cumbersome.
Neural Networks have recently become the
center of interest largely due to their wide
domain of applications in highly nonlinear
dataset (Kalyani, V.K., et al, 2008). Neural
network technique is highly suitable in solving
complex problems of mineral processing
industry. ANN’s are based on the concept of
interconnected system of simple processing
elements (called neurons) that can develop
c omplex nonlinear relationship between
independent and dependent variables (Kalyani,
V.K., et al, 2008). Neural Networks with
275
MPT-2013
remarkable ability to derive meaning from
complicated or imprecise data can be used to
extract patterns and detect trends that are too
complex to be noticed by either humans or other
computer techniques.
In the present paper, the effects of important
process variables viz., conditioning time, pH of
pulp during conditioning and percent solids by
weight in the pulp on the yield percent of
agglomerates were investigated in detail using
three layer feed forward ANN technique. The
results indicate that predictions from ANN
model are in good qualitative and quantitative
agreement with the experimental results,
thereby validating the ac c urac y of the
developed model.
2. Experimental
2.1. Materials used
The following materials have been used during
the experimentation:
1. Middlings (-0.5mm) as basic raw
materials having an ash content of 38.7
percent.
2. Diesel oil (sp. gr. 0.84) for conditioning the
pulp.
3. Furnace oil (sp. gr. 0.95) as agglomerating
reagent of the conditioned pulp.
4. Petroleum ether to deoil the agglomerates
prior to ash determination.
2.2. Machine used
i) Vertical cylindrical stirring vessel of 150
mm diameter and 600 mm height equipped
with four longitudinal baffles of 12.5 mm
width for conditioning.
ii) Bench scale horizontal cell of 114 mm
diameter and 920 mm length for
agglomeration.
2.3. Procedure
The representative sample of middlings was
subjected to wet grinding in a batch ball mill.
The top size of the ground middlings for all the
experiments was kept the same, at 100 meshes
B. S. (152 microns). Pulp of 40 percent solids by
weight in the slurry was prepared. The pH of
 MPT-2013

the pulp was adjusted to 8.5 and 2.0 percent possible from the historic process data only, i.e.,
diesel oil by weight of coal fines was added to without having the knowledge of process
the pulp, which was then thoroughly mixed phenomenology; approximation of even the
(conditioned) for 300 seconds in the vertical nonlinear, multiple input–multiple output
stirring vessel. The conditioned pulp was relationships can be simultaneously performed;
diluted to 20 percent solids by weight by adding
the model possesses a good generalization
water. The diluted conditioned pulp was then
ability, by the virtue of which it is possible to
agglomerated in a bench scale agglomeration
cell with the addition of 10 percent furnace oil precisely predict the outputs corresponding to
by weight of coal and stirring was continued a new set of process parameters which were
for another 300 seconds at 2100 rpm and then earlier not part of the data used for developing
stopped. The agglomerated products were the ANN model; and finally, even when any
separated from the unagglomerated residue relationship between the process parameters
using a sieve. The agglomerates thus obtained does not exist, the ANN has the capacity to
were dried and sized. A portion of agglomerates generate the relationship by ‘training’ the model.
was deoiled by petroleum ether. Ash percent of Because of these advantages, ANN models are
the oil free agglomerates were determined. being preferred over c onventional
Different tests were performed to find the effect mathematical techniques. The most widely used
of process variables of conditioning on the yield
neural network topology is the multilayer
of agglomerates at different levels of process
‘perceptron’ (MLP), which, by definition, is a
variables, which are listed in Table 1.
simple neural network consisting of input layer,
Table 1: Effect of process variables of condi-
output layer, and possibly one or more
tioning on the yield of agglomerates
intermediate layers of neurons. The perceptual
schematic s of multilayer perceptron are
Variables Levels Yield % of Agglomerates
Levels of conditioning oil dosage, depicted in Fig.1.
percent by weight of coal
1.5 2.0 2.5
Conditioning 60 45.9 47.83 47.73 y1 y2 yk yK
time (seconds) 180 54.67 58.20 58.59
300 58.45 63.24 63.41
420 59.07 63.28 63.72
1 2 k K Output layer
PH of pulp maintained 7.5 46.69 53.00 52.93
during conditioning 8.0 52.09 58.23 58.27
8.5 58.45 63.24 63.41
9.0 58.56 63.60 63.65
Percent solids by weight 20 50.92 56.86 56.57 Bias-2
in the pulp, (percent) 25 53.07 58.29 58.36 1 2 L Hidden layer
30 55.07 59.87 59.92
35 57.15 61.27 61.33
Bias nodes
40 58.45 63.24 63.41
Bias-1
45 58.53 63.65 63.69
1 2 n N Input layer

3. Fundamentals of Neural Networks x1 x2 xn xN

An artificial neural network is a computing

technique based on the mechanisms of highly
interconnected parallel structure of the human
brain (Tholudur and Famirez, 1998). An ANN-
based process model has a distinct edge over
phenomenological or empirical models (Hornik
et al., 1989; Hagan et al., 1996; Freeman and
Skarpura, 1991) in that its development is
Fig. 1: Multilayer Perceptron Neural Network
Model
The MLP can also be understood as a ‘feed
forward’ artificial neural network technique
consisting of three or more layers of neurons
(nodes) with nonlinear activation function. The
total (net) input to a neuron and its output are
calculated using a transfer function. Different

276
 MPT-2013

transfer functions are used in neural network It is seen from this table that an optimal MLP
analysis. In the present study, the sigmoidal architecture obtained has three input nodes
function [28], represented by the equation (N=3), six hidden layer nodes (L=6), and two-
below, has been used: output layer node (K=2). A general and usual
1 dy feature of an MLP network with good function
y  ( 0 ,1 ) ;  y( 1  y ) (1)
1  exp(  x ) dx approximation and generalization abilities is
Thus, in a multilayered ANN, each layer that it results in small but comparable root
consists of a number of neurons. Each neuron is mean squared error (RMSE) values for both the
connected to the neurons of the next layer by training set (Etrn) as well as the test set (Etst). The
‘weights’, which is simply defined as the MLP network developed in the present work is
strength of connection of one unit to another. in consonance with this characteristic feature,
The weights for each connection are initially as evidenced by the obtained small values of
assumed as random numbers. Once the ANN the ‘train’ and ‘test’ error.
structure is defined, the network goes to
‘training phase’ to obtain the relationship 72

67
between input and output variables through
62

learning process. ‘Learning’ is carried out

Yield % (Predicted)

57

through a back propagation algorithm, which 52

is essentially a gradient method. In a back 47

47 52 57 62 67
propagation algorithm, weights are adjusted Y ie ld % ( O b s e r v e d )

in such a way that the error between the

desired output and the ac tual output is Fig.2: Comparison of predicted with observed
yield%
propagated backward through the net. The
backward propagation of the error is used to 27

update the weights to get the desired output.

26

26

25

4. Development of ANN based model

Predicted Ash%

25

24

24

The data set, comprising process variables, 23

23

forms the network’s input space, and the 22

22

corresponding y values (target yield % and ash 22 23 24

Actual Ash%
25 26 27

%) represent the network’s desired (target)

output space. Using this dataset, an optimal
MLP model has been developed employing the
software STATISTICA, Version 7.0. The various
neural network structures, using linear and the
logistic function, were tested. The results of the
ANN structure, evincing the best performance
only, are mentioned in Table-2.
Table 2: The ‘train’ and ‘test’ error values,
showing the best performance of ANN
structure
Network Structure Train Error Test Error
Coefficient (Yield%)
MLP 3:3-6-2:2 0.011539 0.119284
Fig.3: Comparison of predicted with observed
ash%
The plots depicted in Figs. 2 and 3 lead to the
following observations:
1. The plots of ANN-predicted and observed
responses (yield% and ash%) in both the
figures indicate that the predictions from
ANN models are in good agreement with
the experimental results.
2. The high correlation coefficient obtained for
the predicted yield% and observed yield%
Correlation Correlation Coefficient is 0.99, which indicates that the ANN model
(Ash%)
has the ability to explain the 99% of the total
0.99
0.97
variations of the system.

277

3. The c orrelation coeffic ient between
predicted ash% and actual ash% is 0.95,
which indicates that the ANN model has
the ability to explain the 95% of the total
variations of the system in case of ash%.
5. Conclusions
In this study, a three layer feed forward
artificial neural network model, which is
trained using back propagation algorithms has
been employed for modeling three process
parameters of the highly c omplex oil
agglomeration process for beneficiation of fine
coals. Present work indicated that neural
network could be successfully applied to the
highly complex oil agglomeration process
incorporating three important variables,
which govern the oil agglomeration process.
Various network structures were tested to
evaluate the predictive capabilities of the
artificial neural network. The study indicates
that the artificial neural network having one
hidden layer consisting of six neurons is the
best network for prediction of the response
variables. It is observed that the predicted
values obtained using ANN model are in very
good agreement with the experimental values
(R2 = 0.99 for yield % and R2 = 0.95 for ash %). As
such the ANN modeling has great potential in
significantly improving the oil agglomeration
process performance. The present modeling of
oil agglomeration process for beneficiation of
fine coals has reaffirmed the excellent validity
of ANN model of coal beneficiation in respect of
different variables, in that it has greatly help in
optimizing the process parameters for highest
yield%.
References
Aktas, Z., 2002. Some factors affecting spherical
oil agglomeration performance of coal fines.
Int. j. Miner. Process. 65, 177-190.
Aslan, N., Unal, I., 2009. Optimization of some
parameters on agglomeration performance
of Zonguldak bituminous c oal by oil
agglomeration. Fuel 88, 490-496.
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278
MPT-2013
Cebeci, Y., Sonmez, I., 2006. Application of the
box-wilson experimental design method for
the spherical oil agglomeration of coal. Fuel,
85, 289-297.
Chary, G.H.V.C., Dastidar, M.G., 2010.
Optimization of experimental conditions for
rec overy of c oking c oal fines by oil
agglomeration technique. Fuel 89, 2317-2322.
Freeman, J.A., Skapura, D.M 1991. Neural
network algorithms. Applic ation and
programming techniques, addition wisely,
reading, M.A.
Hagan, M.T., Demuth, H.B., Beale, M.H., 1996.
Neural network. PWS publishing, Boston
Hornik, K., Stinchcombe, M., White, H., 1989.
Multilayer feed forward networks are
universal approximation . Neural network
2, 359-366.
Kalyani V K , Pallavika, Gouri Charan T and
Choudhury S. 2005. Optimization of a
laboratory scale froth flotation process
using response surface methodology. 25,
141-153.
Kalyani, V.K., Gouri Charan, T., Haldar DD,
Sinha A. Suresh N. 2008. Coal-fine
beneficiation studies of a bench-scale water
only cyclone using artificial neural network.
Int. J Coal Preparation and utilization. 28.
94-114.
Kalyani, V.K., Pallavika et al., 2008. Study of
laboratory scale froth flotation process
using artificial neural networks. Miner.
Process. Extract. Metall. Rev.. 29, 130-142
Panda, L., Sahoo, A.K., Tripathy, A., Biswal, S.K.,
Sahu, A.K., 2012. Application of artificial
neural network to study the performance of
jig for beneficiation of non-coking coal. Fuel
97, 151-156.
Tholudur, A., Ramirez, W.F., 1998. System
modeling using neural network parameters
func tions. Applied mathematic s and
computer science 8, 887-897.
Valdes, A.F., Azpiroz, M.D.G., Blanco, C.G.,
Garcia, A.B., 2007. Experimental prediction
of the agglomeration capability of waste
vegetable oils (WVO) in relation to the
recovery of coal from coal fines cleaning
wastes (CFCW). Fuel 86, 1345-1350.
 MPT-2013

COAL PREPARATION

279
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280
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Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Chemical Beneficiation of High Sulphur North-East Indian Coals

by Alkaline Oxidation

Runjun Chetia, Binoy K Saikia*, Dileep K Dutta, Bimala P Baruah*

Coal Chemistry Division, CSIR-North East Institute of Science & Technology, Jorhat-
785006, India
Abstract
The sulphur present in coals is retardant to its uses in thermal and steel industries. In this study,
chemical desulphurization of few high organic sulphur Indian coal samples was performed by
alkaline oxidation in air. The total sulphur, pyritic sulphur, sulphate sulphur and organic sulphur
contents were found to be reduced by 32.94, 59.57, 99.41, and 11.71% respectively in this process.
The FT-IR and XRD analyses of desulphurized coal samples are discussed.

Keywords: Indian coal; sulphur; desulphurization; alkaline oxidation; ariel oxidation; FTIR-XRD.

1. Introduction Borthakur, 2001; Masciantonio, 1965; Gala et al.,

Coal is a heterogeneous material, which
consists of organic and inorganic material with
mineral matter including sulphur. It contains a
variety of trace elements like Fe, Mn, Be, Co, Cd,
Cl, Mo, Pb, Cr, V etc. India is the third largest
produc er of c oal in the world has been
prominently used in the thermal plants along
with other countries of the world.
However, the high sulfur and mineral matters
in c oals imposes several environmental
problems (Chadwick et al., 1987). Thus, the
removal of the unwanted sulfur is essential
before its further utilization. The sulphur in
coals generally present as inorganic and
organic forms (Kozlowski et al., 2003). Although
the inorganic component can be completely
eliminated from coal, the complete removal of
organic portion is difficult. Desulphurization
of these types of sulfur is possible only by
c leaving the C-S bonds (Mukharjee and
* Correspending Author: bp baruah @yah oo.com BPB;
bksaikia@gmail.com
1989; Liu Kaicheng et al., 2008). Thus the
removals of organic sulfur using these methods
are very much complex and expensive. Thus
there is an urgent need to consider the economic
factors of the different coal beneficiation
processes (Chuang et al., 1983; Demirbaº, 1999;
Pietrzak and Wachowska, 2003; Baruah and
khare, 2006; Wheelock, 1977). Many efficient
oxidizing agents have been used by different
researcher, such as performic acid (Banerjee et
al., 1987), aqueous sodium hydroxide followed
by HCl treatment (Mukharjee et al., 2001),
chlorinolysis and hydrothermal techniques
(Sain et al., 1991), mineral acids such as nitric
ac id (Baruah et al.,1987), organometallic
compounds(Mazumdar et al.,1989), solvent
extraction and alkali treatment (Baruah and
khare 2006), oxygen(Slagle et al.,1980, Sareen et
al.,1977) sodium hydroxide (Ali et al.,1992),
pyrolysis techniques(Baruah and Khare, 2007).
These processes have been used to reduce
sulphur and ash contents in coals. These

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 MPT-2013

processes also increase the calorific value of 3286 (Table 6). The trace elements in coal and
coals. alkaline leachates were determined by Atomic
The main objective of this experiment is to Absorption Spectrophotometer (Model: Perkin
remove sulfur from high sulfur bearing coals Elmer; Analyst-700) (Table 5). The combustion
from Assam NE India by using atmospheric effic ienc y and energy of ac tivation was
oxidation in alkali medium. In this study, the calculated by using the method as reported
atmospheric air was used during alkaline (Table 4) (Khare et al., 2011).
oxidation of high sulphur coals. The effect of Table1: Physico- chemical characteristics of raw
time on the extent of organic and inorganic and oxidized coals (as received wt%)
sulfur removal was also determined. Sample M VM Ash FC TS PS SS OS
% Removals
Ash TS PS SS OS
Raw 2.49 43.08 3.27 51.16 3.43 0.47 0.56 2.39 -- -- -- -- --
AO-1hr 0.87 42.04 2.12 54.97 2.79 0.41 0.00 2.38 35.16 18.65 12.76 99.52 0.41

2. Experimental sections AO-4hr

AO-5hr
0.455
0.433
42.85
40.91
2.08
2.05
54.65
56.61
2.43
2.38
0.23
0.20
0.00
0.00
2.20
2.18
36.39
37.30
29.15
30.61
51.06
57.44
99.64
99.36
7.94
8.78
AO-6hr 0.380 41.7 1.72 56.20 2.30 0.19 0.00 2.11 47.40 32.94 59.57 99.41 11.71

2.1. Coal samples

The high sulfur bearing coal sample was
collected from Tirap colliery of Makum coalfield
latitudes 27°132 –27°232 N and longitudes
95°352 –96°002 E, Assam. The coal sample was
ground to –72 BS 0.211 mm size and was stored
in air tight container for further analysis.
2.2 Physico-chemical analysis
The proximate analysis of the coal samples has
been carried out by using Proximate Analyzer
(TGA 701, Leco, USA), the total sulfur was
determined by sulphur analyzer (S-144 DR,
Leco, USA). The forms of sulphur were
determined by following standard methods
ASTM D 2492.The physic o-c hemic al
characteristics of the coals are summarized in
Table 1.
X-ray diffraction data of coal samples were
obtained using computer controlled X-ray
Diffractometer, (Model Rigaco, ULTIMA IV) and
shown in Figure 3. FT-IR spectra of the coal
samples were recorded in FT-IR Spectrometer
by Perkin Elmer system, 2000, Model 640B by
using KBr pellet (Figure 2). Thermal analysis of
the coals have been obtained in the thermal
gravimetric analyzer TGA TGA 701, Leco, USA
in O2 atmosphere heating rate :100C/min ;final
temperature:800 0 C (Figure 4). The calorific
value of coal determined by using Bomb
Calorimeter (Leco, AC-350) following ASTM D
* M: moisture; VM: volatile matter; FC: fixed
carbon; TS: total sulphur; PS: pyritic sulphur;
OS: organic sulphur.
2.3. Alkaline oxidation in air
The coal samples of about 250g were mixed
with 0.25N NaOH in a beaker and placed on a
hot plate. The mixture was stirred mechanically
at about 300 RPM. Atmospheric oxygen was
passed through the solution at the flow rate of
0.136m3hr-1. This procedure was repeated for 1,
4, 5 and 6 hours continuously at 80ºC under the
similar conditions. The coal residues were
collected at each time intervals and filtered,
washed by dilute HCl solution along with hot
water till the pH of the solutions become neutral.
The physico-chemical analysis of the residues
was carried out in further studies.
Figure 1: Schematic diagram of alkaline
oxidation process
3. Results and Discussions
3.1. Physico-chemical analysis of
desulphurized coals

282
 MPT-2013

The physico-chemical characteristics of the
raw and alkaline oxidized coal samples are
given in Table 1. The ash removal of 35.16, 47.40,
36.39 and 37.30% were observed for 1, 4, 5, and
6 hrs respectively in the process. The effects of
alkaline oxidation on the removal of total sulfur
and forms of sulphur c ontents are also
presented in Table 1. It shows that alkaline
oxidation leads to removal of considerable
amount of total sulfur from these coal samples.
The total sulfur removals were 18.65, 29.15,
30.61and 32.94 % respectively at 1, 4, 5 and 6
hrs. Moreover, the process could remove a
maximum of 99.41, 59.57 and 11.71 % sulphate,
pyritic, organic sulphur respectively from the
coal samples at different time intervals.
Thus, alkali oxidation in air has been observed
to be a cost effective process for removal of all
the forms of sulphur from coals and can be
utilized for low organic sulphur coals. The
possible reactions behind the pyritic sulphur
and organic sulphur are as suggested [Baruah
and Khare, 2006; Fridman et al., 1977;
Mukharjee, 2003].
2NaOH + FeS2  Na2S + Fe OH2+S
Na2S+ 2H2O  2NaOH + H2S
RCH 2SCH 2R+2NaOH  RCH 2O+R’
CH2O+Na2S+H2O 2RSSR + 4OH-  3RS- +
RSO2 +2H2O
RSH +2NaOH  Na2S +2H2O +R’CH=CH2O
Álkali may also react with sulfoxides and
sulfones formed during oxidation as follows:
coal samples (Table 2 and Figure 2). The
absorption band in the region of 550 cm -1 is
observed due to the stretching vibration of S-S
bonds of sulfide and C-S bonds in primary and
secondary thiols. However, the peak intensity
is reduced for treated coal samples, which
indicate the elimination of these groups. The
bands at 3324, 1190, 1100- 400 cm-1 are assigned
to mineral matter present in these coals. The
vibration bands in the region of 1415-1380 cm -
1
and 1200-1185 cm-1 are observed due to the
presence of organic sulfur in coal. The stretching
vibration in sulfoxides generally occurs in the
range of 1070-1030 cm-1. The absorption band
for -SO2 in sulfones occur at 1350-1300 cm-1 for
asymmetrical vibration and at 1160-1120 cm -1
for symmetric al vibration respec tively.
Moreover, the intensity of S=O peak of the
oxidized samples was found to be slightly
higher that of the raw coal sample indicating
their participation during oxidation.
Figure 2: FT-IR Spectra of T2-Raw and oxidized
coals
Table 2: FTIR peak assignment of coals
Wave No cm-1 Assignments Wave No cm- Assignment
1

3427,3445 H-O-H, Quartz 1372 CH2/CH3 def.

3412 N-H 1300-1350 -SO2

3384-3406 O-H 1120-1160 -SO4

3.2. FTIR analysis of coals 3324,1190 Quartz 1134 Gypsum

2800-3000 CH3,CH2,CH 754 Kaolinite, S-OR

The FTIR spec tra along with their 1506-1665 C=O 570-705 C-S
.
interpretations of raw and oxidized coal 1600 C=C 400-1100 Clay minerals-Quartz,
Kaolinite, illite,
samples reveal the partial removal of sulfur 1384 SO42- 420 Pyrite
components and mineral matters from the raw

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 MPT-2013

3.3. XRD analysis of coals 3.4. Thermal analysis of coals (TGA-DTG)

The d-values of the XRD peaks are shown in the
Table 3. The XRD peaks (Figure 3) of the raw
and oxidized coals were assessed and observed
that some of the mineral peaks including Calcite
(C), Kaolinite (K), Quartz (Q) and Muscovite (M)
were disappeared during the process. Thus,
theses mineral components were partially
removed during the alkaline oxidation process.
Figure 3: XRD spectra of T2-raw and treated
coal samples
Table 3: XRD peak assignment of coal samples
Sample 2theta d-value Assignment
Following major changes are observed during
thermal analysis of the coals
i. The coal contains residual moisture. The
initial peak is relates to loss of moisture at
around 100 0C.
ii. As the volatile start to be released, the rate
of weight loss increases and is characterized
by the change at around 240 0C in TGA
spectra.
iii. At higher temperature, the fixed carbon
begins to oxidize and the volatiles become
totally liberated as indicated by fixed carbon
initiation temperature.
iv. The reactivity of coal is evaluated from the
peak temperature (PT). Coal with greater
weight loss rates at lower temperature are
generally easier to ignite and burn, while
profiles with high peak temperature
indicate maximum thermal decomposition
and slow burning coals. Here, the peak
temperature is around 470 0C.
v. The burn out temperature (BT) is the
temperature at which combustion ceases;

T2- Raw 12.700 6.9645 Kaolinite

high burnout temperature indicates poor
20.900 4.2468 Variscite, Orthoclase, Quartz, combustion efficiency. Here, the BT is around
26.620 3.3459 Quartz, Orthoclase, Biotite 740 0C for the coal samples.
AO-1hr 20.880 4.2509 Orthoclase, Quartz, Gypsum

23.240 3.8243 Calcite

23.740 3.7448 Antigorite

24.880 3.5758 Kaolinite

26.680 3.3385 Orthoclase, Quartz, Biotite

50.080 1.8199 Calcite, Anatase, Quartz

AO-4hr 20.960 4.2348 Orthoclase

23.200 3.8308 Calcite

26.700 3.3360 Orthoclase, Biotite, Quartz

AO-5hr 12.1 7.3116 Gypsum

8.54 10.346 Biotite

20.12 4.3103 Quartz, Gypsum

20.82 4.2639 Gypsum, Quartz, Orthoclase.

26.54 3.356 Quartz, Biotite, Orthoclase.

78.7 1.2148 Hemetite, Dolomite.

AO-6hr 18.4 4.8187 Chlorite

20.8 4.267 Quartz, Chlorite, Gypsum

26.6 3.3484 Biotite, Quartz.

41.78 2.1603 Kaolinite, Dolomite, Calcite,

Quartz.

45.46 1.9937 Quartz, Dolomite, Hemetite

Figure 4: TG A and DTG curves of raw and treated

coal samples
284
 MPT-2013

Table 4: Activation energy (Ea) and Table 6: CV and AFT of raw and treated coal
combustion efficiency (S) of raw and oxidized samples
coal samples Sample CV AFT0C
Kcal/kg
IDT HT FFT
Samples Ea KJ/mol S
T2- raw 7810 1210 1360 1460

T2-Raw -175.597 4.9260 x10-08 AO-1hr 8075 1060 1350 1500

AO-4hr 8105 1060 1320 >1500

AO-1hr -179.29 1.63867 x10-05
AO-5hr 8160 1120 1360 >1500
AO-4hr -188.62 1.56762 x10-05
AO-6hr 8350 1070 1450 >1500
AO-5hr -213.587 1.54046 x10-05

AO-6hr -287.20 1.29645 x10-05 * CV: c alorific value; AFT: ash fusion
temperature; IDT: initial deformation
3.5 Trace element analysis of leachates temperature; HT: hemispherical temperature;
The trace elements in the final leachates were FFT: final flow temperature.
determined and shown in Table 5. It is observed
3.7 Effect of time
that the leachates contain the high amounts of
As with 0.070 ppm and 0.024 ppm respectively. The alkaline oxidization in air at different time
Arsenic are harmful and undesirable, which intervals (1, 4, 5 and 6hrs) shows that total
must be taken care before implementation of sulphur removal was increased with time. On
the process in industries. the other hand, the removals of other
Table 5: Trace element in alkali oxidized coal components remain more or less same with time
leachates (in ppm) (Table1).
Sample Al As Fe Cd Pb V K Mg Zn
AO-1hr 6.9 0.070 BDL BDL BDL 0.0097 0.00345 BDL 0.11
AO-4hr 9.4 0.024 BDL BDL BDL 0.0073 0.0013 BDL 0.05
3. Conclusions

3.6 Determination of calorific value and ash
fusion temperature
The calorific values (CV) and ash fusion
temperature ranges (AFT) are very important
indexes of any coal characteristics. The CV of
the alkali oxidized coals were determined and
observed to be appreciably increased with the
removal of sulphur components (Table 6). Ash
with low fusion temperature causes serious
problems during combustion in power plant.
The AFT of the alkali oxidized coals is also
slightly increased from 1450 to 1500ºC during
the process. Thus, qualities of the coals were
found to be enhanced by the present process
and it could be considered for application in
thermal plants. The difference in AFT could be
attributed by these reasons: (a) –C-C- bond was
oxidized during the treatment; (b) part of the
soluble organic was washed away when the
coal was treated.
285
The results obtained explores the possibility
of removing sulphur from the North-Eastern
high sulphur coals in a low cost process by
using the atmospheric oxygen and dilutes
NaOH solutions. The atmospheric oxygen is
inexpensive, so it is highly promising. The
proposed method is an effec tive way of
removing organic sulphur from any high
organic sulphur coals. The TGA-DTG curve
indicates that burning quality of the coals is
improved. The quality of coal is suitable for
using in various industries like c ement
industries, steel industries, textile industries,
railway industries, thermal plant etc. However,
the disposal of liquid waste should be taken care
of.
Acknowledgements
Authors are thankful to Director, CSIR-NEIST,
Jorhat for giving permission to report the works.
Authors are also thankful to CSIR, New Delhi
for funding.

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 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Microbial Upgradation of Meghalaya Coal by Rhodococcus

Rhodochrous and Pseudomonas Aeruginosa

A.Ghosh, Sujata, Abhilash*, B.D.Pandey

CSIR-National Metallurgical Laboratory, Jamshedpur-831007
Abstract
Meghalaya coal contains 1.61 to 8.92 % of sulfur. The sulfur commonly exists as inorganic sulfur
found mainly as pyrite and organic sulfur (mainly found as heterocyclic aromatic compounds
like thiophene, dibenzothiophene and phenyl disulphide). In this investigation, bacterial strain
enriched with L.ferrooxidans isolated from Tirap coal mines, Assam in 9K media at 40oC and pH 1.6-
1.8, was able to remove 51.4% pyritic sulfur using 10%( w/v) Meghalaya coal sample of <50mm
size in 3 days. Consequently, two different bacteria Rhodococcus rhodochrous and Pseudomonas
aeruginosa pre-adapted on 75mM of dibenzothiophene (DBT) and Phenyl disulphide (PDS)
respectively resulted in maximum 51% and 52% desulfurization 10 %(w/v) non-depyritised feed
coal sample at an optimum pH 6 and 40oC, in 72h. The various parameters governing the process
are discussed.

Keywords: Coal; sulfur; organic sulfur; bacteria; desulfurization.

1. Introduction disulphide, thiophene, thioketone, thiol and

Coal is one of the most abundant fossil fuel with
3700 million tons of hard coal produc ed
worldwide per year and about 940 million tons
of lignite (Fakoussa and Hofrichter, 1999).
During the combustion of coal, the sulfur present
in the coal get oxidized and produce SO‚ along
with NO‚ it cause acid deposition, may be
detrimental effect on soil, agriculture and
ecosystem (Klein et al.1994). So, removal of
sulfur before combustion is the best policy to
ignore such kind of problem. Coal from NE
region of India possesses high amount of sulfur
and the major portion in the form of organic
sulfur (Borah and Baruah, 1999). Organic Sulfur
present in NE coal in different form like
* Correspending Author: Abhilash, Tel: +91-657-2345274;
Fax: +91-657-2345213; Email: abhibios@gmail.com
many more. But when this coal is subjected to
pyrolysis there made a change in organic sulfur
content of coal. After pyrolysis the thioketonic
and thiophenic sulfur content changes into
condensed thiophenic structure and chemical
could not react with these structure (Ali et al.
2009).The Indian coal contain different types of
mineral matters like quartz, kaolinite, calcite,
siderite, dolomite, illite, gypsum (Mukherjee
and Srivastava, 2005). These types of mineral
matters increase the impurities in coal, which
causes reduction in heat value and this also leads
to the environmental pollution (Singh and Naik,
1997). Due to the environmental problem
associated with the coal combustion, there are
many regulation are developed to control the
emissions of unwanted pollutants.

287

In spite of the physical and chemical method
practiced, biological techniques have been
recently subjected to remove the sulfur from
coal. The biological processes are performed
under mild conditions with no harmful reaction
products and the value of coal is not affected
(Monticello 1998). Coal contain different forms
of sulfur such as inorganic sulfur as pyritic
sulfur, organic sulfur as dibenzothiophene,
thiophene. Certain microorganisms oxidize the
reduced sulfur found in coal and convert them
into product which is water soluble. Thiobacillus
ferrooxidans type bacteria first showed the
extraction of pyrite from coal in aqueous phase
at low pH (Silverman et al. 1963). Thermophilic
microorganism Sulfolobus acidocaldorius could
remove 96% inorganic sulfur and about 50% of
total sulfur from coal (Kargi and Robinson,
1982). A microorganism metabolically related
to Xanthomonas maltophila, was able to remove
both organic and inorganic sulfur at neutral
pH, with effic ienc ies of 69% and 68%
respectively (Gomez et al.1999). Rhodococcus
erythropolis (Izumi et al.1994), Rhodococcus
rhodochrous ATCC No.53968 and Bacillus sphaericus
ATCC No. 53969 were proven to be capable of
selectively degrading the organic C-S bond in
organic sulfur component of coal (Kilbane,
1994). Some microorganisms like Hansenula
sydowiorum, Hansenula ciferrii, Hansenula lynferdii
and Cryptococcus albidus were also used to remove
the sulfur content from carbonaceous solids
(Stevens and Burgess, 1989).
In this study, bac terial strain with good
tolerance to organosulfur compounds like
dibenzothiophene (DBT), phenyl disulphide
(PDS) were isolated from Tirap coal mines,
Assam for depyritization and organic sulfur
degradation. The ability of the selected strains
for the removal of both inorganic sulfur and
organic sulfur from high sulfur coal was also
investigated.
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MPT-2013
2. Materials and Methods
2.1. Microorganisms
Pyrite sulfur degrading bacteria L.ferrooxidans,
was isolated and cultivated in 9K medium
[(NH4)2SO4 - 3 g, KCl- 0.1 g, K2HPO4 - 0.5 g, MgSO4
.7H2O -0.5 g, CaNO3 . 4H2O -0.01 g, FeSO4 . 7H2O
to a final volume of 1L with distilled water,pH-
1.6-1.8]. Organic sulfur utilizing bacteria
Pseudomonas aeruginosa and Rhodococcus
rhodochrous, were cultivated in nutrient broth
medium in presence of different organosulfur
compound such as DBT, PDS. L.ferrooxidans is
gram negative in nature, single in arrangement
and vibroid in shape. Organic sulfur utilizing
Pseudomonas aeruginosa is gram negative, single,
long rod in shape. Rhodococcus rhodochrous is
gram positive in nature, single, long rod shape
bacteria. To know the metabolic activity of the
bacterial strains some biochemical tests like
indole test, methyl-red, Vogus- proskauer test,
citrate utilization, triple sugar iron and oxidase
tests were performed. Biochemical tests of
L.ferrooxidans strain showed positive for methyl
red, vogus- proskauer and triple sugar iron
tests. Rhodococcus rhodochrous and Pseudomonas
aeruginosa tested negative for Indole, Methyl
Red, Vogus- Proskauer, Citrate utilization,
Triple Iron Sugar whereas positive for presence
of oxidase. Morphological characteristics of the
bac terial strains showed in mic rosc ope
depicted in Fig.1.
(b) (c)
(a)
Fig. 1: Microscopic view of bacterial cultures
at 1000x magnification: (a) L.ferrooxidans, (b)
Pseudomonas aeruginosa,(c) Rhodococcus
rhodochrous
2.2. Coal sample
The coal sample of Meghalaya obtained in the
rock form is washed and cleaned and processed

to <50µm size for further benc h sc ale
experiments. This coal sample was also tested
for pyritic sulphur, sulphate sulphur, organic
sulphur and total sulphur using the ASTM
(D2492) method as depicted in Table-1.
Table 1: Sulfur content in Meghalaya coal
Pyritic sulfur 0.15%
Organic Sulfur 1.69%
Sulfate Sulfur 0.40%
Total Sulfur 2.25%
2.3. Medium and chemicals
9K media used for isolation and cultivation of
pyrite degrading bacteria. Nutrient broth
medium (HIMEDIA) used for isolation and
cultivation of organic sulfur utilizing bacteria.
Dibenzothiophene (DBT), Phenyl disulphide
(PDS), was purchased from Sigma-Aldrich and
Folin-Cioc alteau from Sisc o researc h
laboratories Pvt. Ltd. All chemicals were of
analytical grade and commercially available.
2.4. Optimization of growth parameters of
isolates
To determine the effect of pH and temperature
on bacterial growth, pH values was adjusted
to 1-10 and temperature was varied in range
30-45oC. Each medium was inoculated with an
overnight c ulture (1% v/v) of the
microorganism and incubated in a shaker at
100rpm at 37oC for 48 h. At an interval of 24h,
representative aliquot of sample was collected
from each flask and their O.D (Optical Density)
was measured using spec trophotometer
followed by protein estimation. Lowry method
was used to determine amount of protein
produced by the bacteria at different pH and
temperatures.
2.5. Adaptation of bacteria in different
concentration of various organosulfur
compounds
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MPT-2013
Rhodococcus rhodochrous and Pseudomonas
aeruginosa were adapted on various
concentrations of DBT and PDS in the range of
1-75mM. Nutrient broth media were prepared
with DBT and PDS of different concentration as
a substrate for bacteria; the growth was then
quantified by cell growth.
2.6. Biodesulfurization experiments
Bio-desulfurization experiments were carried
separately to remove pyritic sulfur with
Meghalaya coal sample (size <50mm) as
substrate using L.ferrooxidans. Batch experiment
was performed in 9K media in respective to
their growth using 10% (v/v) inoculum at 10%
(w/v) pulp density of coal at 40ºC,unless stated
otherwise. Meghalaya coal of (size <50mm) was
also subjected for bioremoval of organic sulfur
at varying condition of pH 4-8, temperature 30-
45oC and 10-30% pulp densities by using the
pre-adapted strains. The flasks were incubated
in a shaker at 100rpm at 40oC for 72 hours.
After 72 hours, solution in each flask is filtered
using a vacuum filtration unit. The leached
residue in the form of coal was washed 5 times
using distilled water. The washed residue is
then dried at room temperature. This dried
residue is then tested for pyritic sulphur,
sulphate sulphur, organic sulphur and total
sulphur using the ASTM (2492) method.
3. Results and Discussion
3.1. Optimization of growth parameters
It was observed that the amount of protein
increased as their optical density increased after
48 hours of incubation at different pH. After
inoculation of Pseudomonas aeruginosa, different
optic al density values and protein
concentration values were recorded at different
pH using UV-VIS spectrophotometer for 48h
and showed that the optical density and protein
concentration were higher at pH 6.0. After 48h,
the optical density rose to 2.201 and protein
 MPT-2013

yield was 0.41 mg/mL. Identically, in Rhodococcus

rhodochrous after 48h the optical density was
2.316 and protein yield being 0.6 mg/mL.
Optimum pH required for the growth of both
microorganisms as illustrated in Fig.2-3, is
concluded as pH 6.0.
The growth of two bac teria Pseudomonas
aeruginosa and Rhodococcus rhodochrous were also Fig. 4: Variation of optical density in different
optimized at different temperatures. After 48 temperature after 48h of incubation
hours at 40oC, Pseudomonas aeruginosa and Pseudomonas aeruginosa at pH 6.0
Rhodococcus rhodochrous, produced higher amount
of protein with higher O.D. Protein
concentration was obtained to be 0.47mg/mL
with O.D value of 2.879 for Pseudomonas
aeruginosa. The amount of protein produced by
Rhodococcus rhodochrous was 0.87mg/mL with
O.D being 3.1613. The results of temperature
optimization are shown in Fig.4-7 and
concluded 40oC temperature as most optimum Fig. 5: Variation of protein concentration in
for its growth. different temperature after 48h incubation of
Pseudomonas aeruginosa at pH 6.0

Fig. 2: Variation of protein concentration in

Fig. 6: Variation of optical density in different
respect to their optical density at different pH
temperature after 48h of incubation
for Pseudomonas aeruginosa
Rhodococcus rhodochrous at pH 6.0.

Fig. 7: Variation of protein concentration in

Fig. 3: Variation of protein concentration in
different temperature after 48h incubation of
respect to their optical density at different pH
Rhodococcus rhodochrous at pH 6.0
for Rhodococcus rhodochrous

290

3.2. Adaptation of bacteria on organosulfur
compounds
Bacterial strains were grown and maintained
in nutrient broth medium. To show their
activity in presence of organic sulfur, the
microorganisms were grown in nutrient broth
medium in presence of synthetic organic sulfur
compounds as substrate. Dibenzothiophene
and phenyl disulphide were provided as sulfur
source in the medium. Microorganisms were
adapted on different concentration of these
organic sulfur c ompounds. Rhodococcus
rhodochrous was adapted up to 75mM
concentration of DBT and Pseudomonas aeruginosa
was adapted up to 75mM concentration of PDS.
The adapted strains are currently being tested
for their potential ability to remove organic
sulfur from the coal. Adaptation efficiencies of
microorganisms on different concentration of
organosulfur derivatives are depicted in Table-
2.
3.3. Results of bio desulfurization experiment
3.3.1. Removal of pyrite sulfur
Bacterial strain L.ferrooxidans isolated from coal
mines able to remove 51.4 % of pyritic sulfur
from 10% (w/v) feed sample of Meghalaya coal
(size<50mm) in presence of 9K medium at 40oC,
in 3 days.
Table 2: Growth of the bacteria on various
substrates as a sulfur source
Substrate Rhodococcus Pseudomonas
Concentration rhodochrous aeruginosa
DBT PDS DBT
1 mM +++++ ++++ ++++ +++++
10 mM ++++ ++ ++
50 mM ++ + +
75mM ++ - -
+ indic ates extent of growth of bac teria
observed under microscope (1000X).
- indicates absence of growth of bacteria
observed under microscope (1000X).
MPT-2013
3.3.2. Experiment for removal of organic sulfur
Pseudomonas aeruginosa adapted on 75 mM PDS
and Rhodococcus rhodochrous adapted on 75 mM
of DBT were tested to remove organic sulfur
from coal on varying pH in range of 4-7, at 40oC
temperature, 10% (w/v) pulp density.
Pseudomonas aeruginosa was able to remove 52%
of organic sulfur from Meghalaya coal at pH
6.0. Other bacteria Rhodococcus rhodochrous was
also able to remove 51% organic sulfur from
feed coal sample of Meghalaya at pH 6.0. The
result for effect of variation of pH is shown in
Fig.8.
While studying the effect of temperature (30-
45oC), it was clearly seen that Pseudomonas
aeruginosa was able to desulfurize 19%, 36%, 52%,
and 23% of organic sulfur at 30oC, 35oC, 40oC
and 45oC respectively. Whereas, Rhodococcus
rhodochrous was able to desulfurize 23%, 37%,
50.66% and 24% of organic sulfur from 10% (w/
v) Meghalaya coal (size<50mm) at pH 6.0 in 3
days. The result of variation in temperature in
desulfurization illustrated in Fig.9.
Mic roorganisms were also tested for
desulfurization at various pulp densities in
range of 10-30% at 40oC, pH 6.0. Pseudomonas
aeruginosa could remove 52%, 22%, 18.19% of
organic sulfur by using 10gm, 20gm, and 30gm
of coal sample. Whilst Rhodococcus rhodochrous
could desulfurize 50.66%, 29.31%, 26.76% of
organic sulfur from 10gm, 20gm, and 30gm of
Meghalaya coal sample. It showed that as the
pulp density increases, the desulfurization
efficiency decreased. At 10 % pulp density, the
PDS
sulfur removal was maximum by using both
++++ of the microorganisms separately are showed
++
in Fig.10. The final and best optimized results
++
were obtained by using the all bacteria are
showed in Table 3.
291

Fig. 8: Desulfurization of Meghalaya coal
(size<50mm) from 10% (w/v) pulp density at
various pH using PDS adapted Pseudomonas
aeruginosa and DBT adapted Rhodococcus
rhodochrous at 40oC in 3 days
Fig. 9: Desulfurization of Meghalaya coal
(size<50mm) from 10% (w/v) pulp density at
various temperatures using PDS adapted
Pseudomonas aeruginosa and DBT adapted
Rhodococcus rhodochrous in 3 days at pH 6.0
Fig. 10: Desulfurization of Meghalaya coal
(size<50mm) at various pulp densities using
PDS adapted Pseudomonas aeruginosa and DBT
adapted Rhodococcus rhodochrous at 40oC in 3
days at pH 6.0
292
MPT-2013
Table 3: Desulfurization efficiencies of bacteria
for Meghalaya coal
Pyritic sulfur Organic sulfur
MICROOR L.ferrooxidans Pseudomonas aeruginosa Rhodococcus rhodochrous
GANISMS
% of Sulfur 51.4 52 51
removal
4. Conclusions
 Newly isolated strain L.ferrooxidans was able
to desulfurize the coal sample by degrading
the pyrite. This strain was isolated and
grown in acidic medium and the metabolite
produced by this microorganism helps the
medium to keep its pH very low. Acidic
condition favored the breakdown of pyrite
from coal. L.ferrooxidans showed 51.4 % of
pyritic sulfur removal from feed coal
sample (<50m) at 400 C, pH 1.6-1.8 in 3
days.
 Two microorganisms Pseudomonas aeruginosa
and Rhodococcus rhodochrous are already
established for desulfurization of organic
sulfur. Microorganisms were adapted to
high concentration of different organic
sulfur compounds and then used for
desulfurization was different in this
approach. Both microorganisms could
tolerate high concentration of organosulfur
compound and also efficient to remove the
organic sulfur at their optimized condition.
 Pseudomonas aeruginosa adapted in 75mM of
PDS and Rhodococcus rhodochrous adapted in
75mM of DBT were able to remove 52% and
51% of organic sulfur from 10% (w/v)
Meghalaya coal (size<50m) at 400 C, pH-
6. Adaptation in high sulfur compound
showed the efficiency of sulfur removal
from high sulfur coal of Meghalaya.
 Testing the batch optimization studies in
tandem as c ontinuous process could
improve the overall efficiency of sulfur
removal.

Acknowledgements
The authors would like to thank the Ministry
of Steel, Government of India for their financial
support to take up this project.
References
Ali, Abdul., Srivastava, N.K., Srivastava, S.K.,
Goswami, R.N., Yadav, R.S., and Hazra,
S.K., 2009. Upgradation of High Sulfur NE
Region Indian Coals by Pyrolysis in
Presence of Hydrogen. The Open Fuels &
Energy Science Journal, 2, 40-46.
Borah, D., Baruah, M. K., 1999. Electron transfer
process, removal of organic sulfur from
high sulfur Indian coals. Fuel, 78, 1083-
1088.
Fakoussa, M., Hofric hter, R. M., 1999.
Biotechnology and microbiology of coal
degradation. Appl. Microbiol. Biotechnol.
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Gomez. F., Amilis. R. and Marin.I., 1999.
Bioremoval of organic and inorganic sulfur
from coal samples. Appl. Microbiol.
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Izumi, Y., Ohshiro, T., Ogino, H., Hine, Y., and
Shimao, M., 1994. Selective desulfurization
of dibenzothiophene by R. erythropolis D-1.
Appl. Environ. Microbiol. 60, 223–226.
*******
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Kargi, F., and Robinson, J.M., 1982. Removal of
sulfur c ompound from c oal by the
thermophilic organism Sulfolobus
acidocaldorius. Appl. Environ. Microbiol.
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Kilbane, J., September 1994. U.S.Patent
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Klein, J., Beyer, M., Van Afferden, M., Schacht, S.,
1994. Microbial desulfurization of coal and
oil, Fuel Processing Technology. 40, 297-
310.
Monticello, D.J., 1998. Riding the fossil fuel
biodesulfurization wave. CHEMTECH,
28(7), 38-45.
Mukherjee, S., Srivastava, S.K., 2005. Trace
Elements in High-Sulfur Assam Coals
from the Makum Coalfield in the
Northeastern Region of India. Energy &
Fuels, 19(3), 883.
Silverman, M.P., Rogoff, M.H., Wender, I., 1963.
Removal of pyritic sulfur from coal by
microbial action, Fuel, 42,113-124.
Singh, K.P., Naik, A.S., 1997. Coal microscopy as
a tool to understand the beneficiation
problems of Indian Gondwana coals. J. Sci.
Technol., 53-70.
Stevens, Jr. Stanley E., Burgess, Wilella D., July
1989. U.S. Patent 4,851,350.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Washability Curve Versus Mayer’s Curve

Ajit Singh Choudhary 1 , Eshan Tiwari1* and I. Narendra Kumar 2
1
SGS India Pvt. Ltd, 15 C, Hemanta Basu Sarani, LMJ Chambers, 3rd & 4th floor, Kolkata-
700001, West Bengal, India
Email: ajit.choudhary@sgs.com/mremmanuel@gmail.com, Email: eshan.tiwari@sgs.com/
tiwarieshan1990@gmail.com, Mobile – +91-869723934
2
SGS India Pvt. Ltd, C/O Pioneer Paper Plasts Pvt. Ltd, H.O.S- 3/21, SECTOR – A,
Zone -B, Mancheswar Industrial Estate, Bhubaneswar – 751 010, Odisha, India,
Email: narendra.kumar@sgs.com
Abstract
Indian coal has high ash content and low calorific value. Hence, coal preparation is very critical in
Indian scenario. Through coal preparation, a uniform and upgraded product, in terms of carbon
value, can be achieved, which improves the productivity and efficiency in the downstream processes.
The selection of the logical separation process in based upon sink float study on feed coal which is
done at the laboratory scale. Through sink float study, washability characteristics of coal are being
estimated by developing various washability curves. Developing washability curves and other
parameters involves a lot of calculation and are time intensive. Therefore, M-curve is developed as
an alternative which is less time intensive and fewer calculations are involved. Fundamentals of
co-ordinate geometry are required for M-Curve as interpretation from M-curve requires plotting
different straight lines. This paper will discuss a comparative washability study carried out with
the help of both washability curves and M- curve and will provide details of various applications
of M-curve. Washability study for blended coal is also studied with the help of both washability
Curves and M-curve.
Keywords: Coal Preparation; washability; washability curves; m-curve.

1. Introduction in quality. Also as per policy of Coal Ministry of

India, Coal having more than 34 percent ash
The relative abundance of coal in India in
cannot be transported over a distance of 1000
comparison to other fossil fuel make it a natural
km. Also as per the draft notification dated 11
choice as the primary source for fuel, be it for
July, 2012 by Coal Ministry of India in respect of
steel making, power generation or for other use.
use of washed, blended or beneficiated coal in
Indian coal reserves account to 293 billion tonnes
thermal power plants, on and from 1st day of
(as on 31 March 2011). Coal is one of the primary
January 2014, the following coal based thermal
sources of energy, accounting for about 80% of
power plants shall use raw or blended or
the total energy consumption in the country.
washed coal with an ash content not exceeding
Indian coal is of Gondwana origin and is inferior
34 percent and gross calorific value not less than
* Correspending Author: Eshan Tiwari 4000 kcal on daily average basis, namely:-

294

(a) any standalone thermal power plant located
beyond 500km from pit-head;
(b)any captive thermal power plant with
installed capacity of 100 MW or above, and
located beyond 500km from pit-head
(c) any captive power plant above 100MW or
standalone thermal power plant located in
urban area or ecologically sensitive area notified
by Central Government or critically industrially
polluted cluster or area irrespective of its
distance from pit-head expect any pit-head
power plant. Above mentioned draft further
strengthens the critical role of coal preparation
in thermal power industry. Coal is also an
essential input in the production of steel. India
has very limited reserves of coking coal which
is a key raw material for the production of steel.
Coking coal accounts for only 15% of the
country’s overall proven coal reserves. The
Indian steel industry has been facing acute
shortage of coal for the last several years.
Acceptable ash content in steel grade coal is 18%
which is much lower than the ash content of
Indian coking coal. So coal preparation is very
critical for Steel Industry and Thermal Power
Industry. Coal preparation is a technique to
remove undesired inorganic matter from coal
by deploying various separation/up gradation
processes, after communition which is able to
differentiate between the physical and surface
properties of the coal and the gangue. Hence coal
preparation improves the productivity and
efficiency in the downstream processes. The
selection of the logical separation process for
coal preparation is based upon sink float study
on feed coal which is done at the laboratory
scale. Through sink float study, washability
characteristics of coal are being estimated by
developing various washability c urves.
Washability data gives basic information for
equipment/technology selection. Developing
washability curves and other parameters
involves a lot of calculation and are time
intensive. Therefore, Mayer’s curve, which is
less time and calculation intensive, is introduced
as an alternative to washability curves.
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MPT-2013
2. Area description/ materials and methods
2.1. Washability
The washability is the ease of washing of coal. A
series of sink float test is carried out for
generating washability data. The washability
of a given coal sample is then determined with
the help of a series of curves showing the result
of sink float test. These are the curves providing
information about the easiness of washing of
coal. Generally washability curves are used to
determine washability characteristics of a given
coal sample.
Washability Curves composed of following
curves
1. Float/Yield Curve
2. Sink Curve
3. Characteristic Curve
4. Densimetric Curve
5. NGM Curve
With the help of these curves, washability
characteristics of a given sample of coal can be
c alc ulated. Washability c urves provide
information such as yield at a particular density,
yield at a particular ash percent, cut density for
a particular yield and NGM. Washability data
also helps in estimating washability index,
washability number etc. which are indications
of easiness of washing.
2.2. Mayer’s curve
Washability characteristics can also be
determined with the help of M- Curve. M- Curve
is developed as an alternative to washability
curves which is less time intensive and fewer
calc ulations are involved. Mayer ’s Curve
comprises of curve between cumulative weight
percent of float and cumulative weight percent
of ash. M-Curve provides information such as
yield at a particular ash percent, middling ash
etc. M-Curve can also provide information like
yield at a particular density, cut density for a
particular yield and NGM when cumulative
weight percent is plotted against specific gravity.
Fundamentals of co-ordinate geometry are
required for Mayer’s Curve as interpretation
 MPT-2013

from Mayer’s curve requires plotting different 2.2.2. Use of m-curve for the blended coal
straight lines and parallel lines.
For plotting the curve for blended coal and
2.2.1. Construction of the m-curve determining the separation density at which
For plotting M-Curve, the ash content of different two raw coals should be washed, these steps
gravimetric fraction in the sink and float test should be followed:
(Table-1) can be changed to the average ash
1. Connect equal density points on curves of
content of the coal sample to use in the “mean
raw coal samples A and B.
value polygon or M-Curve” (Fig: 1). This change
2. Divide the connected lines according to the
is done graphically or simply through use of
ratio of blending (blending point)
coordinates. The coordinates of different points
3. Connect the point of blending of connected
at the angle of the polygon can be calculated in
lines by a curve that represents the curve
Table-1. In Table-1, columns 1 and 2 present the
for 40:60 mixture of coal A and coal B.
weights (%) and ash content of different
4. Determine the separation density on blended
gravimetric fraction in the sink float tests. The
curve of A and B coals as well as the yield of
entries in column 9 are mathematical products
coal A and coal B at the separation density.
that result when values in column 1 and 2 are
multiplied and then divided by 100. Column 3 2.3. Comaprative study: washability curves
and 10 are cumulative of the values of column 1 versus m-curve
and 9, respectively. Columns 3 and 10 present
2.3.1. Detrmination of washability
coordinates of the angle point of the mean value
characterisitcs
polygon (Fig: 1). Usually, a centimetre scale should
be selected, so 1 cm is equal to 1% ash. When A comparative study is c arried out for
table-1 is constructed, the whole mathematical determining washability characteristics of a
basis for the M-Curve (Fig: 1) is available. given coal sample by washability curves and
Table 1: Washability data for three product M-Curve for a sink float data of a particular
washability studies sample. The aim is to determine washability
1 2 3 4 5 6 7 8 9 10
characteristics of a given coal sample subjected
Sp. Gravity
Sink Float
Differential %
Wt % Ash%
Cum. Float
Wt.% Ash%
Cum. Sink Cum. Float
Wt% Ash% Midpoint
NGM
Ash
wt%
Cum
ash
for three products washing i.e. clean coal,
1.30 0.93 4.79 0.93 4.79 99.07 38.28 0.47 0.04 0.04 middling and rejects. M-Curve (Fig: 1) and
1.30 1.35 7.42 8.14 8.35 7.77 91.65 40.73 4.64 0.60 0.65
1.35 1.40 10.36 12.18 18.71 10.21 81.29 44.36 13.53 39.58 1.26 1.91 washability curves (Fig: 2) are constructed using
1.40 1.45
1.45 1.50
10.91 17.73
10.89 22.72
29.62 12.98
40.51 15.60
70.38 48.49 24.17
59.49 53.21 35.07
39.37
35.09
1.93
2.47
3.84
6.32
given sink float data (Table-1). The desired ash
1.50 1.55 7.21 26.83 47.72 17.30 52.28 56.85 44.12 28.25 1.93 8.25 for clean coal is 20% and that of reject is 75%.
1.55 1.60 6.08 30.82 53.80 18.82 46.20 60.27 50.76 20.89 1.87 10.13
1.60 1.65 4.07 34.97 57.87 19.96 42.13 62.72 55.84 - 1.42 11.55 The yields of individual fractions i.e. clean coal,
1.65 1.70 3.53 40.44 61.40 21.14 38.60 64.76 59.64 13.87 1.43 12.98
1.70 1.80 6.27 46.95 67.67 23.53 32.33 68.21 64.54 13.47 2.94 15.92 middling and rejects and ash content of
1.80 1.90
1.90 2.00
7.20 52.02
4.70 59.05
74.87 26.27
79.57 28.20
25.13 72.85 71.27
20.43 76.02 77.22
11.90
25.13
3.75
2.78
19.67
22.44
middling are determined with the help of both
2.00 20.43 76.02 100.00 37.97 0.00 89.79 15.53 37.97 the curves. The ease of determining washability
characteristics and other parameters like yield,
middling ash are compared for the two curves.

Figure: 1 M-curve for three product washability Figure 2: Washability curve for three product
studies washability studies

296
 MPT-2013

2.3.2 Washability characteristics of blended coal Table 2: Washability data for Coal-A
Coal A
Sp. Gr. Float Cum. Float Cum. Sink Cum. Float Cum.ash
Washability characteristics of sample obtained Sink Float Wt.% Ash% Wt.% Ash% Wt.% Ash% Midpoint
NGM Ash wt%
Wt.%
1.40 11.00 12.72 11.00 12.72 89.00 52.26 5.50 1.40 1.40
from blending of two different coal samples are 1.40 1.50 14.05 27.65 25.05 21.09 74.95 56.88 18.03 32.45 3.89 5.28
1.50 1.60 18.40 37.62 43.45 28.09 56.55 63.15 34.25 24.25 6.92 12.21
also determined by using both washability 1.60 1.70 5.79 44.59 49.30 30.00 50.76 65.27 46.35 17.40 2.58 14.79
11.61 49.48 60.85 33.74 39.15 69.94 55.10 18.90 5.74 20.53
curves and M-Curve. The aim is to compare the 1.70
1.80
1.80
1.90 7.28 57.09 68.20 36.20 31.87 72.88 64.49 13.95 4.16 24.69

washability characteristics provided by both 1.90

2.00
2.00
2.10
6.62
5.09
62.34
68.71
74.80
79.90
38.52
40.44
25.25
20.16
75.64
77.39
71.51
77.35
11.70
8.77
4.12
3.50
28.81
32.31

Washability curves and M-curve . Figure-3 2.10

2.20
2.20 3.73
16.43
71.64
78.81
83.57
100.00
41.86
47.93
16.43 78.70
85.00
81.77
91.79
20.10 2.67
12.95
34.98
47.93

shows the M-curve for two raw coal samples A Table 3: Washability data for Coal-B
and B. These coals were washed separately to a Sp. Gr. Float Cum. Float Cum. Sink Cum. Cum.ash
NGM Ash wt%
required clean coal ash percent (29%) in a Sink Float Wt.%
20.01
Ash%
12.34
Wt.% Ash%
20.01 12.34
Wt.% Ash%
79.99 40.32
Float
10.00 2.47
Wt.%
2.47
1.40
separate washing system. The curves, A and B, 1.40 1.50 25.28 25.40 45.28 19.63 54.72 47.22 32.64 47.76 6.42 8.89
1.50 1.60 22.48 36.03 67.77 25.07 32.23 55.02 56.52 28.92 8.10 16.99
are intersected by reading line at 29% ash. The 1.60 1.70 6.38 42.16 74.20 26.52 25.80 58.31 70.96 14.61 2.69 19.68
1.70 1.80 8.23 49.01 82.37 28.79 17.63 62.48 78.31 12.27 4.03 23.71
intersection point indicates the relative yields 1.80 1.90 4.09 54.34 86.47 30.00 13.53 64.94 84.42 7.99 2.22 25.94
of 46.2% and 83.35%, respectively. With an 1.90
2.00
2.00
2.10
3.90
1.89
60.40
64.96
90.37
92.26
31.31
32.00
9.63
7.74
66.79
67.23
88.42
91.31
5.79
4.19
2.36
1.23
28.29
29.52
assumed mixture ratio of two raw feed coals 2.10 2.20 2.30
5.43
65.80
67.91
94.56
100.00
32.82
34.72
5.44 67.84 93.41
97.28
7.74 1.51
3.69
31.04
34.72
2.20
A:B = 40:60, a total yield of 68.9% can be
Table 4: Washability Data for blended coal
achieved. The separation density and relative
Sp. Gr. Float Cum. Float Cum. Sink Cum. Float Cum.ash
yields of both blended coal determined at ash Sink Float Wt.% Ash% Wt.% Ash% Wt.% Ash% Midpoint
NGM Ash wt%
Wt.%
1.40 16.40 12.44 16.40 12.44 83.60 45.40 8.20 2.04 2.04
point of 29% with the help of M-curve and 1.40 1.50 20.79 26.01 37.19 20.02 62.81 51.84 26.80 41.64 5.41 7.45
washability curve ( Figure 3 and Figure 4) are 1.50
1.60
1.60
1.70
20.85
6.15
36.59
43.07
58.04
64.18
25.98
27.61
41.96
35.82
59.42
62.23
47.61
61.11
27.00
15.72
7.63
2.65
15.08
17.72
shown in table 6. The ease of determining 1.70 1.80 9.58 49.24 73.76 30.42 26.24 66.97 68.97 14.95 4.72 22.44
1.80 1.90 5.37 55.83 79.13 32.14 20.87 69.84 76.45 10.35 3.00 25.44
washability characteristics for blended coal is 1.90 2.00 4.99 61.43 84.12 33.88 15.88 72.48 81.63 8.16 3.06 28.50
2.00 2.10 3.17 67.37 87.29 35.10 12.71 73.75 85.71 6.05 2.14 30.64
compared for both the curves. 2.10 2.20 2.87 68.83 90.17 36.17 9.83 75.19 88.73 12.71 1.98 32.62
2.20 9.83 75.20 100.00 40.01 0.00 95.08 7.39 40.01

3. Results
3.1. Washability characteristics of a given coal
sample
It is evident from the Table-5 results from both
the c urves are in agreement. However,
developing washability curves require more
data and determining washability
c harac teristic s requires more c urves in
comparison to M-curve (Table-7). Moreover,
Figure 3: M-curves for coal A, coal B and middling ash cannot be read directly from
blended coal washability curves but can be calculated.
Table 5: Comparison of washability curves and
M-curve for washability study of a given coal
sample

Results Washability Curves M-Curve

Clean Coal Yield 60.8 60.8
Reject Yield 22.05 21.9
Middling Yield 17.15 17.3
Figure 4: Washability Curve for blended coal Middling Ash 51.02 51.04

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 MPT-2013

3.2. Washability characteristics of blended coal particular coal sample or blended coal sample.
Moreover, M-curve is less calculation intensive
The results shown in table 6 indicate that
and easier to plot whereas plotting washability
washability characteristics determined for
curves is tedious activity and calculation
blended coal from both the curves are in
intensive. M-curve also determines ash percent
agreement. However, washability study for
in middling whic h is not possible with
blended coal involves a lot of data calculation
washability curves. Hence utilising M-curve for
and developing washability curves (for blended
washability studies would be more preferable
coal). On the other hand complete washability
as it is less time consuming and requires fewer
characteristics can be determined with the help
data.
of M-curve which requires fewer curves and
data calculation (table-7). Acknowledgement
Table 6: Comparison of washability curves and The authors are grateful to the SGS management
M-curve for washability study of a blended coal for their encouragement to carry out the work.
sample
References
Results Washability Curves M-Curve Choudhary, A.S., Bhattacharya, S., Kumar, I.N.,
2012. Sink Float Tests of Coal: Sampling and
Clean Coal Yield 69.00 69.05 Washability Data Validation Issues.
International Mineral Processing Congress 2012.
Separation Density 1.63 1.64 Paper no. 240. Page no. 942-951.
Table 7: Comparison between number of curves Habetinejad, Hamidreza., Jorjani, Esmaeil., Sam,
required to predict washability characteristics Abbas., 2011. Evaluation of M-curve validity on
of a given coal sample with the help of feed blending at Zarand Coal Washery plant.
washability curves and M-curve. International Journal of Mining Science and
Washability Curves M-curve Tec hnology 01/2012; DOI:10.1016/
Parameters Curves Required Curves Required
Clean Coal Yield Float Curve M-curve
j.ijmst.2011.07.003
Middling Ash Cannot be directly read but can be calculated M-Curve
Reject Yield Sink Curve M-Curve Ministry of Coal, 2012.Draft notification G.S.R.
Separation density Float Curve, Densimetric Curve M-Curve, Densimetric curve
Boundary Ash Characteristic curve M-Curve
522(E), dated July11, 2012 in respect of use of
washed, blended or beneficiated coal in thermal
power plants for substitution to sub rule 3(8) of
4. Conclusion environment (Protection) Rules, 1986-reg
It is evident from that washability Osborne, D.G., 1988. Coal Preparation
characteristics determined from M-curve is Technology, Vol.1, Graham & Trotman Limited,
always in agreement with those determined London.
from the washability curves whether it is for

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Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Media Stability Issues with Dense Medium Separators

Pankaj Kumar Jain* and S. Bhattacharya

Indian School of Mines, Dhanbad, 826004, Jharkhand, India

Abstract
Heavy medium separation is a special case of gravity concentration in which a heavy media of
specific gravity between the heavier mineral and lighter mineral is used. The heavy material
sinks into the medium and lighter material floats. The effective separation depends on the various
factors such as concentration criterion, liberation, stability of media, type of separator, etc. Stability
of suspension is very important requirement for efficient separation of minerals and coals in close
specific gravity range. Slight change in the density of the media can lead to inefficiencies resulting
in poor separation of heavy material from the lighter ones thus degrading the grade of the final
product.
The stable composition of suspension is needed to ensure high accuracy heavy medium systems.
Preparation of ultralow-ash coal needs two stage similar density separations, it is necessary to
reduce the suspension condense in cyclone. Factors which affect suspension condense include:
centrifugal factor, suspension concentration, the density and size of heavy media. Various measures
are adopted to maintain the stability of the suspension of the solids. Size of the suspension particles
plays an important role in the stability. Present paper aims at covering various factors affecting
the stability of suspensions. Defining various terms such as stability, critical volumetric
concentration, limiting concentration, stability index, etc. Issues related to magnetite media,
ferrosilicon and other mediums will be discussed. The extent of variation of the density of a fairly
stable medium in different static and dynamic separators will be discussed. Effect of various
contaminants on the stability of the suspension. Various methods adopted at industry for
maintaining the suspension stable.

Keywords: Heavy medium separation; dense medium separation; media stability; stability of
suspension; heavy media; dense media; media stability issues.

light mineral is used. The heavy material sinks

1. Introduction
Dense media separation is a special case of
gravity concentration in which dense media of
relative density between the heavy mineral and
* Correspending Author: Pankaj Kumar Jain, Assistant
professor, Department of Fuel and Mineral Engineering,
Indian School of Mines, Dhanbad 826004, Contact: 0326
22 3 5 094 (O), Mo bile: +9 1-7 766 904 994 , Email:
pankaj.k.jain@live.com
into the medium and light material floats.
The importance of dense media separation has
increased significantly in last two decades,
reason being the need for sharp, efficient and
easy to control system to meet the demand for
high quality clean coal. Heavy media bath
handles coarse coal (+10mm) while cyclone
handles fines (-50 +0.5mm). Most of the plant
uses dense medium cyclone for +0.5mm coal

299

because of fines separation efficiency. Now a
days, plants are also striving to go for +0.1 mm
coal beneficiation with dense medium cyclones.
There are several difficulties encountered
during the plant operations in such cases.
(Mikhail and Osborne, 1990)
The primary objec tive of dense media
separation is the sharpness of separation (Ep)
which in general terms depends upon the
hydrodynamic properties of materials to be
separated under operational conditions and the
rheological properties of the suspension under
operational conditions. For a given coal with
fixed – size, density, density of separation and
for a given operating conditions the sharpness
of separation (Ep) will depend upon- 1) the
effective viscosity of suspension, žE, which is
the viscosity experienced by the ore particles,
2) the yield stress, qs, of the suspension which
ideally should be as low as possible, and 3) the
stability of the suspension, So, which should be
as high as possible. Stability is defined as the
inverse of the settling rate for a suspension and
has units of sm-1. (Burt, 1984)
Out of above mentioned parameters, stability
of suspension is the most important factor to
keep under control since it determines the
density gradient of the medium in the
separation zone and thus directly influences the
separation sharpness. High medium stability
is favoured by ore fines, fine medium particles
and high medium densities. The present paper
aims to cover dense medium (magnetite and
ferrosilic on) stability related issues and
important findings from the literature.
2. Definition of Some of the Basic Terminology
and Their Importance
There are many of the important terms which
have been used in this paper and a better
understanding to the importance of these can
be established if the definition and importance
of each of them is known. These terms include
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stability of suspension, critical volumetric
c onc entration, limiting c onc entration,
viscosity, stability index, rheology, sharpness
of separation, dilatant liquid etc.
The term stability of suspension is defined in
various ways by different authors. Stability,
So, is defined as the inverse of settling rate of the
supernatant – suspension interface (mud line) with time
and has the units of sm-1. (Burt, 1984) It is a measure
of the ability of the suspensions to remain
homogeneous with respect to medium density;
it has also been defined as the degree of
stratification of particles in the separator
(Graham and Lamb, 1982).
The term critical volumetric concentration
(CVC) refers to the medium volume concentration
(critical concentration) above which the apparent
viscosity increases rapidly even for a small increase in
the suspension density. When the viscosity of the
medium suspension becomes very high it
inhibits the movement of particles in it and the
medium does not remain fit for separation. This
critical limit of volumetric concentration can
be extended to certain extent with the external
aid of such as vibration and agitation of the
media, but beyond certain limit of volumetric
concentration this external aid also does not
remain useful. This is known as limiting
concentration,i.e., the volumetric concentration above
which a suspension cannot be suitable for use as a media
for separation even with the aid of external factors such
as vibration and agitation. (Burt, 1984)
Viscosityof a fluid is a measure of its resistance
to gradual deformationby shear stress or tensile
stress. A fluid is said to be Newtonian-fluid if the
“viscous stress” that arises from its flow, at
every point, are proportional to local strain rate,
i.e. the rate of change of strain (deformation)
with respect to time. A fluid is said to be non-
Newtonian fluid if the viscosity is dependent on
shear rate, i.e. the rate at which progressive
shearing deformation is applied to some
material. (Wikipedia)

Stability index or stability F5 index, also known
as the measure of stability of suspensions, is
defined as the ratio of the weight of the
suspension between the first two tapping
points and the weight of the suspension below
the third tapping point, on the standard
apparatus under standard conditions. (Mikhail
and Osborne, 1990)
Rheology is the study of deformation and flow
of matter. Suspension rheology refers to the
deformation and flow of suspension. The
rheological properties of suspension such as
yield stress, effective viscosity and stability can
be inherent or acquired and influence the
hydrodynamics of particles to be separated and
hence influence the sharpness of separation.
(Wikipedia)(Burt, 1984)
Sharpness of separation (Ep) is generally
indicated by the tromp curve and is a measure
of misplacement of near gravity material at the
specified cut density in the washer. It is also
known as the probable error which is likely to
occur during the separation of material in the
dense media as result of misplacement, i.e. the
amount of float material reporting to sink and
vice versa.
A dilatant (also known as shear thickening)
material is the one in which viscosity increases
with the rate of shear strain. A dilatant fluid is
a non-Newtonian fluid in which the shear
viscosity increases with applied shear stress.
It is controlled by factors such as particle size,
shape and distribution. (Wikipedia)
3. Rheology and Dense Medium Separation
There are several factors which affect the
rheology of dense medium separation. These
factors can be categorised for simplification.
(Burt, 1984)
3.1. Feed Characteristics based factors which
influence rheology
- Liberation size and size range of the feed,
the density difference between the minerals
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and the theoretic al density of
separation;these influence hydrological
properties of the partic les and hence
sharpness of separation and capacity of
equipment
- The separation density; it fixes the volume
concentration of media solids making up
the suspension, which cannot be altered to
improve the stability. The variable with the
operator in such case are limited i.e. mainly
the size, contaminant such as slimes etc.
- Size, amount & mineralogy of products of
ore under processing. These products
remain in Dense Media after washing and
influence its rheology
- Both adhesive properties of medium to
separation products and retention of ore
fines in dense media separation circuit;
influence medium loss and contamination.
3.2. Operational factors which influence
hydrodynamics of particles and rheology
of suspension
o The rate of shear due to flow and
agitation of suspension
o Method and rate of feeding
o Method of product discharge
o The applied field of force (gravitational
and centrifugal)
3.3. Physical and mineralogical characteristics
of medium (magnetite) which influence
suspension rheology, medium recovery
and product contamination
o Size
o Shape
o Size distribution
o Density of medium
3.4 Physical properties of medium which
influence rheology of suspension and
recovery of medium (magnetite)
- Surface energy; it quantifies the disruption
of intermolecular bonds that occur when a
surface is created or it can also be said that

total amount of energy required to create a new
surfac e is known as surfac e energy.
(Wikipedia)
- Permeability; it is the measure of ability of
material to transmit fluid.
- Coercivity; the resistance of a magnetic
material to changes in magnetization,
equivalent to field intensity necessary to
demagnetize the fully magnetized material.
Or in simple terms it can be stated as, for
ferromagnetic material the Coercivity is the
intensity of the applied magnetic field
required to reduce the magnetization of
that material to zero after the
magnetization of the sample has been
driven to saturation.
3.5. Chemical properties of the Medium
(magnetite)
- Degree of oxidation
- Degree of hydration
3.6. Physico-mechanical parameters which
control rheological properties of magnetite
dense media
- Solids content
- Particle size
- Particle size distribution
- Particle roughness and shape
3.7. Physico-chemical parameters which
control rheological properties of magnetite
dense medium
- pH and Dissolved Ions
- Dispersing agents
- Magnetization
4. Rheological Properties of Dense Medium
There are three inherent and ac quired
rheological properties of the suspension under
operational conditions:
4.1 Yield Stress
4.2 Effective viscosity
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4.3 Stability
For a given ore with fixed – size, density, density
of separation & for a given operating conditions,
the sharpness of separation (Ep) also depend
on above rheological properties.
5. Issues Related to Media Loss and its
Recovery
Normal method of medium recovery is by
intense water washing of separator products
on vibrating screens followed by low intensity
wet drum magnetic separation (wet LIMS) of
combined ‘product screen undersize’.
5.1. Reason for loss of media:
As the particle size of ores treated by dense
medium separation decreases, wet screening
must be conducted at increasingly finer sizes
and this leads to the increased difficulty of
making a product / medium separation, which
results inc reased medium losses to
product.(Burt, 1984)
Magnetic fineness usually increases magnetic
separation efficiency but since finer particles
are more difficult to recover, it may lead to
higher losses. If the treated coal is very fine, e.g.
covers large proportion of -3.0mm + 0.5mm
fraction and considerable misplacement of fines
(-0.5mm) in the feed, in that case, increased
surface area of fine coal particles increases the
amount of magnetite attached to coal particles,
which is difficult to rinse off. Lower the level of
magnetic content, higher is the loss of magnetite
per tonne of raw coal treated. Magnetic
property of magnetite is not a rheological
property but it influences the rheology and
stability of the magnetic slurry (Mikhail and
Osborne, 1990).
5.2. Reason for difficulty in medium recovery
Also as the particle size of the medium is
decreased to improve suspension rheological
properties, so the difficulty of recovering clean
medium by magnetic separation increases. For

better recovery two or three stage magnetic
separation may be required. Still ultra-fines are
preferentially lost.
5.3. The two important process controlling
economic factors because of medium losses
are
o Screening: rinsing of media is done over the
screen. If not rinsed properly it is lost.
o Magnetic separation: Recovery of magnetite
contents for recirculation to the circuit.
6. Measurement of Stability of A Dense
Media:
6.1. F5 Index stability method
This method was developed by National
Institute for Coal Research (NCIR), South Africa.
The apparatus used is copper tube with an
overall length of 1.225m. It includes three
tapping points. After five minutes of settling,
the medium between tapping points 1 & 2 (A)
is run off and weighed. After discharging the
medium between tapping points 2 & 3, the
remaining medium in the tube is weighed (B).
The ratio of A & B gives F5 Index also known as
stability index. (Mikhail and Osborne, 1990)
6.2. Jar settling test
The demagnetized sample is mixed with
distilled water (with added wetting agent) in a
500ml calibrated cylinders. The relationship
between the height and time produces the
settling rate. The slope obtained during the free
settling zone represents the settling rate in mm/
min with typical rates of 10-20 mm/min.
(Mikhail and Osborne, 1990)
6.3. Standard practice for stability:
Suspension is agitated and then allowed to
settle under gravity. During settling the rate of
descent of the suspension/ clean water interface
(mudline) is measured (ms-1). The inverse of this
settling rate, (sm-1) is the stability. (Burt, 1984)
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7. Stability of Magnetite Dense
Media(Bernhard Klein, 1985)
The medium stability is the most important
parameter that influences the performance of
both static and dynamic dense medium
separators. Stability has been defined in the
previous section. Gravitational and centrifugal
acceleration causes media particles to settle and
segregate, c reating a non-homogeneous
environment.
Both physic o-mec hanic al and Physic o-
chemical parameters affect settling properties
of dense media. Magnetite dense medium is a
concentrated poly-disperse suspension of
interacting, irregularly shaped particles. Brief
and general specifications for dense medium
magnetite, based on British Coal Mining
Industry Standards and accepted world-wide
are: ((Mikhail and Osborne, 1990)
a) Particle Size Distribution: Maximum 5% by
mass larger than 45µm and 30% by mass
smaller than 10µm.
b) Relative Density: 4.9 to 5.2 g/cm3
c) Magnetic content: Not less than 95% by
mass
It is also usually required that the magnetite
moisture content be less than 10%.
The remnant magnetism exhibited by magnetic
particles as well as colloidal forces, may affect
media stability via formation of aggregates. In
order to control it, demagnetization is preferred
after magnetic separation in the magnetite
recovery circuit.
7.1. Settling in suspensions
The settling in suspension depends on same
physico-mechanical and physicochemical
parameters that influence the rheological
properties.
Stokes equation is applied for settling rate of
non-interacting, spherical particles in a dilute
(solids c ontent less than few perc ent)
suspensions at low Reynolds numbers, given
by

This equation shows the relationship between
settling velocity, v, and particle size, d, particle
density, , fluid density, , acceleration due
to gravity, g, and fluid viscosity, ç.
Steinour (1944) considered that with increasing
solids concentration, the particle settling
velocity is lower than predicted by Stoke’s
equation due to hindering effects which include:
I. partic le-partic le c ollisions c ausing
particles to lose momentum and,
II. hydrostatic pressure c aused by the
upward flowing fluid that is displaced by
the settling particles (Richardson and Zaki,
1954, Garside and Al-Dibouni 1977,
Zimmels, 1985)
For prediction of settling rates under such
conditions, an equation is given by Zimmels
(1985) that is also an extension of Stoke’s
equation as follows:
Where, Ø is the solids volume fraction, and
n is a multiple of the gravitational acceleration.
For poly-disperse systems, large particles settle
faster than small ones; this leads to differential
settling. The amount of differential settling also
depends upon solids content in the suspension.
At intermediate concentration, large particle
displace small ones along with the fluid; the
result is a reduced or even a negative settling
velocity for small particles. In addition, the
small particles and fluid provide “carrier ”
properties to large particles thereby hindering
their settling. These carrier properties have
been explained with the help of buoyancy and
viscosity exerted by the suspension of smaller
ones. (selim et al, 1983, Williams and
Amarasinghe, 1989). At high solids
concentration, these hindering effects prevent
differential settling and he suspension settles
with constant composition (Williams and
Amarasinghe, 1989).
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A concentrated poly-disperse suspension
settling in a column forms four distinct zones
(Greenspan and Ungarish, 1982). As the
particles settle, a supernatant will form a top
of the column. This region extends vertically to
the position of smallest settling particle that
was originally at the top of the column. Below
this position is a transition region, which is
characterized by an increasing particle size
with depth. This region also has an increasing
solids c onc entration with depth. Below
transition region is a constant density zone,
which has a solids concentration and size
distribution approximately equal to that of
original suspension. Immediately below this
zone is a consolidation zone in which the
settling particles form a sediment. With
increasing solids concentration, the transition zone will
diminish in size such that at high solids content it will
not exist.
7.2.Settling properties of magnetic dense
media
The effec ts of the physic o-mec hanic al
parameters (solids concentration, particle size
and particle density), the physicochemical
parameters (magnetization and dispersants)
and of fine contaminating particles (coal fines
and clays) on stability of magnetite dense
media have been c onsidered in several
publications. However, data on the effects of
particle size distribution, particle shape, pH or
dissolved ions are not available.
In particular, at low solids concentrations, large
partic les settle faster than smaller ones
resulting in differential settling and poor
medium stability properties. (Berghofer, 1959).
For low medium densities it has been shown
that fine grades of magnetite provides greater
stability (DeVaney and Shelton, 1940). Fine size
grades (95% -45µm) are recommended for low
density separations (1200-1500 kg m-3), while
coarser grades (95% -53µm) can be used at high

densities (1400-2000 kg m -3) (Graham and
Lamb, 1988).
As mentioned earlier, the remnant magnetism
in magnetite partic les may result in the
formation of aggregates. This magnetic
aggregation increases the settling rate of the
medium. The effect of aggregation depends on
the strength of the magnetic force which is
specific to the sample. The effect of magnetic
aggregation on the medium stability in
dynamic separators is not c lear. Some
investigators believe that dynamic separator
will break up the aggregates and reduce such
effects. Graham and Lamb, 1988, found that
shearing a suspension of magnetic ally
aggregated partic les had little effec t on
subsequent settling results and concluded that
either shearing did not break the aggregates or
the aggregates quickly reformed. Therefore it is
highly recommended to install a demagnetizing
coil after magnetic separation in dynamic
process.
The effect of variety of dispersing agents on
medium settling properties shows that they did
not significantly influence the stability of pure
suspensions. They have, however, been shown
to affect significantly the settling properties of
the dense medium containing clays. Aplan and
Spedden (1964) found that sodium
hexametaphposphate was effec tive in
dispersing clay which lowered the structure
and resulted in higher settling rates. The
dispersant reduce the medium viscosity. Since
clays such as bentonite and kaolinite can be
added to dense medium to improve stability,
the addition of dispersing agents can be used to
control their effects on medium viscosity.
8. Stability of Ferrosilicon Dense Medium
Suspensions
Ferrosilic on is used for high density
applications (medium density: 3200-4200 kg m-
3
). A ferrosilicon suspension must have large
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fraction of solids in water to achieve high
densities. The rheology of ferrosilic on
suspension c an be best desc ribed by its
visc osity and stability. The visc ous
characteristics of dense medium are generally
non-Newtonian and the term apparent
viscosity (at defined shear rate) is preferred to
describe it. An ideal medium has low viscosity
to maximise separation and pump efficiency. A
higher viscosity is undesirable as it reduces the
veloc ity of the mineral partic les being
separated, inc reasing the c hanc e of
misplacement and reducing the separation
efficiency. A low viscosity is typically obtained
for a low medium density, coarse particles,
smooth rounded partic les, and c lean
uncontaminated medium.
Ferrosilicon is an alloy if iron and silicon, with
a specific gravity of 6.8-6.9, is widely accepted
as most suitable medium for ore separations in
the range of 2.5 to 4.0 Kg L-1. Ferrosilicon
contains silicon in the range of 14 to 16 % to
have the optimum combination of properties.
If the silicon content is lower than 14 %, then
the specific gravity and magnetic properties are
improved, but resistance to corrosion decreases
rapidly. On the other hand, above 16% corrosion
properties are not significantly improved, but
the magnetic properties and specific gravity
deteriorates. (Collins et al. 1974).
The shape of ferrosilicon particles depends on
the manufac turing proc ess. There are
essentially two forms of ferrosilicon available;
milled and atomised. Production methodology
for both types are different.
Production method of milled ferrosilicon is to melt
steel scrap, quartz & a reductant is submerged
into a sand-bed, allowed to cool and then
broken into lumps. After which it is crushed in
two stages and milled to required size range.
While, for atomised ferrosilicon, the molten alloy
from the furnace is steam atomised and water
quenched. Atomised ferrosilicon consist largely
of round particles & results in lower viscosity

pulps; permitting higher separation densities
to be obtained.
The limiting density of milled ferrosilicon is 3.3
kg L-1, whilst that of atomised ferrosilicon can
be as high as 3.9 Kg L-1 (Voges, 1975). Ferrosilicon
can be mixed with magnetite for lower density
separation in the range of 2.2 to 2.9 Kg L-1.
Corrosion of ferrosilicon can cause high losses
and degradation of the medium which leads to
increased viscosity. However, few investigator
consider this drawback as advantage when
pure ferrosilicon is used, since the slowly
degrading ferrosilicon makes up for the fine
medium particles lost in tailings of magnetic
separation, thus avoiding the need for addition
of fresh fine media solids. But Chasten (1973),
noted that harder ferrosilicon abrades softer
magnetite, causing more medium loss. The
addition of a mixture of borax and sodium
nitrate to the medium, does, however
essentially overcome the corrosion problem.
Although atomised ferrosilicon is considered
more expensive than milled ferrosilicon, its
higher density and lower viscosity can result
in a more effic ient operation with lower
medium losses.
Stability is related to rheology of solid phase in
an environment constituted by liquid phase.
The relative movement of solids in liquid phase
under mass and surface forces determines the
degree of homogeneity of suspension. The
medium stability determines the density
gradient of the medium in the separation zone
and thus directly influences the separation
sharpness. An ideal medium density has a high
stability, which results from high medium
densities, fine medium particles, irregularly
shaped particles and presence of low density
contamination (clay/ ore slimes).
9. Conclusions
For obtaining sharp separation of minerals and
coal using dense media separation it is very
important to maintain the stability of media
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MPT-2013
(magnetite and ferrosilicon). Detailed study
needs to be carried out with generation of
sufficient data on the effects of particle size
distribution, particle shape, pH or dissolved
ions. To achieve good stability and rheological
properties in dense media, it is recommended
to use fine magnetite for low media densities
and large particles for high media densities.
More detailed information concerning particle
interaction effect may assist in determining
optimum particle sizes for specific media
densities.
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sedimentation behaviour of concentrated
polydisperse suspensions”, Trans IMM,
C68-C82.
Zimmels, Y., 1985, “Accelerated and steady
particle Flows in Newtonian Fluids”,
Encycl. Of Fluid Mech., 5, Cheremisinoff,
N.P. (Ed), Gulf Publ. Col, Housten, 94-153.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Application of Native Microbes for Biodesulphurization of North

East High Sulphur Coal

S. Mishra*, P. P. Panda, N. Pradhan, D. Satapathy, S. K. Biswal and B.K.

Mishra
CSIR-Institute of Minerals and Materials Technology, Bhubaneswar 751013, India.
Abstract
Coal has served as a central source of energy for centuries now. But recently, the reduction of
sulphur from coal is befitting as an essential aspect for several coal industries due to the stringent
new regulations by government and the various environmental issues associated with sulphur
emissions. Sulphur in coal occurs in the form of pyritic sulphur, sulphate sulphur and organic
sulphur. The inefficacy of physicochemical techniques for removal of organic sulphur from coal
has motivated the researchers to investigate the biological methods of sulphur removal. Indian
coal from North eastern region of India contains significant amount of sulphur.
In the present study, microbial species isolated from various soil and water samples collected
from Margherita coal mines in Assam state of India (North-east) were examined for coal
biodesulphurization. Enrichment of the isolated strains in MSM (Mineral Salt Media) media
containing 0.5mM Dibenzothiophene demonstrated the tolerance ability and faster growth of
certain strains over other microbial species. These selected strains were used for coal
biodesulphurization and it was observed that some pure cultures of bacteria were capable of
removing up to 30-34% of sulphur from Meghalaya coal using MSM media with pH 6.5±7. Sequential
leaching of the Meghalaya coal sample with one of the isolated strain Sinomonas flava 1C followed
by Acidithiobacillus ferroxidans further enhanced the biodesulphurization efficiency resulting in a
removal of 50% of total sulphur from Meghalaya coal.

Keywords: Coal, Biodesulphurization, Organic sulphur, Sinomonas flava, Acidithiobacillus ferrooxidans

1. Introduction various economic and environmental aspects,

Coal is vital sourc e of energy due to its
abundance and cost effectiveness. But, SOx
emissions concomitant with coal combustion
have been a major disadvantage for
environmental concerns. Considering the
* Correspending Author: Sraba ni Mishra , PA-II,
Bioresources Engineering Department, CSIR-Institute of
Minerals and Materials Technology, Bhubaneswar, 751013,
Odisha, India. Email: srabani_seema@yahoo.co.in
recently, mic robial approac h for sulphur
removal from coal is attaining momentum (Achi
1994, Acharaya et al 2005, Pandey et al 2005,
Acharya et al 2004, Afferden et al 1993). Physical
methods have been successfully used for the
removal of pyrite sulphur from coal. However,
the organic sulphur portion present in coal is
recalcitrant to physical methods of sulphur
removal. Use of chemical methods for removal

308

of organic sulphur from coal requires high
temperature and pressure conditions. Such
methods are deficient in selectively and unable
to preserve the calorific value of coal.
The organic sulphur portion of coal is made up
from various thiophenes, benzothiphenes,
thiols sulphides, disulphides and about 70% as
dibenzothiophene whic h is rec alc itrant.
Dibenzothiophene is finely distributed in the
c oal matrix and requires more invasive
techniques for its removal from coal. In the
present study, native microbial species were
investigated for the removal of sulphur from
coal. Coal from Meghalaya region of North
Eastern India have high sulphur content and
selected for desulphurization purpose. All the
native microbial strains were screened for
dibenzothiophene degradation and the efficient
strains were further employed for c oal
desulphurization. Various process parameters
were optimized for carrying desulphurization
experiments and both bacterial and fungal
species were used to remove sulphur from coal.
2. Materials and Methods
2.1. Coal sample
Coal sample was collected from Meghalaya Coal
mine situated in North-eastern region of India.
The coal was grinded and sieved to obtain
different size fractions. The size fractions used
in the present study were (a) -1mm + 850 ìm (b)
– 500 ìm + 300 ìm, and (c) -150 ìm.
2.2. Isolation and screening of efficient
microbes
Water and soil samples were collected from
various coal contaminated sites of Marghetteta
coal mines. Enrichment of microbes was carried
out using dibenzothiophene as the sole sulphur
and carbon source in MSM media (Mineral Salt
Media) composition. One of the isolate,
identified as Sinomonas flava 1C, showing
maximum desulphurization capabilities was
selected for further study.
309
MPT-2013
2.3. Two-step sequential leaching
After optimization studies, Meghalaya coal
were subjected to microbial desulphurization
in an innovative two-step sequential leaching
method in order enhance desulphurization
from the coal sample. The same size fractions
used during the preliminary optimization
studies were subjected to a two-step sequential
microbial treatment. In the first step, the coal
sample was treated with bacterial isolate
Sinomonas flava 1C for removal of organic sulfur.
About 30 g of coal was added to 600 ml of MSM
media at 5% (w/v) pulp density in 1 L flasks.
After inoculation with 10% (v/v) of overnight
grown bac terial culture, the flasks were
incubated at 35 oC, 150 rpm in an orbital shaker.
The initial pH of the medium was maintained
at 6.9±0.2. After 7 days, the coal was recovered
by filtration. The second step involved the
sequential microbial treatment of the same coal
sample used in the first step using A. ferrooxidans
strain for the removal of pyritic sulphur. For
the growth of A. ferrooxidans, 9K + medium
containing 3 g/l (NH4)2SO4, 0.1 g/l KCl, 0.5 g/l
MgSO 4.7H 2O, 0.5 g/l KH 2PO 4 and 44.2 g/l
FeSO4.7H2O was used (Silverman et al., 1959).
For this experiment, the biodesulphurized coal
from the first step was added to 600 ml of 9K-
medium (9K media without ferrous sulphate)
inoculated with active A. ferrooxidans culture
(10% v/v), incubated at 35oC and 150 rpm. The
pH of the medium was maintained at 1.8±0.1.
After 7 days, the coal samples were recovered
by filtration and dried prior to analysis of
sulphur.
Fig. 1: Two-step sequential leaching using
bacteria 1C and A.ferrooxidans

2.4. Sulphur analysis
The total sulphur content of the original coal
and microbially processed coal samples were
estimated by TRUSPEC CHNS analyser by
LECO corporation, USA. The chemical nature
(pyrite and sulpahte) of the sulphur present in
the original and microbially processed coal
sample were analysed using wet chemical
analysis by using standard proc edure
mentioned in BIS-1350 (part- III). The sulphur
content of coal in organic form was calculated
by deducting the inorganic fraction (pyritic and
sulphate sulphur) of sulphur from total sulphur
of coal.
3. Result and Discussion
3.1. Composition of Meghalaya coal sample
Table 1: Meghalaya coal characteristics
Meghalaya Coal
Ash
Fixed Carbon
Moisture
Proximate analysis
Volatile
Gross calorific value
(cal/g)
Total ( S T)
Organic (S O)
Sulphur
distribution Pyritic (SP)
Sulphate (SS)
North eastern states of India comprises of coal
having low ash content with high volatile
content, higher calorific values and high
sulphur. The proximate analysis for Meghalaya
coal has been shown in Table 1, which display
a low ash, high volatile matter and high sulphur
composition. The total sulphur content was
analyzed and found to be 6.17% ((Organic- 4.7
% + Pyritic- 0.35 % + sulphate sulphur- 1.12 %).
3.2. Sequential leaching: organic and pyritic
sulphur removal
MPT-2013
Under optimum c onditions, a maximum
desulphurization of 38% was achieved with
S.flava 1C from the finest particle size of -150
µm. Since, S. flava 1C is a chemoorganotrophic
bacteria, it mainly attacks the organic sulphur
part of the coal. Therefore, under optimum
conditions about 40 % of the ‘S’ was removed
which may be due to the removal of organic
sulphur present on surface of the coal particles.
Since coal is a solid particle, the bacterium is
unable to penetrate beyond a certain limit
depending upon the porosity and surface area
of the material. In order to achieve enhanced
desulphurization, a two-step sequential
biodesulphurization method was investigated
where S. flava 1C was used to remove organic
sulphur followed by pyritic sulphur removal
using A. ferrooxidans. The bacteria A. ferrooxidans
is a chemolithotrophic bacterium adept in
growing on pyrite as energy source.
7.7 Results of the study indicated that size fractions
37.9 of -500 +300 µm and -150 µm were much
6.53
amenable towards enhanced desulphurization
47.87
(Table 2). During the first step of
biodesulphurization, about 40% and 41%
6261
sulphur could be removed from -500 +300 µm
6.17 and -150 µm size fractions respectively using
4.7 S. flava 1C. In addition, 17% and 19 % pyritic
0.35
sulphur could be removed in the subsequent
1.12
stage upon treatment with A. ferrooxidans from
the same -500 +300 µm and -150 µm size
fractions respectively. Collectively, a total of
50% and 53 % sulphur removal was achieved
from the -500 +300 µm and -150 µm size
fractions of Meghalaya coal by the sequential
treatment of S. flava1C and A. ferrooxidans.
However, desulphurization from the -1 mm
+850 µm size fraction was significantly lesser
as compared to the other lower size fraction
under study. (Table 2). Sulphur removal during
the 1st and 2nd step were 13% and 6%
respectively. In total, 18% sulphur removal was
achieved from the -1 mm +850 µm size fraction.
310
 MPT-2013

It was therefore c lear that the two step- from the acidic pH of 2.0 ( used for growth of A.
sequential biodesulphurization method using ferrooxidans).
native bac terial isolate S.flava 1C and Table 3: Coal composition analysis of original
A.ferrooxidans is beneficial towards enhanced and microbially desulphurized coal samples
desulphurization from the coal sample.
Sulphur in coal Original Sulphur in treated coal with ‘S’ ‘S’ Removal %
Table 2: Effect of Sequential Leaching on (%) Coal S. flava 1C S. flava 1C+Af Removal / from total sulphur
microbial desulphurization of coal (conditions Total (ST) 6.17 3.69 3.09 3.08 50
Organic (SO) 4.7 3.04 2.57 2.13 35
- incubation time 6 days; pulp density 5%) Pyritic (SP) 0.35 0.35 0.25 0.1 1.6
Sulphate (SS) 1.12 0.3 0.27 0.85 13.7

Initial
Sulphur content after treatment Table 4: Detailed comparison of original and
Size S. flava1C A. ferrooxidans Total S
fraction
Sulphur
After %S Before After %S Removal microbially desulphurized coal samples
%
Leaching Removal Leaching Leaching removal
-1 mm, % (W/W)
6.9 6.00 13 6.00 5.64 6 18.26
+850 µm Treated coal
Components Original
-500 +300 S. flava 1C+
6.17 3.69 40 3.69 3.08 16.5 50.05 coal S. flava 1C
µm A. ferroxidans
-150 µm 6.8 4.01 41 4.01 3.24 19 53 Proximate analysis of original and treated coal
Ash 7.7 7.43 3.18
Fixed Carbon 37.9 38.95 37.66
3.3. Effect of microbial desulphurization on Moisture 6.53 4.95 4.71
coal characteristics Volatile 47.87 48.67 54.45

Gross calorific value (J/g) 26,208 27,317 29,481

The XRD and wet chemical analysis of the coal
Ultimate analysis of coal on dry mineral matter free (d.m.m.f) basis
confirmed that sulphur in coal exists in both Carbon 77.86 79.55 80.22

organic and pyritic (inorganic ) form. Hydrogen 3.82 4.23 4.61

Biodesulphurization process was effective Nitrogen 1.54 1.52 1.43

towards removal of both organic and pyritic Sulphur 5.52 3.49 2.79

form of sulphur from the coal, whic h is Oxygen 11.26 11.21 10.95

attributed to the heterotrophic and

chemolithoautotrophic mode of nutrition of the
microbial species. It is clear from Table 3 that
treatment with S. flava 1C did not affect pyritic
sulphur, however both organic and sulphate
sulphur were removed. On comparison of K
Q,C
a.u .

proximate analysis of original, S. flava 1C and C1 bacteria

P
A. ferroxidans treated coal valuable information
P Q
were obtained (Table 4). Ash content of 7.7% in P P
Q
C1+ A ferrooxidans

Q
the original sample had marginally reduced Original Meghalaya Coal

upon S. flava 1C treatment to 7.13%, indicating 10 20 30 40

2Q
50 60 70 80

that only organic sulphur was attacked.

Moreover, after subsequent treatment with A.
Fig. 4: X-ray diffraction analysis of coal; K-
ferroxidans the ash content further reduced to
Kaolinite, Q- Quartz, P- Pyrite, C- Quartz carbon
3.18%, which is approximately 50% of the
original. The decrease in ash content observed 4. Conclusions
in the second stage may be due to loss of pyritic
sulphur as well as some kaolinite minerals Meghalaya coal is a high grade coal with low
(supported by XRD as shown in Fig. 2) resulting ash content but presence of high sulphur poses

311

environmental threat. After reduc tion of
sulphur the coal may be used for various
applications. A native bacteria isolated from
high sulphur coal mines and identified as S. flava
1C was capable of removing about 40 % of
sulphur from coal sample bearing 6.17 % total
Sulphur. A sequential leaching with S. flava 1C
and A. ferrooxidans was capable of removing
about 50 % of sulphur under optimum condition
decreasing the total sulphur content of coal to
about 3.09 %. In the present study calorific
value of coal increased from 26,208 J/g to 29,481
J/g which shows that coal energy value is not
adversely affec ted by the process. It is
important to achieve high sulphur reduction
keeping intact the combustion parameters.
Thus biodesulphurization with bacteria S.flava
1C and A. ferrooxidans may be used for removal
of sulphur from high sulphur Meghalaya coal.
A biotec hnologic al solution for
desulphurization of coal would lead to a green
technology with least environmental pollution
and availability of low ash -low sulphur coal.
Acknowledgement
Authors are thankful to Ministry of Steel,
Government of India for financial support
*******
312
MPT-2013
(Project GAP-220). Authors are also grateful to
their respective Head of Departments for their
cooperation and permission to carry out the
study.
References
Acharya, C. Sukla, L. B., Misra, V. N., 2005.
Biological elimination of sulphur from
high sulphur coal by Aspergillus-like fungi.
Fuel. 84, 1597-1600.
Acharya, C., Sukla, L. B., Misra, V. N., 2004.
Review: Biodepyritisation of coal. J. Chem.
Technol. Biotechnol. 79, 1-12.
Achi, O. K., 1994. Growth and coal solubilizing
activity of Penicillium simplicissimum on coal
related aromatic compounds. Bioresour
Technol. 48, 53-57.
Afferden, V. M., Tappe, D., Beyer, M., Truper,
H.G., Klein, J., 1993. Biochemical
mechanisms for the desulphurisation of
coal relevant organic sulphur
compounds. Fuel. 72, 635-643.
Pandey, R. A., Raman, V. K., Bodkhe, S. Y., Handa,
B. K., Bal, A. S., 2005. Mic robial
desulphurization of c oal c ontaining
pyritic sulphur in a continuously operated
bench scale coal slurry reactor. Fuel. 84,
81–87.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Semi-Supervised Classification of Mapping between Coal Blend

Parameters and Coke Strength after Reaction (CSR)

T. Ray1*, A. Suresh1, P.S. Dash2 and P. K. Banerjee2

1
Research & Development, Tata Steel, Visakhapatnam – 530012.
2
Research & Development, Tata Steel, Jamshedpur – 831001.

Abstract
Normally supervised methods are able to comprehend and classify labelled data which is more
expensive and time consuming than unlabelled ones. Also supervised methods are suitable for
classifying only labelled data but not unlabelled data. Consequently, semi-supervised learning or
classification performs better while learning from a combination of labelled and unlabelled
datathan using the labelled data alone.In this methodunlabelled data is classified by cluster
assumption.So it has attracted many attentions during the last decade.
In this paper semi supervised method has been tested by introducing cluster concept to supervised
methodology of ANFIS. Basically the result of carbonation test of different coal blendhas been
chosen as platform for this study. Functional relationship between input parameters as coal
blend properties and output parameters as CSR has been developed in supervised mode of ANFIS
by taking input and output randomly.Thereafter fuzzy c-means clustering has been invoked for
making a choice of input and output in cluster wise rather than random choice. As far as the
outcome is concerned, correlation coefficient indicates the superiority of clustered choice to random
choice of data.
There are number of techniques prevalent in technical community to optimise number of fuzzy
rules in ANFIS. Singular value decomposition (SVD) has been implemented. Its choice has been
compared to existing manual technique for number of fuzzy rules determination.

Keywords: Clustering; supervised classification; SVD; ANFIS.

1. Introduction combination of labeled and unlabeled data for

better performance than using the labeled data
The collection of unlabeled data is relatively
alone, has attracted considerable attention.
much easier than that of labelled data from the
During the past decades, lots of semi-supervised
point of view of cost and time. (Xu et al., 2010,
classification methods have been developed,
Hu et al., 2010). Consequently, semi-supervised
and comprehensive reviews can be found
learning, and more spec ific ally, semi-
(Chapelle et al., 2006, Zhu and Goldberg, 2009,
supervised classification, which learns from a
Zhou and Li, 2010).
* Correspending Author:T. Ray, Researcher, Research & Generally semi-supervised classific ation
Development, Tata Steel, Visakhapatnam – 530012. approaches can be categorized into four
313
 MPT-2013

paradigms, that is, generative approaches, reactives, vitrinite distribution (V 9 – V 13),

semi-supervised large margin approaches, crucible swelling number, basicity index.
graph-based approaches, and disagreement- In this paper neuro fuzzy semi supervised
based approaches (Zhou and Li, 2010, Zhu, classification have been carried out on set of
2008) while this paper focuses on the second input and output features of carbonation test.
one. Generally, semi-supervised classification Before classification number of cluster has been
methods attempt to exploit the intrinsic data identified hidden in input data by criteria
distribution hidden in unlabeled data. This proposed by Hu and Dennis (1994). Co-relation
data distribution information is generally coefficient between input and output shows the
helpful to construct a better prediction model. efficacy of clustered data over random data.
To exploit unlabeled data, some assumptions While doing neuro fuzzy classification fuzzy
need to be adopted. One of the most common rules have been optimised by singular value
assumptions is the cluster assumption, which decomposition (SVD) technique. So input versus
assumes that “similar instances should share output mapping of carbonation test becomes
the same label” (Chapelle et al., 2006, Zhu and faster. Introduction has been covered in section
Goldberg, 2009, Xue et al., 2011). This 1. Theory underlining the analysis has been
assumption has been adopted and found useful described in section 2. Section 3 consists of
by many semi-supervised c lassific ation result and disc ussion. Finally sec tion 4
methods. But as per this assumption, every concludes the paper.
instance should have a crisp class label
2. Theory
assignment. In real applications it is difficult in
some cases to assume that an instance definitely 2.1. Anfis model development
belongs to one class and does not belong to other First order sugeno type ANFIS structure
neighboring classes (Vapnik, 1998). At the same (Suresh et al., 2012) consisting a number of fuzzy
time there are several techniques to predict rules has been shown in Fig. 1. It consists of
cluster number from unlabelled data. Among five number of layers where each node performs
existing techniques measures like within cluster a particular function on incoming signals. Here
distance and it’s derivative proposed by Hu et. the sigmoidal membership function has been
al are quite popular (Hu and Dennis, 1994). There chosen. Coal blend properties such as ash,
are methods to predict coal strength after volatile matter, average vitrinite reflectance,
reaction from coal blend properties (Kanjilal, total reactives, vitrinite distribution (V – V ),
9 13
1998, Bhattac harjee, 1999). Suresh et al., crucible swelling number, basicity index have
(2012)proposed prediction model based on been considered as input variables whereas the
adaptive- network-based fuzzy inference coke CSR has been fixed as an output variable.
system (ANFIS) network to forecast CSR from Input variables and output variable are related
coal blend properties such as ash, volatile through fuzzy rules.
matter, average vitrinite reflectance, total
Fig. 1: ANFIS structure
Calculation of
membership Calculation of
Calculation of Bias output of Calculating
normalised
function using firing strength normalised overall
firing strength
sigmoidal of fuzzy rule firing strength output
function of fuzzy rule

314
 MPT-2013

2.2. Fuzzy c-means clustering picked up as a test set and remaining fifty
constitute the training set.
A given set of objects characterized by a set of
features are partitioned into a suitable number 2.3. SVD based QR decomposition method
of clusters with a proper distance metric by Singular Value decomposition (Yen and Langari,
c lustering tec hnique. Among different 2003) of matrix of dimension is
clustering techniques Fuzzy c-means used to
obtained as A  UV T . QR decomposition
assign crisp membership values to partitioned
with column pivoting factorisation algorithm
objects. The membership value can be anything
between 0 and 1. Fuzzy toolbox of Matlab 7.0 is applied on to keep number of rules by
has been used for said clustering. removing rules. U ltimately
Always number of cluster prevailing in input permutation matrix is computed to select
dataset is one parameter to be known before number rules .
clustering. Among different methods within
3. Results and Discussion
cluster distance along with it’s first, second
order derivative prove to be successful (Hu and Carbonization tests have been conducted under
Dennis, 1994). stamp c harging c onditions on seven kg
Within-cluster distance, WTK is defined as electrically heated laboratory scale test oven
(Dash et al., 2005) by keeping operating
K
1 parameters like bulk density, oven temperature,
WTK 
N
  D C
k 1 tg k
k , Xt 
moisture, granulometry and carbonization
where g1 ,..., g K  is a K group (c luster) time constant for all the tests. The different
partition of the full source data set containing c ompositions of c oal blend have been
N objects, C k , is the cluster centre of g k and formulated for each experiment. For each
X t ,is an object in one of the clusters. experiment, ash, volatile matter, average
DC k , X t  is the metric measuring the vitrinite reflectance, total reactives, vitrinite
distance between an object and its cluster distribution (V 9 – V 13 ), cruc ible swelling
centre. number, basicity index and the coke CSR
For fixed number of clusters, any clustering properties of differently composed coal blend
method tries to cluster X in K groups by have been recorded.
minimizing WTK . As due to nonlinear nature
of iterative updation process in fuzzy c-means,
global optimum partition may not be
reached(Hu Y. and Dennis T., 1994). The true
cluster number is indicated by the elbow of
WTK/K curve as seen from Figure 2. First and
second difference of WTK/K curve are often used
to ascertain the elbow. From the entire curve as
shown below, true cluster number has been
Cluster numberNumber
determined to be equal to eight.
Followed by clustering the entire data set into Fig. 2: Plot for
WTK versus number of clusters
eight groups, seventeen data sets uniformly K

315
 MPT-2013

Seven parameters have been identified as input

parameters whereas coke CSR has been chosen
as output parameter.
Now set of experiments performed with ANFIS
for input and output parameters as mentioned
above are as follow.
1. Training data and testing data are chosen
randomely or without clustering
2. After clustering only training and testing Test data number
data are chosen Fig. 4 Predicted and actual CSR value for
Performance criteria of ANFIS using 50 epoch seventeen number of test data for non-
in the form of root mean square error (RMSE) clustered feed to ANFIS.
and c orrelation coeffic ient (R 2) between As seen from Table 1 correlation is better for
predicted and actual data has been shown in clustered data than non-clustered data. RMSE
Table 1. Input data has been normalised to the might be lower for particular batch of training
range between zero and one. and testing set. Predicted and actual CSR for
As discussed earlier, after fuzzy c-means clustered and non-clustered networks are
clustering measures e.g WT K K , it’s first and shown by Fig. 3 & 4.
second difference have been used to determine Aftermath SVD based QR decomposition has
number of clusters hidden in input data as been implemented to reduce number of rule
eight. After clustering ANFIS classification has based considered for classifying clustered data.
been accomplished with seventeen and fifty Originally eight number of rule bases are used.
number of data as test and train. Without Depending upon the singular values of rule base
clustering ANFIS classification has been done matrix, eight number of rule bases has been
with same number of train and test data.
minimised to only three. With three number of
Table 1: Result of ANFIS for with and without rule base, using ANFIS performance in terms of
clustered data set RMSE and R2for training and testing are 4.77,
Choice of training Training Test Set Training Test Set 3.31 and 0.65, 0.84 respectively. So after
and testing RMSE Set R2 R2
dataset RMSE optimising number of rule base also
Without cluster 4.76 3.23 0.66 0.77 performance is remaining unchanged.
With cluster 4.77 3.31 0.65 0.84
Table 2: Singular values of firing strength
matrix corresponding to different fuzzy rules

Serial number of Singular value of

Fuzzy rules the firing strength matrix for
corresponding fuzzy rule
1 3.2467
2 0.2788
3 0.0877
4 0.0635
Test data number 5 0.0294
6 0.0224
7 0.0051
Fig. 3: Predicted and actual CSR value for sev-
8 0.0026
enteen number of test data for clustered feed
to ANFIS

316

4. Conclusions
Supervised and semi supervised classification
have been implemented on c oal blend
properties to predict coke CSR. It has been found
that semi-supervised classification with ANFIS
is ahead of supervised method in terms of
correlation measure. For semi supervised
classification number of clusters hidden in the
input data has been determined by within
cluster distance, it’s first difference and second
difference. Number of fuzzy rules has been
optimised with SVD based QR optimisation
technique.
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*******
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1530.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Studies on the Cleaning Potentialities of Ib Valley Coals by

Washability Investigations

T. Gouri Charan, P.C.Nagnoor and B.P.Ravi

Coal Preparation Division, Central Institute of Mining & Fuel Research, Dhanbad-828108,
India
Professor, Department of Mineral Processing, P.G.Centre, Nandihalli - Sandur, Karnataka,
India

Abstract
India’s energy sector is primarily dependent on coal which is the abundant indigenous resource.
Such dependence on coal is going to continue in the foreseeable future. Indian coals, which are of
Gondwana origin, contain high ash wherein the extraneous material was intimately mixed in the
coal matrix during the formation stage, causing a high level of impurities in the run-of-mine
(ROM) material. These coals possess difficult to very difficult washability characteristics.
Beneficiation of high- ash non-coking coals of India has become the prerequisite for improving the
overall economics and efficiency of power generation. The state of Odisha contains approximately
23% of India’s reserves of non-coking coal. This paper describes the washability characteristics of
non-coking coals from the Ib Valley Coalfields of Odisha aiming at 34% ash level in the clean coal
as per the stipulations laid by environmental gazette notification of Govt. of India. Conventional
float – and - sink testing was carried out to determine the theoretical yield of clean coal at 34% ash
content. The washablity data was used for prediction of practical yield which may be achievable
by using a Jig washer. Based on the simulated results a conceptual flow sheet was developed.
1. Introduction w.e.f. June 2001. Comparatively high levels of
Indian coals are of Gondwana origin, which are ash in Indian coal causes concern both in terms
inferior in quality. The characteristics of these of the high costs of coal movement and the
coals differ significantly from other coals of associated environmental impacts. The high-
Gondwana origin, partic ularly in their ash coals without any beneficiation are directly
chemical and petrographic makeup, which fed to the majority of the power plants in India.
have direct bearing on their utilization The state of Odisha contains approximately
potential. Most of the non-coking coal produced 23% of India’s reserves of non-coking coal, and
in India has high ash content (40-45 percent on the major supplier is Mahanadi Coalfields
an average) and the users are unhappy with limited (MCL). The state has two major
the quality. Govt. of India has promulgated a coalfields, namely Talcher coalfields and Ib
Gazette Notification (GSR 560(E) & 378(E), dated Valley coalfields. The state is the main supplier
September 19, 1997 and June 30, 1998 of coal to the various thermal power stations
respectively) on use of beneficiated/blended in the Southern part of India, which are at a
coal containing ash not more than 34 percent distance upto 1000 kms and in case of some

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 MPT-2013

plants even more. One of the major problems sample was subjected to dry screen analysis at
in the power sector is the varying and high- sizes 50, 25, 13, 6, 3 and 0.5 mm. The size
ash content in the ROM coals averaging above distributions of coal crushed to minus 75 mm
45%. The stipulation laid by the Ministry of are shown in Table 2. The individual size
Environment and Forest (MOEF), is posing fractions were subjected to float – and - sink
problems to MCL for the despatch of its coal to tests, and the relative density range was 1.40
the power plants situated in the Southern part to 2.00. The minus 0.5 mm coal fractions were
of India. The only solution to this problem not subjected to float-and- sink tests
appears to be setting up of coal wasaheries to Table 2: Size analysis of coal crushed to 75mm
reduce the ash content. Keeping this in view, of all the coal samples
detailed investigations on washability
characteristics for Ib Valley coals was carried. Size, mm
IB-SOCP
Wt. % Ash%
IB-BAS
Wt. % Ash%
IB-LAJ
Wt. % Ash%
IB-BEL
Wt. % Ash%
The paper highlights the detailed findings with 75 - 50
50 - 25
32.5
30.8
59.4
56.6
52.9
22.0
54.9
54.7
31.1
32.4
47.5
46.1
34.1
33.4
54.4
54.4
respect to washability tests on coals collected 25 - 13
13 - 6
13.8
9.0
52.1
48.9
11.0
5.5
57.0
56.5
15.3
9.1
44.0
41.4
12.6
7.8
53.0
51.6 1.
6 – 0.5 10.1 46.3 6.3 55.4 9.2 34.0 8.5 49.5
from four major sources. The paper suggests a - 0.5 3.8 55.5 2.3 62.0 2.8 40.0 3.6 54.0
100.0 40.8 100.0 55.4 100.0 44.5 100.0 53.6
suitable flow scheme for beneficiation of the
3. Results and Discussions
non-coking coal.
It may be seen from Table-1 that all the coal
2. Experimental
samples contain very high ash percent. It may
The coal samples were collected from the be seen from Table -2 that when the raw coal
working benches with the help of a Haulpack was crushed at 75 mm, the ash distribution is
and payloader, by scraping the entire cross almost uniform in all the size fractions and
section of the bench at various places from each further is may be noticed that the ash percent
of the collieries. After proper and thorough of the fraction below 6mm is also on the higher
mixing, about 10 tons of sample from each side and hence this fraction also needs washing
colliery were collected and brought to the to the required ash level.
laboratory for further studies.
Source Cut Density Cleans Rejects
Table 1: Proximate analysis of coal crushed to Wt% Ash% Wt% Ash%
IB - LAJ 1.725 54.5 33.8 45.5 57.5
75mm of all the coal samples IB - SOCP 1.785 50.9 33.8 49.1 75.6
IB - BEL 1.675 43.1 33.7 56.9 67.3
Parameters IB-SOCP IB-BAS IB-LAJ IB-BEL IB - BAS 1.725 46.9 34.0 53.1 73.8
Moisture, % 8.2 6.9 7.0 7.5
Ash, % 20.4 19.7 21.5 20.4 Hence for studying the cleaning possibilities for
Volatile Matter, % 50.8 51.8 42.0 49.8 achieving 34% ash content in the clean coal the
Fixed Carbon 20.6 21.6 29.5 22.3
100.0 100.0 100.0 100.0 combined washability data generated for the
dry ash% 55.3 55.6 45.2 53.8 size frac tion 75 – 0.5 mm was used and
The raw coal was taken and first screened at 75 accordingly the theoretical yield% at 34% ash
mm; the plus 75 mm fraction was crushed in a content was estimated and the data is shown
single roll crusher. Representative samples in Table – 3.
from the overall combined fraction of the It may be seen from Table - 3 that the theoretical
product below 75 mm was taken for studies yield at 34% ash content for the coal sample IB-
like raw coal characterization, size analysis and LAJ is 54.5%, for IB-SOCP it is 50.9%, for IB-BEL
size wise float and sink tests. The raw coal was it is 43.1% and for IB-BAS it is 46.9%.
characterized with respect to proximate and The theoretical yields as mentioned above may
the data is shown in Table 1. Representative not be achievable in actual plant practice due
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 MPT-2013

to dynamic system of the washers. The practical a. Run of Mine coal from the open cast mines
yield to be obtained from the commercial plants may be fed to a primary crusher to crush
varies in quality and quantity depending on the ROM coal down to 200 mm. The crushed
the efficiency of the washing system. However, coal – 200 mm may be conveyed for further
it is possible to predict the yield of the clean crushing.
coal at desired quality considering the normal b. The – 200 mm coal may be screened by
efficiency values of the washers by taking the using a vibrating screen of aperture 75 mm.
concept of Gaussian equation. The partition The + 75 mm coal may then be crushed
data represents the fraction of the feed in a down to below 75 mm in a single roll
density interval which goes to the clean coal crusher. The coal of below 75 mm size may
and d50 is the density at which the 50% of the be conveyed to a raw coal surge bin.
feed in that density that goes to the clean coal. c. The fraction i.e., 75 - 0 mm may be washed
The parameters derived from the partition/ in a Jig. The Jig may produce 2 products –
Tromp curves are the a) Relative density at the washed coal and rejects. Rejects will be
cut point ‘d50’; b) Ecarte Probability Moyen dewatered on perforated bucket elevators.
‘Ep’; c) Imperfection T d) Error area. In general Dewatered rejects will be conveyed by
the partition c urves are spec ific to the means of belt conveyor to rejects stockpile.
separation units for which they are established Washed coal from jig shall be dewatered
and are independent of the density and blended with – mm fraction to get total
dis­tributions of the feed and depend on size cleans
composition, feed rate and other operating d. The rejec ts may be used for power
conditions. generation through FBC route.
It was assumed that the quantity of misplaced Fig. 1: Flow Sheet for Beneficiation of IB-SOCP
material decreases exponentially with the
increase in difference between its specific
gravity (X) and the specific gravity of cut (X*).
 y(X) = 100-50exp[(X-X*)/Z] for X<X*
 y(X) = 50exp[(X*-X)/Z] for X>X*
 y(X) = 50
where y(X) is the recovery of component of the
float fraction (%) and Z= Ep/ln0.5
The above three equations can be used for
predic ting the performanc e of washer
considering normal efficiency of the washer
(known Ep).
Taking the washability data of the fraction 75 –
6 mm, the above model, was used to develop a
flow scheme by taking the efficiency values of
the Jig washer.

4. Development of A Beneficiation Strategy

The flow sheet developed for all the coal

samples is shown in Figures 1 to 4.
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 MPT-2013

Figure 4 Flow Sheet for Beneficiation of IB -

BEL
Figure 2: Flow Sheet for Beneficiation of IB - 5. Conclusions
BAS
The washability studies on the coal samples of
IB Valley coalfields show that the coal possesses
good washability characteristics. The studies
indicated that full scale beneficiation may be
practiced for all the coal samples. By taking the
efficiency values of the Jig washer it was possible
to predict the practical yield at the required ash
level. A conceptual flow scheme was suggested
for all the four coal samples and the yield of
total clean coal is as follows:
a. For the coals of IB-LAJ, the yield of clean
coal at 34% ash level is 32.0% and the
corresponding rejects ash being 50.8%.
b. For the coals of IB-SOCP, the yield of clean
coal at 34% ash level is 44.2% and the
corresponding rejects ash being 70.4%.
Figure 3: Flow Sheet for Beneficiation of IB – c. For the coals of IB-BEL, the yield of clean
LAJ coal at 34% ash level is 33.0% and the
corresponding rejects ash being 50.8%.
d. For the coals of IB-BAS, the yield of clean
coal at 34% ash level is 37.1% and the
corresponding rejects ash being 67.6%.
The rejects may be used for generation of power
through FBC route.
*******
321
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Chemical Fractionation Analysis of Some Indian Coal Sources

and their Correlation with Ash Fusion Temperature

S. Chakravarty*, Ashok Mohanty, Anita Kumari, Arun K Mahato and Mamta

Sharma
CSIR-National Metallurgical Laboratory, Jamshedpur-831007
Abstract
Coal from different sources have a wide variation in their chemical and physical properties and
has direct impact on gasification behaviours. Due to large variation in chemical as well as physical
properties of different coal sources, it is very difficult to predict the fate during combustion and
gasification. The ash in coal is considered as an anti-calorific substance which has a detrimental
effect on coal combustion. During the process of combustion, the mineral matter in coal transforms
into ash and part of the minerals are deposited on the wall of the boiler resulting to slagging and
fouling. Therefore, mineral matter present in coal is responsible for the formation of fouling and
slagging. The composition of ash varies substantially from seam to seam of a particular borehole.
Therefore, seam wise characterization of mineral phases of coal sources is very critical to analyze
the behaviour of coal ash decomposition during the process of combustion. Present study aims to
obtain mineral species-specific information on different coal seams of a particular borehole of
Samaleswari block, Ib river coalfield, Odisha, India. Chemical fractionation is applied to determine
the mode of occurrence of inorganic elements present in coal mineral phases based on their
solubility. The results of chemical fractionation test have been correlated with the mineral phases
identified by X-ray diffraction (XRD). The major mineral phases present in coal seams are identified
as quartz, kaolinite, bassanite, siderite, apatite and pyrite. In chemical fractionation test, almost
90% of Fe-based minerals are removed by acid leaching whereas Ca based minerals have variation
in leaching behaviour in different coal seams of a particular borehole of Samaleswari block, Odisha.
Further, Ash Fusion Temperature (AFT) of coal indicates the extent to which ash agglomeration
and clinkering are like to occur within the gasifier. The results obtained from AFT of different coal
seams and chemical fractionation indicate the decomposition behaviour of mineral phases present
in particular coal seams.
Keywords: Chemical fractionation, ash fusion temperature
1. Introduction samples. In this process, different elements are
Chemical fractionation reflects the mode of selectively extracted from coal based on their
occurrence of mineral phases associated in coal solubility (Van Dyk et. al., 2005). Different
solvents like water, ammonium acetate and
* Correspending Author:S. Chakra varty ,CSIR-Natio nal
concentrated HCl are used sequentially in this
Metallurgical Laboratory, Jamshedpur-831007
Contact No. : 91 657 2345063; email: method to leach the inorganic phases present
sanchita@nmlindia.org in coal moiety. Generally water soluble and ion

322

exchange part (ammonium acetate soluble part)
includes various salts of alkaline and alkaline
earth metals which are considered to be easily
decomposed in a high temperature processes.
Carbonate and sulphates are expected to leach
out in HCl medium whereas the oxides and
silicates are left as an insoluble residue. Detail
knowledge of mineral phases present in coal
and its behaviour during the process of
c ombustion pose a great importanc e in
understanding the fusion characteristics of coal
and coal ash (Teixeira et. al., 2012 and Pettersson
et. al., 2008).
The measurement of Ash Fusion Temperature
(AFT) is one of the major factors to predict the
combustion and gasification behaviour of coal.
AFT of a coal source gives an indication to the
problem related to slagging and clinckering in
industrial boilers. AFT analysis consists of four
temperatures, namely, Initial Deformation
Temperature (IDT), Softening Temperature (ST),
Hemispherical Temperature (HT) and Flow
Temperature (FT). However, investigation on
the relation between mineral species present
in coal and AFT are still very limited with
respect to Indian coal. Some information is
available on relation between mineral species
and AFT on South African coal and Bulgarian
coal (Van Dyk et. al., 2005, Vassileva and
Vassilev, 2002). In this work, effort has been
made to investigate the mineral phases present
in different coal seams of Ib valley coalfield,
Odisha and to explore some correlation with
AFT.
2. Materials and Methods
2.1 Sample Preparation
Three bituminous coal samples having non
coking property from different seams of a single
coal source of Ib river coalfield was selected for
the chemical fractionation study. The coal
samples were powdered using jaw crusher and
ball mill. The samples used for chemical
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MPT-2013
fractionation test were of <150µm size. The
samples were then homogenized by quarter
and coning technique to make a representative
sample.
2.2 Chemical Fractionation
In the present study the experimental procedure
followed for chemical fractionation test was
same as reported by Van Dyk et. al., 2005.
Briefly, air dried samples from three individual
seams identified as seam A, seam B, and seam
C, of a single coal source (Samaleswari block, Ib
river coalfield, Odisha, India) was taken as
“original” sample. 10 g of original coal sample
along with 30 ml of water was used for H2O
leaching. The coal-water mixture was mixed
for 18 hr using rotospin (Tarsons, India). After
18 hr mixing, the sample was filtered and rinsed
with distilled water. The filtrate along with the
rinsed water was collec ted in a 50 ml
volumetric flask and kept aside for further
measurements. Similar method was applied for
Ammonium Acetate (NH4OAC, 1M) leaching
and HCl (6 N) leaching, sequentially, for every
sample. In every leaching procedure, the initial
and final weight of the residue was determined
and properly labelled as “NH4OAC leached”
and “HCl leached”. The filtrate obtained after
each extraction was diluted to 50 ml using
distilled water. All the filtrate containing
leac hed elements were measured by
Inductively Coupled Plasma Optical Emission
Spectrometer (ICP-OES), VISTA MPX, VARIAN.
2.3 AFT
For AFT analysis, the leached residue along
with the original coal samples was ashed at
815 0C. A melting test to measure initial
deformation temperature (IDT), softening
temperature (ST), hemispherical temperature
(HT) and fluid temperature (FT) was conducted
in presenc e of air using Ash Fusion
Determinator, AF-700, LECO.
 MPT-2013

3.0 Result and Discussion block, Ib river coalfield, Odisha, India is

3.1 Analysis of coal ash before and after presented in Fig 1 A-C. It is apparent from Fig. 1
leaching that leaching behaviour of three samples is
quite different. While 30-40% of Na is leached
Coal sample of seam A was taken to study the
out from the seam A and seam C coal samples
mineral matters present in the coal sample
by washing with water, only 6 % Na can be
before and after leaching experiment. The
removed in seam B sample. Similarly, 20-30 %
original coal sample (prior to leaching) and the
of Ca and Mg can be leached out from seam C
coal sample obtained after leaching study
sample by washing with water but only little
(sequential leaching with water, ammonium
amount leached out from other two samples.
acetate and hydrochloric acid) were ashed and
This suggests that minerals are present in
chemical analysis of ash was performed. The
different phases in these three coal samples.
ash composition of the original coal and the
After H2O leaching traces of Ca and Mg were
insoluble coal residue after acid leaching is
leached from the coal. Part of the Na was leached
represented in Table 1. All the mineral elements
by water extract whereas rest of Na minerals
are expressed in oxide form. Data in Table 1
along with the part of Ca minerals were leached
indicates that minerals like Fe, Ca are removed
from coal by NH4OAC. After HCl wash Fe and
from the coal sample after leaching. However,
Ca were the two main minerals types leached
minerals like Na, K and Mg are only partially
from coal in high concentration. 90% of Fe
removed after leaching. This suggests that these
minerals and 65% of Ca were soluble in HCl
minerals are strongly bonded in the silicate
medium. A very interesting finding was that
matrix.
almost 100% of K and 70% of Mg was associated
Table 1. Chemical analysis of coal ash
with the insoluble silicate matrix as observed
samples before and after leaching study
in Fig. 1.
Composition Original coal Coal ash sample
Sea
ash sample after leaching study mA

Al2 O3 21.46 % 21.41 %

SiO2 62.59 % 62.12 %

Fe2 O3 5.51 % 0.56 %

CaO 1.73 % 0.08 %

Sea
mB
MgO 0.60 % 0.44 %
Na 2 O 0.11 % 0.09 %
K2 O 1.05 % 1.01 %

P 2 O5 1.57 % -

TiO2 1.72 % - Sea

mC
SO3 0.06 % -

3.2 Chemical Fractionation

The result of chemical fractionation study of
coal samples of three different seams (seam A, Fig. 1 Leaching behaviour of coal samples of
B & C) of the same borehole of Samaleswari three different seams of same borehole.

324

3.3 Ash Fusion Test
Result of AFT study of the original coal and the
coal after leaching is shown in Fig. 2. It indicates
that HCl leaching removed the mineral elements
from the coal that caused the AFT to increase
>1600oC. Very little changes were observed
after the removal of mineral elements by
NH4OAC and H2O leach. It appears from the
Fig. 2 that the presence of Fe and Ca has direct
influences on AFT.
Fig. 2 Effect of water, ammonium acetate and
hydrochloric acid leaching on AFT of seam A
coal sample.
Finally, XRD was used to identify the presence
of mineral phases in original coal as well as the
insoluble coal residue. The mineral phases in
original coal were identified as Quartz,
Kaolinite, Bassanite, Siderite, Apatite and
Pyrite.
4. Conclusion
The present preliminary study emphasize that
coal samples collected from different seams of
same borehole of the Samaleswari Block, Ib
river coalfield contain different mineral phases,
Quartz, Kaolinite, Siderite, apatite and pyrite.
Chemical fractionation test indicates that the
*******
325
MPT-2013
leaching behaviour of the coal samples is very
different from each other. Effort was made to
establish relation between ash-fusion
temperature (AFT) and chemical fractionation
test. The presence of Ca and Fe based minerals
in coal was found to have influence on ash fusion
temperatures.
Acknowledgement
The authors gratefully acknowledge Director,
CSIR, National Metallurgical Laboratory for his
kind support and guidance to publish the work.
This work is the part of the ongoing project
sponsored by CMPDIL, Ranchi, India. Special
thanks to CMPDIL, Ranchi for their support in
cola characterization.
References
Van Dyk, J. C., Baxter, L. L., van Heerden, J. H. P.,
Coetzer, R. L. J., 2005. Chemic al
fractionation tests on South African coal
sourc es to obtain spec ies-spec ific
information on Ash Fusion Temperature
(AFT). Fuel 84, 1768-1777.
Teixeira, P., Lopes, H., Gulyurtlu, I., Lapa, N.,
2012 Use of chemical fractionation to
understand partitioning of biomass ash
constituents during co-firing in fluidized
bed combustion. Fuel 101, 215-227.
Pettersson, A., Zevenhoven, M., Steenari, B.,
Åmand, L., 2008, Application of chemical
frac tionation methods  for
c harac terisation of biofuels, waste
derived fuels and CFB co-combustion fly
ashes.
Vassileva, Ch. G., Vassilev, S. V., 2002, Relation
between ash-fusion temperatures and
chemical and mineral composition of some
Bulgarian coals. Geologie Mineralogie 55,
61-65.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Process Amenability Studies for Deshaling of Coking Coal

Sample from Bokaro, Central Coalfields Limited, India

P.C.Naganoor1, T.Gouricharan2, B.S.Prasad1*, S.M.Gowda1, K. Manjula1 and G.

B. Balachandar1
1
Mineral Processing Department, VSKU PG Centre, Nandihalli 583119.
vskubminpro@gmail.com
2
Coal Preparation Division, CSIR-CIMFR, Dhanbad 828108. gouricharan@yahoo.com

Abstract

Coking coal is an essential input for production of Iron & Steel through blast furnace route. To save
steel industry facing acute dependence on imported coking coal, domestic availability of coking
coal in right quality and quantity has become imperative. The good quality coking coals of both
Jharia and Bokaro coalfields are fast depleting leaving behind the inferior quality coals. The
washability characteristics of these coals are poor. This paper presents the laboratory beneficiation
studies on run-off-mine coal crushed to minus 6 mm and suggests a suitable beneficiation route
for the improvement in the quality for steel making reducing ash content. Detailed analysis with
respect to characterization, washability investigations and flotation of coal fines is presented.
The coking propensities and the petrographic analysis of the clean coal strongly support its use
for the metallurgical purposes.

Key words: coking coal washability, fine coal flotation.

1. Introduction The demand of coal and so its production in the

The relative abundanc e of c oal in India
compared to other fossil fuels makes it a natural
choice as the primary source of fuel, be it for
steel making, power generation or for other
uses. Total reserves of coal in the country are
estimated to the order of 299 Billion Tons.
Coking coal, which is merely 14% of the total
deposits, is available mainly in Eastern part of
India, in the BCCL and CCL areas. Superior type
of coking coals is now depleting from its unique
source in and around Jharia coalfields.
* Correspending Author:: B.S.Prasad, Mineral Processing
Department, VSKU PG Centre, Nandihalli 583119. Email:
vskubminpro@gmail.com
country is increasing at a fast rate particularly
with the growth of steel and power sectors. The
coking coal reserves are meager therefore the
c ountry c annot increase produc tion fast
enough to keep up with the high growth of its
steel industry. Inevitably, India must rely on
imports, purchasing substantial quantities of
c oke and c oking c oal, partic ularly from
Australia.
To meet the increased demand of coking coal
concerted efforts have to be made to correct the
imbalance between need and availability by
increasing the production of coal of desired
quality through better management of

326

available resources of inferior grade. Low
volatile coking coal (LVCC), though inferior in
qualities but abundantly available in eastern
part of the country may be an immediate choice.
These coals, being of lower seams are likely to
be more matured (Ro ~1.30%) than the upper
seams and consequently exhibit lower values
of volatile matter. The country has a moderate
reserve of such coal, amounting to about 50%
of the total coking coal reserve.
Unfortunately, the washability potential of this
coal is so poor that the existing washeries
having conventional washing technologies may
not able to supply coals of ash 17-18% as desired
by indigenous metallurgical industries and
cannot stand in competition with foreign coals
because of poor yield of Cleans. As such, these
coals are being treated as NLW (Non-linked
washery grade) and are supplied to the thermal
power plants, against augmenting the demand
of metallurgical coal for coke making thus,
wasting the scarce coking coal resources.
Effec tive utilization of this resourc e by
optimum beneficiation will reduce the ever-
increasing dependence on the imported washed
coking coals in India as well as supplements
the requirement of quality feed for power
plants. Keeping this in view, an attempt has
been made in this paper to focus detailed
Washability and Flotation Studies carried out
on Low Volatile Coking Coal of Central
Coalfields, for total utilization of the ‘difficult-
to-wash’ inferior coals.
2. Sample Source
About 10t of Coking Coal sample was collected
from Central Coalfields for carrying out the
detailed washability and flotation studies.
3. Sample Preparation
The representative raw coal was taken and first
screened at 50 mm. The >50 mm fraction was
crushed in a single roll crusher to <50 mm. The
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MPT-2013
below 50 mm fraction was screened at 6 mm
and the 50 – 6mm fraction was crushed to 6
mm in a double roll crusher. The overall
combined fraction of the product below 6 mm
was taken for further studies viz., screen
analyses, Float & Sink tests and flotation tests.
4. Washability Studies
The size distribution of coal crushed to 6 mm is
shown in Table 1. The fraction 6 – 0.5 mm was
subjected to Float & Sink tests, and the relative
density range was 1.40 to 1.80. The washability
data of the combined fraction (6 – 0.5 mm) was
generated and were used for plotting the Mayer
curve and it is depicted in Fig. 1.
Table 1 Screen Analysis of Raw Coal crushed
to 6 mm
Size(mm) Wt% Ash%
6- 3 34.9 25.3
3- 1 25.9 24.7
1 - 0.5 15.6 23.2
-0.5 23.7 30.6
100.0 26.1
Fig. 1 Mayer Curve
5. Froth Flotation Studies
Batch laboratory flotation experiments are
carried out on the coal fines generated by
crushing the raw coal to 6 mm. Experiments
were carried out by taking 250gm of coal fines
(below 0.5mm) and wetting it by keeping
known volume of water for more than one hour
to form uniform coal slurry. This slurry is then
transferred into the Denver D-12 sub aeration
 MPT-2013

type flotation cell. More water was added to The cleans generated from the coarser fraction
maintain the 33% solid concentration and 10% i.e., 6 – 0.5 mm and the finer fraction below 0.5
solid concentration during floatation at the mm was mixed proportionally and was
neutral pH. In each flotation tests, the pulp is c harac terized to understand its c oking
first agitated in the floatation cell for 3 minutes, properties. The characterization data is shown
after which the collector (diesel oil at three levels in Table 3. The coking properties in terms of
Crucible Swelling Number (CSN) and LTGK coke
1.25 kg/t , 1.50 kg/t and 1.75 kg/t) is added and
type and fluidity show that the clean coal is
the pulp is further conditioned for 2 minutes.
suitable for metallurgical purposes.
MIBC as a frother ( at three levels 0.2 kg/t, 0.4kg/
Table 3 Carbonization properties of clean coal
t and 0.6 kg/t) is then added and the pulp is
further conditioned for 1 minute. The impeller Sl. No Carbonization Characteristics
speed of the flotation machine was 1500 RPM. 1 Crucible Swelling Number 4 1/2
Flotation products were collected for 1 minute; 2 LTGK coke Type G6
the concentrate and tailing were filtered, dried 3 Gieseler Fluidity
and weighed. The ash content of the samples
a. Initial Softening Temperature C (Iddpm) 408
was determined. The data is shown in Table 2.
b. Maximum Fluidity Temperature , C 444
Table 2 Flotation of Coal Fines
c. Solidification Temperature, C 474
Collecto
Test r Frother Concentrate Tailings Feed d. Plastic Range, C 66
dosage, dosage
Wt% Ash% Wt% Ash% Ash% e. Maximum Fluidity, ddpm 750
No kg/t , kg/t
1 1.25 0.2 18.5 14.0 81.5 34.3 30.5
2 1.25 0.4 30.4 13.4 69.6 37.7 30.3 7. Conclusions
3 1.25 0.6 34.1 12.8 65.9 39.7 30.5
4 1.50 0.2 34.3 13.1 65.7 38.5 29.8  The low volatile coking coals from Central
5 1.50 0.4 57.8 12.0 42.2 55.5 30.4
Coalfields may be upgraded to the desired
6 1.50 0.6 56.8 13.6 43.2 53.1 30.7
7 1.75 0.2 59.0 13.5 41.0 55.1 30.6 quality if the coal is judiciously beneficiate.
8 1.75 0.4 59.4 13.7 40.6 53.3 29.8  The washability studies on the fraction 6 –
9 1.75 0.6 64.9 13.8 35.1 59.8 29.9
0.5 mm shows that it is possible to achieve
6. Results and Discussions theoretical yield of 52% at 10% ash content.
 The laboratory flotation studies showed
It is seen from Table 1 that about 60.7% of the
that it is possible to recover about 57.8% at
crushed material was above 1 mm and the ash
content being more than 25%. The - 0.5 mm 12% ash content.
fraction is about 23.7%, and its ash percentage  The analyses on the clean coal samples in
being 30.6%. terms of coking properties proved that the
From the washability studies on the size qualities of the cleans have improved
fraction 6 – 0.5 mm, the Mayers curve was remarkably and these may be gainfully
drawn and it may be seen from Fig. 1 that the utilized for coke making and metallurgical
theoretical yield% at 10% ash level is about 52%. purposes.
This data was used for generation of bulk cleans  A conceptual flow sheet may be developed
for characterization studies. by c onsidering H.M.Cyc lone for
The flotation studies as showed in Table 2 beneficiation of 6 – 0.5 mm fraction, while
indicate that it is possible to obtain an yield of
flotation may be c onsidered for
57.8% at an ash content of 12% at about 1.50 kg/
beneficiation of coal fines.
t of collector dosage and 0.4 kg/t of frother
dosage. Keeping this condition, bulk cleans was
generated for characterization studies.
*******
328
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Prediction of Coking Properties of Coals using Thermo-

Gravimetric Analysis

J.V.S. Murty1*, C.V. Nageswara Rao1, Nilu Kumar2, A. Srinivasa Rao2

U. Hari Prasad1 and Ch. V. Ramachandra Murty3
1
G.V.P. College of Engineering (Autonomous), Madhurawada, Visakhapatnam-530 048,
India
2
Visakhapatnam Steel Plant, Rashtriya Ispat Nigam Limited, Visakhapatnam-530 031,
India
3
Andhra University College of Engineering, Visakhapatnam-530 003, India

Abstract
Production of pig iron from Blast Furnaces in the Integrated Steel Plants requires strong coke for
the purpose of reducing iron oxide to metallic iron. Strength of this coke is assured by its
characteristics such as M10, M40 indices, CSR (Coke Strength after Reaction) and CRI (Coke
Reactivity Index). To produce coke of the required characteristics, bituminous coals (metallurgical
coals) having specified properties such as MMR (Mean Max Reflectance), VM (Volatile Matter),
Fluidity, TMF (Temperature of Maximum fluidity), Ash content, FSI (Free Swelling Index) etc., are
charged in coke ovens and pyrolized up to around 1000oC. This process is known as carbonization.
Since carbonization is a process in which various physico – chemical changes take place at different
temperature levels, thermo analytical techniques such as Differential and Thermo Gravimetric
Analysis (DTG-TGA) can be a very useful experimental tool to detect the changes and also the
degree of changes for the entire temperature range of carbonization as a continuous function.
The present investigation aims at developing additional parameters of coal from their respective
DTG-TGA thermo-grams and also their correlation with the some of the conventional properties
of coals viz: MMR, TMF, VM. Thermo Gravimetric tests on coal samples were carried out on TGA
701 (make - LECO Corporation) at Visakhapatnam Steel Plant, Visakhapatnam. About 12 samples
of indigenous and foreign coals with a spread of MMR from 0.85 to 1.4, VM from 20% to 36%, TMF
from 442 to 472oC have been subjected to thermo gravimetric analysis and correlations were
developed between TG parameters and coal properties.
Keywords: TGA, bituminous coals, characetization.
1. Introduction by blast furnace method and apart its function
as energy source, coke supplies the reducing
Metallurgical coke is one of the principal raw gases which convert iron oxides to iron. It also
materials used in the production of hot metal provides burden permeability necessary for
* Correspending Author: J.V.S. Murty, Associate Professor, blast furnace.
G.V.P. College of Engineering (Autonomous), Madhurawada,
Blast furnace grade coke is produced from
Visakhapatnam-530 048, India, +91-9346694380; Email:
jvsmurty@yahoo.com coking coals by the process of carbonization in

329

which the coal charge is heated in coke ovens in
absence of air. Not all coals are suitable for
carbonization into metallurgical cokes. Only a
limited range of coals with definite rank (MMR)
can produce acceptable metallurgical coke. A
characteristic feature of the coking coals is their
ability to soften on heating and become fluid/
plastic, swell with evolution of volatile matter
and later shrink on solidification to produce
semi-coke which on further heating undergoes
secondary evolution of volatile matter to give
coke (Murty et al., 2001).
Coal carbonization involves complex physical
and chemical changes associated with the
decomposition of the coal macromolecular
structure and the formation of the coke by an
agglomeration process. The quality of the coke
depends on both the characteristics of the coal
and the carbonization conditions. A number of
experimental methods have been developed to
measure coal and coke properties: physical,
chemical, rheological and petrographic (Varma,
2002). All these properties have been used with
varying degrees of success to predict coke
quality which can be expected from coal and
its potential in formulating a suitable blend.
The influence of the above quality parameters
on c oke quality is often not linear and
independent. Therefore, it is necessary to use
more number of parameters. Moreover, there
are wide differences of opinions as to which
characteristics or combination of properties
determine that coal will be of suitable coking
quality while others are not. Most of the tests
to determine coking properties are essentially
empirical.
Thermal analysis has been used for a long time
to determine the response of substances to
change with temperature. Since carbonization
is a process in which various physico-chemical
changes take place at different temperature
levels, thermo-analytical techniques such as
differential thermal and thermo-gravimetric
analysis (DTG-TGA) can be a very useful
330
MPT-2013
experimental tool to detect the changes and also
the degree of changes for the entire temperature
and time range of carbonization as a continuous
function. By developing an insight into the
mechanism of carbonization process one can
determine the various correlations between
coal and final coke properties.
The objective behind undertaking the present
research work on different coal samples using
thermo-gravimetry (TG & DTG) is to establish
whether it is possible to obtain additional
parameters for evaluation of the coking
properties of coal from their thermograms, viz.,
the temperature of maximum rate of weight
loss (TMRWL) and % Weight loss (% Wt Loss) to
correlate the same with conventional coking
coal evaluation characteristics such as volatile
matter and rank (VM &MMR) and plastic
properties (Gieseler Fluidity parameters).
2. Material and Methods
2.1. Thermo-gravimetric (TG) tests on coal
samples
Earlier studies carried out by RDCIS, SAIL
(Murty et al. 2001), revealed the possibility of
developing c orrelations between TG
parameters like TMRWL and % Wt Loss up to
900oC and the physical properties of cal such as
MMR, VM and TMF. Differential thermal
analysis is carried out on six foreign and eight
indigenous coals used in SAIL plants.
In the present study, only thermo gravimetric
analysis is conducted on a set of five foreign
coals and another set of 11 foreign coals under
inert atmosphere of nitrogen. For the 1st set of
samples, TG analysis is done under inert
atmosphere of nitrogen flow with a
temperature increase at the rate of 10oC/min up
to 1000oC. For the 2nd set of samples the program
is changed as follows:
From ambient to 100oC, the rate of increase is
kept at 15 oC/min and the temperature is
maintained at 100oC without any rise till all
 MPT-2013

the moisture is lost. Then, from 100oC to 300oC,
the rate of temperature increase is kept at 20oC/
min and the temperature of 300oC is maintained
for 7 minutes. A rate of 5oC/min is maintained
from 300oC to 1000oC.
For the above tests a sample of 0.7 to 1.0 gm
weight and size of -72 mesh is taken.
3. Results and Discussion
Table 1 and 2 give conventional characteristics
and TG parameters of 1st set of samples of VSP
and 2nd set of samples of VSP respectively.
Typical thermograms of a coal sample depicting
TG and DTG curve is presented in Fig. 1.
TG thermograms showing % Wt Loss versus
temperature (Fig. 1), it is observed that the
maximum weight loss oc c urs in the
temperature range of 400-600 0C which is
followed by a gradual weight loss beyond
6000C. Derivative thermogravimetry (DTG)
must be used to study the steep decrease in the
weight in the temperature range of 400-6000C.
In all the samples of coal, the temperature of
maximum rate of weight loss (TMRWL) lies in the
temperature range of 450-560 0C. It is also
observed that with increase in the rank of coal,
temperature of TMRWL also increases for all the
coals tested.

Table 1: Conventional Characteristics and TG 3.1. Development of correlations

parameters of 1st set of samples of VSP Methodology adopted to develop correlations
Sample
TMRWL % Wt loss MMR VM TMF
can be broadly separated into data compilation,
Name
V1 503 35 0.85 36.4 --
data treatment, and relationship derivation.
V2 553 22.71 1.18 23.9 460
V3 559 23.07 1.2 24.22 460
3.1.1. Data compilation
V4 526 31.29 0.92 34.23 441
V5 532 25.33 1.04 27.08 450 Conventional characteristics of coal namely,
Table 2: Conventional Characteristics and TG (VM, MMR, TMF) and derived characteristics
parameters of 2nd set of samples of VSP of coals from TG-DTG namely TMRWL and %Wt
Sample loss.
TMRWL % Wt loss MMR VM TMF
Name
VSP1 523.8 20.85 1.43 20.82 470 3.1.2. Data treatment
VSP2 506.6 22.81 1.27 23.97 457
VSP3 486 30.98 0.86 31.77 442
Microsoft Excel was employed in the data
VSP4 509.1 25.7 1.02 26.07 449 analysis. Various correlations that may exist
VSP5 510 24.2 1.18 23.91 461 between classical/conventional coal quality
VSP6 472.4 33.75 0.79 36.31 --
VSP7 512.8 21.44 1.304 19.91 472 parameters and their derived properties from
VSP8 514.1 25.18 1.144 24.18 460 TG-DTG thermograms were attempted.
VSP9 514.1 24.41 1.21 22.79 462
VSP10 495.2 24.14 1.22 25.32 449
3.1.3. Relationship derivation
VSP11 497.8 27.27 1.03 26.82 --
VM Content
The repeatability of this test is ± 0.3% for the
coking coals. Fig. 2 depict relation between VM
content (air dried basis) and weight loss in the
temperature range of 100-10000C (% Wt Loss)
for 1st and 2nd sets of VSP coals respectively.
Correlation coefficient, > 0.93 shows a strong
correlation between
%Wt loss & VM content:
Figure 1: Typical TG and DTG curve

331
 MPT-2013

%VM = 1.061 * (% Wt Loss) + 0.003 for 1st set of ISO 7404-1994 is 0.08%. An attempt has been
sample coals (1) made to develop correlation between this rank
%VM = 1.190 * (% Wt Loss) -4.748 for 2nd set of parameter and derived characteristics of coal
sample coals (2) from thermograms.
TMRWL vs MMR
%Wt Loss Vs VM Fig. 4 shows straight line relation between
40

35 rate: 5 o C/m in MMR and TMRWL from DTA-TG plots of VSP

y = 1.190x - 4.748
30 R² = 0.952 coals for the1st set and 0.716 for the 2nd set. The
25
equations derived are:
VM

20

15
rate: 10 oC/min
MMR=0.006 * (TMRWL) -2.551 for 1st set of samples
10

5
y = 1.061x + 0.003
R² = 0.987 (5)
nd
0 MMR=0.011 * (TMRWL) -4.404 for 2 set of samples
15 20 25 30 35 40
% Wt Loss (6)
VM (5 deg C/min rate) VM (10 deg C/min rate)

TMRWL Vs MMR

Fig. 2: % Wt Loss vs VM for two sets 1.6

1.4 y = 0.011x - 4.404

Fig. 3 depicts relationship between VM content 1.2

1
R² = 0.716
MMR

& TMRWL for 1st set of samples and 2 nd set of 0.8

0.6 y = 0.006x - 2.551
samples of VSP coals respectively. There is a 0.4
0.2
R² = 0.948

strong correlation i.e., R2= 0.95 and 0.987 for 1st 0

460 480 500 520 540 560 580

set and 2nd set respectively. TMRWL

MMR (5 deg C/min rate) MMR (10 deg C/min rate)

TMRWL Vs VM
40
y = -0.240x + 157.7
Fig. 4 :TMRWL vs MMR for two sets of samples
35
R² = 0.866
30
25 Fig 5 shows the relation between % Wt Loss
VM

20
15 y = -0.299x + 176.7 and MMR for both the sets of VSP coals with R2
10
5
R² = 0.871
> 0.94. The equations derived are:
0 MMR = -0.027 * (% Wt Loss) + 1.797 for 1st set of
460 480 500 520 540 560 580
TMRWL
samples (7)
MMR = -0.047 * (% Wt Loss) + 2.352 for 2nd set of
VM (5 deg C/min rate) VM (10 deg C/min rate)
samples (8)

Fig. 3: TMRWL vs VM for two sets % Wt Loss Vs MMR

As VM content increases, TMRWL decreases, thus 1.6

showing an inverse relationship with R 2 of 1.4

1.2
about 0.87 for both the sets. 1
ra te: 5 o C/m in
y = -0.047x + 2.352
MMR

%VM = -0.240 * (TMRWL) + 157.7 for1st set of sample 0.8 R² = 0.942

0.6
coals (3) 0.4
rate: 10 oC/min
y = -0.027x + 1.797

%VM = -0.299 * (TMRWL) + 176.7 for 2nd set of 0.2 R² = 0.941

0
sample coals (4) 15 20 25 30 35 40

% Wt Loss
Rank of Coals MMR (5 deg C/min rate) MMR (10 deg C/min rate)

Mean Max Reflectance of vitrinite (MMR) is the

rank parameter of coal. The reproducibility of Fig. 5: % Wt Loss vs MMR for two sets of
petrographic test for MMR determination as per samples

332
 MPT-2013

Temperature of Maximum Fluidity (TMF) 4. Conclusions

Fig. 6 gives the direc t dependenc e of
 TG-DTG thermograms of coals show that the
temperature of maximum Gieseler fluidity
maximum weight loss oc c urs in the
(TMF, 0C) on TMRWL for the two sets of VSP coals.
temperature range 400-6000C, followed by
While 1 st set of coals show a very strong
a gradual weight loss beyond 600 deg c.
correlation R2 = 0.91), the 2nd set of coals give
moderate dependence (R2 = 0.82). The equations  The temperature of maximum weight
are given below: loss(TMRWL) increases with increase in the
TMF = 0.547 * (TMRWL) + 155.9 for 1 st set of rank of coal and can be considered as a
samples (9) characteristic parameter for evaluation of
TMF = 0.737 * (TMRWL) + 81.22 for 2nd set of coal
samples (10)  TMRWL has a direct correlation with TMF as
determined in the gieseler Fluidity test and
T MRWL Vs TMF
475
also with the VM of the coals.
470 y = 0.737x + 81.22
465
R² = 0.819
 Wt loss up to 1000 0C from TG thermogram
460
correlates with rank (MMR), VM and TMF
TMF

455
450
reasonably well.
445
y = 0.547x + 155.9
440
R² = 0.913
435 Acknowledgements
480 500 520 540 560 580

TMRWL
Authors wish to acknowledge with thanks the
TMF (5 deg C/min rate) TMF (10 deg C/min rate)
Managements of G.V.P. College of Engineering
(Autonomous) and Vishakhapatnam Steel
Fig. 6: TMRWL vs TMF for two sets Plant for their support in carrying out the
Fig. 7 shows the relation between weight loss studies and extending the laboratory facilities
percent with temperature of maximum fluidity for the work.
(TMF) of coals. The equations derived are:
TMF = -2.233 * (% Wt Loss) + 509.9 for 1st set of References
samples with R2 = 0.938 (11)
TMF = -2.817 * (% Wt Loss) + 526.7 for 2nd set of Murty, J. V. S., Amit Parti., 2001. Internal Project
samples with R2 = 0.701 (12) report “Studies on Correlation between
Conventional Characteristics of Coal and
% Wt Loss Vs TMF
Coke with DTA-TG Plots”, Project No:
475 51:04:91, RDCIS, SAIL.
470
465
ra te: 5o C/min
y = -2.817x + 526.7 Ulanvoskii, M. L., Drozdnik, I. D., 1991. Coke &
R² = 0.701
460 chemistry. 1, 4-6.
TMF

455
450
Varma, A. K., 2002. Thermo gravimetric
rate: 10 o C/min
445
y = -2.233x + 509.9 investigations predic tion of c oking
440 R² = 0.938
435 behavior and coke properties derived from
15 20 25 30 35
% Wt Loss
inertinite rich coals. Journal of FUEL. 81,
1321-1334.
TMF (5 deg C/min rate) TMF (10 deg C/min rate)

Fig. 7: % Wt Loss vs TMF for two sets of samples

*******
333
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Studies on the Effect of Coal Beneficiation on Ash Fusion

Temperatures

Banashree Mahanta, Binoy K Saikia*, Arju Moni Dutta, Prasenjit Saikia and
Bimala P Baruah
Coal Chemistry Division, CSIR-North East Institute of Science & Technology, Jorhat-
785006, Assam, India
Abstract
In this investigation, the Ash Fusion Temperatures (AFTs) ranges of few beneficiated coals have
been reported. Coal sample have been treated by four different methods, i.e, oxidation, alkali
extraction and ultrasonication in presence of alkali. The major oxides of ash in raw and treated
coals are Fe2O3, Al2O3, SiO2, CaO and MgO. Initial Deformation Temperature (IDT) during Ash
Fusion Temperature analysis showed variations with the ash composition in coals and found to
be increased with increase in Fe2O3 contents in ash. The coal samples, characterized by XRD
analysis revealed that the peak intensities for different minerals change with the types of processes
adopted for beneficiation.

Keywords: Ash fusion temperature; ultrasonication; xrd; low rank coal; high sulfur coal.

1. Introduction is very variable and complex with carbon, the

ingredient of use, present as giant hydrocarbon
Coal is the result of the geologic al
molecules.
metamorphosis of plant material. The process
The study of the Indian coal indicated that the
of metamorphosis leads to a reduction in
majority of the reserves consist of weakly to
moisture, oxygen and hydrogen and an
non-c oking variety of bituminous, sub-
increase in percentage carbon. The degree of
bituminous and lignite nature distributed all
metamorphosis is termed “rank”. High rank
over India located at different depths. India, the
coals have low moisture and high carbon
third largest producer of coal in the world after
(Packer and Gray, 2000). Coal is considered from
China and USA, has a total reserve of about 286
the analytical viewpoint to consist of three
billion tonnes and lignite reserve of about 41
distinguishable components, coal substance,
billion tonnes as on 31.03.11. Coal in India has
minerals and moisture. Coal substance contains
increasing demand in near future for power
besides carbon, hydrogen and oxygen other
generation. Currently India has about 10% of
elements such as sulfur, nitrogen, calcium,
the world coal and major contribution come
boron and aluminium. The metallic elements
from North-Eastern part (Assam) (Takematsu
contribute to the coal ash. The structure of coal
and Maude, 1991). North-East region has
around 1.5 billion tonnes of coal reserves
* Correspending Author: bksaikia@gmail.com; Tel:+91-
3762372851 distributed in the states of Meghalaya, Assam,

334

Arunachal Pradesh and Nagaland having
indifferent physico-chemical attributes of low
ash, high heat value, high volatile matter, high
tar yielding during carbonization and per-
hydrous in nature with high sulphur content.
On the basis of physico-chemical analysis,
Assam coal can be classified as sub-bituminous.
Concern about greenhouse gas emissions and
the need for greater effic ienc y in power
generation have led to increasing interest in coal
beneficiation. For the present investigation,
Tirap, Assam coal was selected. For the point of
beneficiation four different treatments were
performed with the sample. The ashes of raw
and four treated samples were analyzed
chemically with standard method. Ash Fusion
Temperature (AFTs) can be considered as one
property that specific ally gives more
information on the suitability of a coal source
for combustion or gasification purposes. XRD
is an efficient analytical technique used to
identify and characterize unknown mineral
matter in coal and coal ash. The inorganic
constituents in coal are mainly minerals, which
are incorporated in various ways in the coal
itself. According to Clark et al. (1998) iron in
coal is associated with sulphur in the minerals
pyrite (FeS2), jarosite (KFe3(SO4)2(OH)6), troilite
and pyrrhotite (both FeS), and non-sulphur
c ontaining minerals suc h as ankerite
(CaFe(CO3)2),illite (clay mineral) and siderite
(FeCO3). Variations in the characteristics of
mineral matter in coal ash have a significant
bearing on the effectiveness of removal of
mineral matter during various treatments. The
mineral matter in coal is very significant to
many different coal utilization processes.
Phosphorus bearing minerals, for example, can
be transferred from coal to coke, and interact
with iron ore to provide difficulties in steel
production (Ward et al., 1996). Hence, the main
objective of this study is to see the effect of
beneficiation types on the AFT of the coals.
335
MPT-2013
2. Experimental Section
2.1. Preparation of samples
The coal sample (TR) from Tirap colliery of
Makum coalfield, Assam was selected for the
four different treatments. The raw sample was
oxidized with hydrogen peroxide in presence
of formic acid, mentioned as ‘TOX’. The second
sample, TOXA5H was prepared by alkali
extraction (1: 1 of KOH and NaOH) for 5 hour
after performing the process of oxidation as
done for the previous sample. Another sample
was prepared by the same process of extraction,
but without undergoing oxidation and coded
as TA5H. The untrasonication was done with
the raw sample in presence of same alkali
(TAUS). The ashes were prepared in muffle
furnace at highest temperature of 8150C, keeping
constant for 1 hour.
2.2. Ash analysis and fusion temperature test
The ash analyses were carried out by using
standard method (Himus, 1954; Vogel, 1969),
which are given in the table1. Ash fusion
temperature (AFT) measurements were carried
out by using Leitz Wetzlar ash fusion point
determination apparatus with maximum
temperature of 1600 ° C following Indian
Standard procedure (IS: 12891-1990). The ash
fusion temperature (AFT) ranges of the coal
samples are also reported in Table 1.
2.3. XRD Analysis
The XRD patterns of the coal ash samples were
taken in the X-ray diffractometer Model XPERT-
PRO (PHILIPS) using Cu k- alpha Fe filtered X-
radiation.
3. Results and Discussion
3.1. Fusion characteristics of raw and treated
coal ashes
The results of the ash analyses along with the
AFT ranges are summarized in the following
Table 1. It reveals that the majority of the coal
 MPT-2013

ash consists of SiO2 followed by Fe2O3. The AFT 3.2. Mineral transformations during various
are ranges from 1020 to 1500 0C. treatments
Table 1: Ash analysis (wt %) The identity of different minerals present in the
raw and treated coal ash and their
transformation during different treatments
AFT(0 C)
Ash SiO2 Fe2 O3 Al2 O3 CaO MgO
IDT HT FT were investigated from their XRD spectra. The
TR 3.51 47.8 28.8 15.7 1.07 0.13 1210 1360 1460
XRD d-values and their assignments are
TOX 2.61 39.07 26.10 12.03 0.05 0.15 1120 1300 1500
TOXA5H 1.62 37.9 9.08 11.4 0.01 0.12 1040 1320 1500 summarized in Table 2.
TA5H 2.02 35.2 20.36 13.5 0.13 0.08 1120 1340 1500
TAU 1.25 34.5 10.71 11.9 0.02 0.11 1060 1300 1480 Table 2: XRD d-values of the coal ash and their
assessment
3.1.1. Effect of Fe2O3 content
As iron in coal is predominantly in the form of S.N. d-spacing values(Å) Possible Assignments
ferric iron in both oxidizing and inert 1. 4.44 Illite(I)
atmosphere (Huffman et al., 1981). It is seen that 2. 4.44 Montmorillonite(M)

the AFT shows a significant change with the 3. 4.29, 3.35,1.81 Quartz(Q)

percentage of Fe2O3. It was reported that the 4. 4.29, 2.96,2.85, 2.67,2.19 Gypsum(G)

oxides that reduce the AFTs of the coal ashes 5. 3.67, 2.23,1.83 Calcite(C)

are in the order SO3>CaO>MgO> Fe2O3 (Li et al., 6. 3.67,2.69,2.51,2.19,1.83,1.69, 1.59,1.45 Hematite(H)

2011). However, AFTs gradually increases with 7. 3.67, 2.69 Kaolinite(K)

8. 2.85, 2.86 Dolomite(D)

increase in its concentration in the present
9. 2.85 Chlorite(Cl)
study.
10. 2.69,2.45,1.98 Aragonite(Ar)
3.1.2. Effect of CaO content 11. 2.45 Pyrite(P)

12. 2.45 Rutile (R)

With the increase of CaO percentage, IDT is
13. 1.37 Alumina(A)
found to be increased gradually. However, the
samples contain very less CaO as compared to
other coals (Song et al., 2010). It was observed that the peak intensity of the
3.1.3. Effect of SiO2 content different minerals changes with the types of the
treatments performed. Some of the minerals
The concentrations of SiO2 do not show any like Montmorillonite(M), Illite(I), Kaolinite(K),
significant change with the AFTs. Calcite(C) are found to be present in most of the
3.1.4. Effect of Al2O3 samples. The Hematite (H) peak is more intense
than that in the raw sample. On extraction with
With the increase of Al2O3 content the IDT is
1:1 alkalies(KOH:NaOH), some of the
gradually increasing. It is to be noted that the
minerals(e.g Hematite) disappears. The
gradual increase of AFTs is may be due to
minerals whose intensity were reduced include
refractory nature of Al2O3.
Calc ite(C), Hematite(H), Illite(I),
3.1.5. Effect of MgO Montmorillonite(M), Gypsum(G), Rutile(R),
It is observed that the IDT gradually decreases Kaolinite(K). The peak intensity is of the
minerals e.g. Quartz (Q), Illite(I),
with increase of MgO.
Montmorillonite(M), Kaolinite(K) in TA5H are
also found to be reduced after alakali extraction

336

for 5 hours. However, the peak intensity for
minerals like Hematite(H), Calc ite(C),
Gypsum(G), Rutile(R) were enhanced during
the extrac tion. Thus, there are drastic
transformations of minerals during the specific
treatments as carried out. There is a need of
more in depth studies to follow this
transformation.
4. Conclusions
In present investigation, it was found that the
Ash Fusion Temperature ranges (AFT) generally
increases with the increase in Fe2O3, CaO, Al2O3
contents in coals. The AFTs more or less
increases with SiO 2 contents in coals and
decreases with increase in MgO contents. The
XRD analysis revealed the presence of minerals
inc luding Illite(I), Montmorillonite(M),
Quartz(Q), calcite(C), Gypsum(G), Hematite(H),
Kaolinite(K), Dolomite. It also revealed the
occurrences of mineral transformations during
their various treatments like oxidation and
alkali treatments, which in turn affect the AFTs.
Reference
Clarke, T. M., Evans, B. J., Wynter, C., Pollak, H.,
Taole, S. and Ratc liffe, D., 1998.
Investigation of virgin coals subjected to
a mild acid treatment. Hyp. Interact. 112,
227-230.
*******
337
MPT-2013
Feng-hai Li , Jie-jie Huang , Yi-tian Fang, Yang
Wang, 2011. The effects of leaching and
floatation on the ash fusion temperatures
of three selected lignites. Fuel 90, 2377–
2383.
G.W. Himus (Ed.) 1954. Fuel Testing, Laboratory
Method in Fuel Technology. Penguin,
London, 67-78.
Huffman, G.P., Huggins, F.E., Dunmyre, G.
R.,1981. Investigation of the high-
temperature behaviour of coal ash in
reducing and oxidizing atmospheres. Fuel
60, 585-597.
John Pac ker and Dr Vinc ent Gray with
information from “Coal Researc h
Analysis Update”, Coal Researc h
Association of New Zealand Inc.1998.
Song, W. J., Tang, L. H., Zhu, X. D., Wu, Y. Q.,
Rong, Y. Q., Zhu, Z. B., Koyama, S. 2009.
Fusibility and flow properties of coal ash
and slag. Fuel 88, 297–304.
Takematsu T, Maude C. Coal gasification for
IGCC power generation 1991. ICEAR/37
IEA Coal Research, London.
Vogel, A. J., 1969. A Textbook of Quantitative
Inorganic Analysis, Including Elementary
Analysis, Longman, London.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Beneficiation of Low Rank North East Indian Coals by

Ultrasonication in Ionic Liquids: A Green Approach

Arju Moni Dutta, Binoy K Saikia*, Lakshi Saikia and Bimala P Baruah
CSIR-North East Institute of Science and Technology, Assam, Jorhat -785006, India

Abstract
The presence of sulphur and mineral matters (ash) in coal is undesirable for its utilization in the
thermal plants. There are several chemical, physical, biological techniques for removal of sulphur
and ash from coal. Application of ultrasonic energy and ionic liquids has been recently practiced
for beneficiation of coals. Our present investigation reports the ultrasonication (20 kHz) of North
East Indian coals in presence of ILs (Ionic Liquids).The effect of ultrasonication time in
desulphurization and deashing is studied. Desulphurization of Bapung coal is found to increase
from 17.80% to 28.69% by ultrasonication with increasing time from one to three hours. Similarly,
Tipong coal shows an increase from 7.62% to 11.86% with increase in time. Ultrasonication in ILs
is not so effective in deashing of the coals during this study. The XRD and FT-IR analysis of raw
and beneficiated coal samples are also discussed. The peak analyses in FT-IR and XRD spectra
have revealed the removal of sulphur and ash from the coal samples.The ILs could be reused for
subsequently, and the process seems to be environmentally sustainable.

Keywords: Ultrasonication; ionic liquids; high sulphur coal; FT-IR; XRD.

1. Introduction which is also danger to human health and

contribute to acid rain, while the mineral matter
Coal imparts hazards to the surroundings if it
of coal is converted into ash during combustion
is utilized before cleaning. The North-Eastern
and deterioration of the turbine blade and boiler
region (NER) of India contains sub-bituminous
(Mukherjee et al 2001) Thus, desulfurization and
type coals with high sulfur (2-8%) with mainly
deashing of coals are very much essential at any
(75-90%) in organic form. They also have ash
cost to sustainable utilization. Several chemical
(>10%) contents, which may create problems
treatments for deashing and desulfurization of
during utilization. Five types of organic Sulfur
coals were carried out by many investigators.
functionalities was found to be present in these
Several researchers used aqueous hydrogen
coals, viz. aliphatic or aromatic thiols, aliphatic
peroxide, sulfuric acid and molten NaOH to
or mixed sulfides, aliphatic or aromatic
remove sulfur and ash from coals at different
disulfides, heteroc yc lic c ompounds of
temperatures (Ahnonkitpanit &. Prasassarakich
thiophenic types etc (Borah et al. 2005). During
1989; Baruah & Khare 2007; Kara & Ceylan 1988;
combustion of coal, sulphur converts to SO2,
Araya et al 1981) However, these chemical
* Correspending Author: bksaikia@gmail.com processes may create hazards to the

338

surroundings. This process also requires extra
investment in chemicals and related apparatus.
In this present study, the coal samples were
extracted with ionic liquids (ILs) in presence of
Ultrasound wave. IL is used here as green
solvents.
1.2 Ionic liquids: green chemicals
Ionic liquids are composed solely of anions and
cations. These are essentially non-volatile
molten salts with a melting point less than
100ºC.Ionic liquids come in two main categories,
namely simple salts (made of a single anion and
cation) and binary ionic liquids (salts where
equilibrium is involved). For example,
[EtNH3][NO3] is a simple salt whereas
mixtures of aluminum(III) chloride and 1,3-
dialkylimidazolium chlorides (a binary ionic
liquid system) contain several different ionic
species, and their melting point and properties
depend upon the mole frac tions of the
aluminum(III) chloride and 1,3-
dialkylimidazolium.
Ionic liquids (ILs) have been employed
extensively as Green solvents due to the
c harac teristic s of nonvolatility,
nonflammablity and high thermal stability.
Thus, these are employed in processes of
catalysis, chemical synthesis and separations.
The use of ILs as extractants to remove aromatic
sulfur c ompounds by extrac tive
desulfurization has been reported in recent
research studies (Bösmann et al 2001; Lo et al
2003; Huang, et al 2004; Zhang et al 2002a;
2004b; Nie et al 2006a, 2007b; Zhao et al 2007;).
Most of the literatures have described with ILs
as simple extractant. The results indicate that
ionic liquids can effectively extract the sulfur
contents from the oil phase of liquid fuels. Wen-
Hen Lo and coworkers (Lo et al 2003) using H2O2
- acetic acid as the oxidant in presence of
[BMIM]BF4 and [BMIM]PF6 as the extractant.
Our present investigation inc ludes the
extraction of sulfur from high sulpur coals using
339
MPT-2013
Ultrasound in aqueous medium and ILs as the
extractant.
Sound waves having frequencies higher than
those to which human ear can response is called
ultrasound. Ultrasonic wave can be used for
the beneficiation of coal by removal sulphur as
well as ash.Ultrasound in the range of 20 to 100
kHz, which produces high energy waves
sometimes referred to as power ultrasound
2. Experimental
The low to high ash and medium to high
sulphur coal samples were collected from
Assam and Meghalaya states and ground to -
72 BS. The proximate analysis of coal samples
were done by using Thermogravimetric
Analyser (TGA 701; M/S Leco Corporation,
USA). Total sulphur was determined by
sulphur determinator (Leco Corporation, USA)
and the forms of pyritic sulphur and sulphate
sulphur were determined by standard method
(ASTM D 2492). The percent organic sulphur
was calculated by difference. The FT-IR spectra
of the coals and treated samples were recorded
in Perkin Elmer system 2000, Model 640B
(wavelength 400-4000 cm-1 with an accuracy of
+3 to -3) using KBr pellet with same weight of
dried coal samples and KBr. The XRD spectra
was obtained inX ray Diffractometer (Model:
Rigako, ULTIMA IV)
In a Teflon beaker, 20 gm of the coal sample was
mixed with 100 ml H2O and 3 ml IL (1 Butyl -3-
methylimidazolium tetrafloroborate) and then
the mixture was exposed to the ultrasound
treatment of frequency 20 kHz in the Ultrasonic
Processor (Sonapros PR-1000 M) at atmospheric
pressure. Duration of ultrasonication was
increased from 1 hr to to 3 hrs by taking
different coal samples, water and IL mixtures.
A sensor was given to the reaction mixture to
detect the reaction temperature. Then, the each
mixture of coal and water was filtered, washed
until pH becomes neutral.
 MPT-2013

3. Results and Discussions Two classes of chemical effect (Webster 1963)

Table 1 and Figure 1 have demonstrated that
the desulfurization is increased with the
duration of the time of ultrasonication for both
the coal samples. However, the ash removals of
the coal samples during ultrasonication are not
linear.
Fig1: Effect of time of ultrasonication
on desulphurization and deashing
2.1 Mechanism of Ultrasonic Coal
Desulphurization in Aqueous medium
Ultrasound in aqueous medium produces
highly reactive species such as OH radicals,
H2O2 and ozone that are strong oxidizing agents
of high oxidation potential (2.8, 1.8 and 2.1 V
respec tively). These radic als initiate and
enhance the oxidation and reduction reactions.
are induced by ultrasonic cavitations viz.
acceleration and cavitations
Moreover, intense ultrasound (Makino et al
1982) c auses c hemic al damage through
c avitations. The highly-reac tive radic als
produced during cavitation can be observed by
spin traps or other methods (Riesz et al., 1985;
Christman et al., 1987; Misik &Riesz, 1994;
Margulis, 1994; Luche, 1994; Jana and
Chatterjee, 1995; Henglein, 1995). Thus, the free
radicals produced by the cavitations effect are
responsible for reaction (Henglein, 1995). The
OH radicals produced by the ultrasound are
strong oxidation agents and lead to H 2O 2
formation.
2.2. Mechanism of Extractive desulphurization
by Ionic Liquids (ILs)
The ultrasonic ation in aqueous medium
produces highly reactive OH radicals which
dissolved in the ILs and oxidizes the sulphur
compounds to the corresponding sulfone. The
polarity of the sulfone was high and thus it
remained in the IL phase (Zhao et al 2009). . It
shows that the sulfur compounds enters into
the IL phase and get easily oxidized by
hydroxyl radicals to form S=O functional
groups.

Table: Physico-chemical characteristics of raw and ultrasonicated coal samples (wt %)

Samples M Ash VM FC SS PS OS Deashing TS Desulphuri

zation
MB 4.30 17.80 33.90 44.00 1.18 0.67 1.74 ----- 3.59 ------
MB+IL+US1hr 2.86 17.20 36.50 43.40 098 0.42 1.55 3.37 2.95 17.80
MB+IL+ US 2hrs 2.00 16.20 35.90 45.90 0.91 0.37 1.53 8.98 2.81 21.72
MB+IL+ US 3hrs 2.74 16.60 37.20 43.50 0.75 0.30 1.51 6.74 2.56 28.69
TPNG 2.40 3.68 42.80 51.10 0.17 0.10 0.91 ------ 1.18 -----
TPNG+IL+ US 1hr 1.50 3.32 41.30 53.8 0.13 0.06 0.90 9.78 1.09 7.62
TPNG+IL+ US 2hrs 1.77 3.44 41.40 53.30 0.11 0.06 0.90 6.52 1.07 9.32
TPNG+IL+ US 3hrs 1.56 3.33 41.50 53.60 0.10 0.04 0.90 9.51 1.04 11.86

M: moisture; VM: volatile matter; FC: fixed carbon; SS: sulphate sulphur; TS: total sulphur; OS:
organic sulphur

340
 MPT-2013

Figure 2: Summary of the oxidation mechanism

of organic sulfur compounds in IL medium
2.3. FT-IR analysis of the raw and the
ultrasonicated coal samples
The FT-IR characterizations of the coals are
performed by usning available literatures
(Silverstein et al 1981); Baruah et al 2001; Kumar
and Srivastava 2013) and given in Table 2. The
changes in the FT-IR spectra (Figure 4) reveals
that the organically bound sulfur has been
converted to sulfoxide (S=O) and sulfone (-SO2)
on ultrasonication in aqueous medium in
presence of ionic liquids. The IL treated
ultrasonicated coal samples shows increase in
intensities in their FT-IR spectra due to the
formation of the sulfone groups. The
mec hanism of this desulfurization by
ultrasound in presence of ionic liquids (in
aqueous medium) may be depicted by Figure
2.The peak for SO 42- in raw coals disappear
completely after ultrasonication. It indicates
that the inorganic sulphur groups are easier to
be removed by ultrasonication in aqueous
medium.
Table 2: FT-IR assignments of sulphur
functionalities
Fig 3: FTIR spectra of raw and ultrasonicated
coal samples
2.4. XRD analysis of raw and ultrasonicated
coal samples
The XRD analysis of ultrasonicated samples is
carried out and the probable minerals present
in the coal samples are shown in the Fig. 4. We
observed that the coal samples mainly contain
minerals like kaolinite, quartz, hematite, pyrite
and others, (Nayak and Sing, 2007), which are
common minerals found in the coals of NE India.
However, the diffraction peaks of some of the
minerals became weak or disappeared after
ultrasonic treatment. It suggests that the
ultrasonication enhances the coal particles
breakage into small piec es, so that the
deoxidizers c an easily ac c ess the
macromolecular structures of coal. Thus, the
ultrasonic enhancement can also improve the
reac tion probability, inc reasing the
desulfurization efficiency of coals.
3 hrs ultrasound
2 hrs ultrasound

FUNCTIONAL GROUPS TRANSMITTANCE (cm -1 )

Thiol or thioether (CH2 -S-,C-S) 710-685
Intensity %

Thioether (CH3 -S) 660-630

Aryl thioether (S-S) 715-670
Disullfide (C-S) 705-570 1 hr ultrasound
Disulfide (S-S) 620-600
Aryldisulfide (S-S) 500-430 Q
Polysulfides (S-S) 500-470
raw coal without
Sulfate ion( SO4 2- ) 1130-1080 / 680-610 K ultrasound
Sulfixide (-SO-) ≈ 1050 H P H
Sulfone (-SO2 -) ≈ 1300(Asymetrical), ≈ 1150
(Symetrical) 20 40 60 80 100
≈ 1150 (Symetrical) 2 theta(degree)

341

Fig 4: XRD spectrum of ultrasonicated coal
samples (K: kaolinite, Q: quartz, H: hematite,
P: pyrite)
Conclusions
The Ultrasound energy can be used for the
beneficiation of high sulphur coals without
using hazardous chemicals. The use of ionic
liquids (ILs) makes the process more eco-
friendly and safe.
References
Ahnonkitpanit, E., Prasassarakich, P., 1989. Coal
desulfurization in aqueous hydrogen
peroxide. Fuel 68,819-824.
Araya, P.E., Ohlbaum, R.B., Droguett, S.E., 1981.
Study of the treatment of sub-bituminous
coals by NaOH solutions, Fuel 60, 1127-
1130.
Baruah, B. P. , Khare, P., 2007. Desulphurization
of oxidized coals with Solvent Extraction
and alkali treatment. Energy & Fuels, Vol.
21, 2156-2164.
Borah, D., Baruah, M. K.; Haque, I., 2001. Fuel,
80, 501-50 Borah, D., Borah, M.K., Haque,
I., 2005. Oxidation of high sulfur coal. Part
3. Desulphurization of organic sulfur by
peroxiacetic acid (produced in situ) in
presence of metal ions. Elsevier, Fuel
Processing Technology 86, 959-976.
Bösmann, A., Datsevich, L., Jess, A., Lauter, A.,
Schmitz, C.,Wasserscheid, P. 2001. Deep
desulfurization of diesel fuel by extraction
with ionic liquids. Chem. Commun., 2494–
2495.
Christman, C.L., Carmichael A.J., Mossoba MM,
Riesz P., 1987. Evidence for free radicals
produc ed in aqueous solutions by
diagnostic ultrasound. Ultrasonics 25, 31–
34.
Gogate, P.R., Tatake, P.A., Kanthale. P.M., Pandit,
A.B.,2002. Mapping of sonochemical
342
MPT-2013
reac tors; Review, analysis and
experimental verification. AIChE J 48,
1542–1560.
Henglein, A.,1995. Chemic al effec ts of
continuous and pulsed ultrasound in
aqueous solutions. Ultrason Sonochem
2,115–121
Hoffmann, M.R., Hua, I., Hochemer, R.,1996.
Application of ultrasonic irradiation for
the degradation of chemical contaminants
in water. Ultrasonic Sonochemistry 3,163–
172.
Huang, C.P.,Chen, B.H.,Zhang, J., Liu, Z.C., Li,
Y.X., 2004. Desulfurization of Gasoline by
Extraction with New Ionic Liquids. Energ.
Fuel. 18, 1862–1864.
Jana, A.K., Chatterjee, S.N.,1995. Estimation of
hydroxyl free radic als produc ed by
ultrasound in Fricke solution used as a
chemical dosimeter. Ultrason Sonochem
2,87–91
Kara, H., Ceylan.R.,1988. Removal of sulfur
from four central Anatolian lignite’s by
NaOH, Fuel 67 , 170-172.
Kumar, A., and Srivastava,S. Pattern of Sulphur
Functional Groups in High Sulphur Ledo
Coals of Assam . Journal of Applied
Chemistry (IOSR-JAC). 4, 01-08.
Lo, W.H.; Yang, H.Y.; Wei, G.T., 2003. One-pot
desulfurization of light oils by chemical
oxidation and solvent extraction with
room temperature ionic liquids. Green
Chem. 5, 639–642.
Luche, J.L., 1994. Effect of ultrasound on
heterogeneous system. Ultrason Sonochem
1,111–11
Makino, K., Mossoba, M.M., Riesz, P., 1982,
Chemical effects of ultrasound on aqueous
solutions evidence for OH- and H+ by spin
trapping. J Am Chem. Soc 104, 3537–3539.
Margulis, M.A., 1994. Fundamental problems
of sonoc hemistry and c avitations.
Ultrason Sonochem 1, 87–90.

Misik, V., Riesz, P., 1994. Free radicals formation
by ultrasound in organic liquids: a spin
trap and EPR study. J Phys Chem 98, 1634–
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Mukherjee, S., Mahiddin, P., Borthakur, C.,
2001.Demineralization and
Desulphurization of sub bituminous coal
using hydrogen peroxide. Energy Fuels 15
1418-1424.
Nayak, S., P,Sing, B. K., 2007.Instrumental
c harac terization of c lay by
XRD,XRF,and XRF;Indian Academy of
Sciences,30 . 235-238.
Nie, Y., Li, C.X.; Wang, Z.H., 2007Extractive
Desulfurization of fuel oil using
alkylimidazole and its mixture with
dialkylphosphate ionic liquids. Ind. Eng.
Chem. Res. 46, 5108–5112.
Nie, Y.; Li, C.X.; Sun, A.J.; Meng, H.; Wang, Z.H.
2006 . Extrac tive desulfurization of
gasoline using imidazolium-based
phosphoric ionic liquids. Energ. Fuel. 20,
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Riesz, P., Berdahl, D., Christman, C.L., 1985. Free
radical generation by ultrasound in
*******
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aqueousand non-aqueous solutions.
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Silverstein, R. M.; Bassler G. C.; Morrill, T.
C.,1981. Spectrometricidentification of
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48.
Zhang, S.G.; Zhang, C.Z., 2002 . Novel properties
of ionic liquids in selective sulfur removal
from fuels at room temperature. Green
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Zhang,S.G., Zhang, Q.L., Zhang, C.Z., 2004 .
Extrac tive desulfurization and
denitrogenation of fuels using ionic liquids.
Ind. Eng. Chem. Res. 43, 614–622
Zhao, D., Wang, Y., and Duan, E.,2009. Oxidative
Desulfurization of Fuel Oil by Pyridinium-
Based Ionic Liquids. molecules 14, 4351-
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desulfurization of diesel fuel using a
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Chem. 9, 1219–1222
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Washability Characteristics of Kusmunda Seam Coals, Korba

Coalfield

A.K. Chattopadhyay, M.K. Sethi and S.K. Konar

CSIR- Central Institute of Mining and Fuel Research, Bilaspur Unit

Abstract
Son-Mahanadi Valley Coalfields is endowed with vast resources of low grade low rank non coking
coals occurring as very thick and highly inter banded seams. Their near surface occurrence has
imparted additional importance to them as mostly they are exploitable through open cast mining.
Korba is one such coalfield where Kusmunda group of seams, viz. upper and lower Kusmunda,
has become the centre of attraction for its vast thickness and potentiality to be used as a prime
resource for power generation. However throughout its thickness the coal quality is very much
inconsistent due to the presence of dirt bands of varying quality and thickness as also varied
inherent dirt contents of coal bands. As such the coals, due to their poor quality, require
beneficiation before being fed into the pulveriser-boiler system of a power plant. Since the quality
of a thick seam varies from section to section and bench to bench during conventional mining, it
is difficult to predict the washability character of ROM coals from a thick seam in the long range
of time. However, a number of washability studies from ROM samples of different times show
that despite the change of quality of coals they bear some common characteristics those make
them predictable as also easily washable through a single washing system.
The present study encompasses 4 ROM samples from different projects working on Kusmunda
seam with head ash varying from 35.2 to 55.6. It can be observed from the study that specific
gravity cut point around 1.9 produce cleans with around 32 percent ash (suitable target for
power plant use) and the cut point eventually coincides with the lowest NGM level in most of the
cases. It shows that the dirt bands occurring throughout the entire thickness of the seam bear
similar lithological character and their prevalence in any chosen section only affects the head ash
of the ROM and subsequently the yield percentage on washing with very little effect on the
difficulty level of washing.

1. Introduction coal seams and finally upper Barakar which is

characterized by the occ urrence of thick
Kusmunda group of seams constituting upper
interbanded low rank, low grade coal seams of
and lower Kusmunda and Kusmunda A seam
Kusmunda group. A further set of seams termed
occur in the southern part of Korba coal field.
as satellite seams overlie Kusmunda seams and
Stratigraphically Barakar measures of that area
are well developed towards western side of the
is divided into 3 parts viz., lower Barakar with
basin. These seams are yet to be exploited. The
relatively thin coal seams of good quality
coalfield is geographically divided into two
followed upward by a middle zone without any
parts separated by one east west trending

344

intra- basinal normal fault. Towards the
northern side lie the lower Barakars with a set
of thin seams known Ghordewa or Rajgamar
group of seams. Towards southern side of the
fault, i.e. the down thrown side occurs the
Kusmunda group of seams and the satellite
seams with formidable thickness of 20 to 75
meters and vast reserves of low grade coal of
around 10 billion tons. These coals are extracted
through a number of coal India mining projects
viz., Kusmunda, Gevra and Dipka. The mining
activity is stretched along the east west strike
length of about 16 km with a target output of
more than 50 million tons per annum. The coals
are mostly used in different thermal power
stations including NTPC and State electricity
board and a number of private power plants.
Besides, these coals are also dispatched to other
State electricity generation companies of Gujrat,
Rajasthan etc.
Throughout its enormous thickness the seams
show different kinds of dirt bands of varying
thickness. Since the whole thickness cannot be
accessed in single mining operation, the coals
are used to be mined in different benches.
Presently the surface miners are also being
used. Thus the mine produce varies widely in
the quality from place to place and bench to
benc h. However, due to Gover nment
stipulation, these coals require beneficiation for
reduction of ash before its use in power plant
boilers. A number of coal washeries have come
up in this area to cater washed coal to the users,
who initially went for laboratory c oal
beneficiation study data to plan their washery
designs. A number of such studies were done
by CIMFR (erstwhile CFRI) Bilaspur Unit. The
findings of those studies show despite wide
variation in quality, there are some common
washability characteristics in Kusmunda coals
which makes them easily washable through a
single washing system.
The present work comprises comparative
study of 4 Lab scale washability studies of ROM
345
MPT-2013
coal with ash content varying from 35.2 to 55.6
percent. The samples were collected from
different locations (different mining projects)
at different times ranging over a period of more
than 5 years. Yet the findings show some
remarkable similarity in the washability
characteristics of all those coals.
2. Washability Study
The four ROM samples, termed as ROM-1,
ROM-2, ROM-3 and ROM-4 have been selected
for the study on the basis of their variation in
quality in terms of ash percent and geographic
location. The samples were studied during the
time span from 2007 to 2012.
ROM-1 was collected from Kusmunda open cast
mine. After sc reen analysis, the +50mm
materials were subjected to crushing by
mechanical means and the crushed fractions
were again screened. Both natural size fractions
of -50mm materials and the crushed fractions
were mixed to get the 50w washability sample.
The fine size materials below 0.5 mm were left
unwashed and float and sink tests were done
on (50 – 0.5) materials. The head ash of the
washability sample was 49.9 percent on dry
basis. ROM-2 was who c ollec ted from
Kusmunda OCP and processed in the same
way. The head ash (dry) in this case is 35.2
percent only. ROM-3 was collected from Gevra
open cast mine and processed to get (100 – 5)
mm size washability sample with head ash
(dry) of 55.6 percent. ROM-4, also processed for
(100 - 5) mm washability sample with 47.0
percent ash on dry basis was collected from
Dipka open cast mine. The detailed washability
study data are given in Table no. 1-4. Also near
gravity materials (NGM) were calculated for
all specific gravity fractions and incorporated
in the tables. The NGM percent present have
been used as the main tool for comparison of
their washability characteristics.
 MPT-2013

Table 1: ROM-1 Washability studies of ROM Kusmunda Open Cast Mine Korba Coal Field
(Raw Coal x 100 mm) Size:(50-0.5)mm Dry Ash % - 49.9 Wt%= 93.4
Sp. Gr. Fractional Fractional Cumulative Cumulative Near
Dry Floats Sinks Chracteristic Mayer's
Gravity
Wt% pt.value
Wt.% Ash% Wt.% Ash% Wt.% Ash% Material
Floats at 1.30 3.2 3.5 3.2 3.5 96.8 51.4 1.6 0.1 15.7
Floats at 1.40 12.5 15.1 15.7 12.7 84.3 56.8 9.5 2.0 25.8
Floats at 1.50 13.3 26.6 29.0 19.1 71.0 62.5 22.4 5.5 23.4
Floats at 1.60 10.1 37.0 39.1 23.7 60.9 66.7 34.1 9.3 21.8
Floats at 1.70 11.7 43.8 50.4 28.3 49.6 71.8 45.0 14.3 20.1
Floats at 1.80 8.4 50.8 59.2 31.5 40.8 76.6 55.0 18.6 13.4
Floats at 1.90 5.0 55.4 64.2 33.4 35.8 79.5 61.7 21.4 10.0
Floats at 2.00 5.0 62.0 69.2 35.5 30.8 81.4 66.7 24.6 35.8
Sinks at 2.00 30.8 81.4 100.0 49.9 84.6 49.9

Table 2: ROM-2 Washability studies of ROM Kusmunda Open Cast Mine Korba Coal Field
(Raw Coal x 100 mm) Size:(50-0.5)mm Dry Ash % - 35.2 Wt%= 93.1
Sp. Gr. Fractional Fractional Cumulative Cumulative
Dry Floats Sinks Near
Characteristic Mayer's
Gravity
Wt% pt. value
Wt.% Ash% Wt.% Ash% Wt.% Ash% Material

Floats at 1.30 12.3 6.2 12.3 6.2 87.7 39.3 6.2 0.8 34.7
Floats at 1.40 22.4 16.0 34.7 12.5 65.3 47.3 23.5 4.3 42.7
Floats at 1.50 20.3 28.0 55.0 18.2 45.0 56.0 44.9 10.0 34.0
Floats at 1.60 13.7 38.2 68.7 22.2 31.3 63.7 61.9 15.3 20.7
Floats at 1.70 7.0 46.1 75.7 24.4 24.3 68.8 72.2 18.5 12.3
Floats at 1.80 5.3 52.9 81.0 26.3 19.0 73.1 78.4 21.3 10.1
Floats at 1.90 4.8 59.3 85.8 28.1 14.2 78.1 83.4 24.1 8.0
Floats at 2.00 2.8 63.1 88.6 29.2 11.4 81.8 87.2 25.9 14.2
Sinks at 2.00 11.4 81.7 100.0 35.2 94.3 35.2

Table 3: ROM-3 Washability studies of ROM Gevra Open Cast Mine Korba Coal Field (Raw
Coal x 100 mm) Size:(100-0.5)mm Dry Ash % - 55.6 Wt%= 96.0
Sp. Gr. Fractional Fractional Cumulative Cumulative Mayer's Near
Dry Floats Sinks Characteristic
pt. Gravity
Wt%
Wt.% Ash% Wt.% Ash% Wt.% Ash% value Material
Floats at 1.30 2.9 5.7 2.9 5.7 97.1 57.1 1.5 0.2 16.9
Floats at 1.40 14.0 16.6 16.9 14.7 83.1 63.9 9.9 2.5 31.1
Floats at 1.50 17.1 26.8 34.0 20.8 66.0 73.5 25.5 7.1 24.6
Floats at 1.60 7.5 37.2 41.5 23.8 58.5 78.2 37.8 9.9 12.8
Floats at 1.70 5.3 44.8 46.8 26.1 53.2 81.6 44.2 12.2 9.0
Floats at 1.80 3.7 52.7 50.5 28.1 49.5 83.7 48.7 14.2 6.0
Floats at 1.90 2.3 58.2 52.8 29.4 47.2 84.9 51.7 15.5 3.7
Floats at 2.00 1.4 62.0 54.2 30.2 45.8 85.6 53.5 16.4 47.2
Sinks at 2.00 45.8 85.6 100.0 55.6 77.1 55.6

Table 4: ROM-4 Washability studies of ROM Dipka Open Cast Mine Korba Coal Field (Raw
Coal x 100 mm), Size:(100-0.5)mm Dry Ash % - 47.0 Wt%= 93.5
Sp. Gr. Fractional Fractional Cumulative Cumulative Near
Dry Floats Sinks Characteristic Mayer's
Gravity
Wt% pt. value
Wt.% Ash% Wt.% Ash% Wt.% Ash% Material
Floats at 1.30 5.0 4.7 5.0 4.7 95.0 49.2 2.5 0.2 18.0
Floats at 1.40 13.0 15.4 18.0 12.4 82.0 54.6 11.5 2.2 31.1
Floats at 1.50 18.1 26.7 36.1 19.6 63.9 62.5 27.1 7.1 29.4
Floats at 1.60 11.3 36.9 47.4 23.7 52.6 68.1 41.8 11.2 21.4
Floats at 1.70 10.1 44.0 57.5 27.3 42.5 73.8 0.0 15.7 16.3
Floats at 1.80 6.2 51.6 63.7 29.6 36.3 77.6 60.6 18.9 10.1
Floats at 1.90 3.9 58.0 67.6 31.3 32.4 80.0 65.7 21.1 6.0
Floats at 2.00 2.5 61.7 70.1 32.4 29.9 81.4 69.4 22.7 32.4
Sinks at 2.00 29.9 81.4 100.0 47.0 85.1 47.0

346

3. Observation
Since the coal quality required for power plant
boilers is with around 34 percent of dry ash, all
the ROM samples were studied to find a
suitable specific gravity cut point to get that. In
ROM-1 the cut point comes around 1.90 in
ROM-2 (with lowest head ash of the lot), ROM-
3 and ROM-4 they lie slightly above 2.0 specific
gravity.
It is seen that sinks at 2.00 specific gravity
contains 81-85 percent ash and their weight
percent (30.8, 11.4, 45.8, and 29.9 for ROM-1, 2,
3 and 4 respectively) varied inversely with
clean coal yield at 32-34 percent dry ash level.
It can also be seen from the washability data
that specific gravity cut at 1.90 show lowest
NGM Level where fractional ash percent is very
much alike. They are 55.4, 59.3, 58.2 and 58.0
respectively for ROM- 1 to 4 with a variation
within only 4 percent. Maximum concentration
of NGM in all the cases is in specific gravity cut
of 1.40 and 1.50 followed by a steady decrease
and a sudden rise at 2.00. Perhaps this has a
direct impact on yield at 1.90 specific gravity
cut point.
4. Conclusion
From the above study it is revealed that the
dirt bands present in different sections of the
entire thickness of Kusmunda group of seams
bear similar lithological character and those
lithofacies persists throughout the working
area of different mines. Their abundance in any
*******
347
MPT-2013
chosen section affects the head ash of the coals
of that part and the theoretical yield of the
cleans that may be obtained on washing. It can
also be observed that specific gravity cut point
for obtaining desired dry ash level of 34 percent
is higher than the lowest NGM level except for
ROM-1 thereby making the coal moderately
difficult for washing. However, coal show much
easy washability character in target ash of
around 30 percent with much less sacrifice of
yield of cleans.
Acknowledgement
The authors are grateful to Director, CSIR-
CIMFR for his kind permission to undertake the
study and prepare the paper for presentation
in seminar.
References
Chattopadhyay, A. K., Tatwadi, S. T., 1991.
Resource Potential of Power Coals in
Korba Coalfield, Proceedings of National
Workshop on Coal Exploration.
Indian Standards IS-6345, 1971
Raja Rao,C.S., Coalfields of India, vol.III (G.S.I.
Bull. A no.45)
Sarkar. G. G, An introduc tion to Coal
Preparation Practic e, Oxford & IBH
Publishing Co. Pvt. Ltd.
Unpublished project reports of CFRI/CSIR-
CIMFR Bilaspur Unit, 2007-2012
Whitaker, J. W., and Sarkar, G. G., 1950-51.
Studies on Coal Washability, Parts 1-6
(CFRI Publication)
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Scope of Selective Washing of Thick Interbanded Coal Seams: Few

Case Studies

A.K. Chattopadhyay, M.K. Sethi and S.K. Konar

CSIR- Central Institute of Mining and Fuel Research, Bilaspur Unit

Abstract
Thick interbanded coal seams of Son-Mahanadi Valley coalfields attained tremendous importance
for power generation due to their vast resources and near surface occurrence that imparted easy
minability through open cast mining methods. However, in almost all the cases the ROM coals of
these mining projects, conventional washing before their end use in power plants is almost
imperative due to their poor quality owing to the presence of much external dirt bands within the
seams. It has been seen that all these coals show some characteristic trend in distribution of dirt
particles in different size fractions of the mine produce. The higher size fractions, viz. +200mm/
+100 mm etc. show higher ash due to two reasons. The dirt bands are harder than coals and break
less easily thus gets concentrated in higher size fractions and secondly bigger pieces of coal contain
parts of dirt bands within it which might have liberated on further breaking. It is also seen that
percentage of ash reduces in lower size fractions and below 13 mm size fraction the ash content
becomes 8-10 percent lower than the ROM. On crushing the whole coal for washing these low ash
materials get affected with the finer fragments of higher materials and thus the product of
secondary crushing show marginal difference of ash in crushed size fractions. In the present work
a few cases of laboratory scale coal preparation and washability studies are presented where it
has been observed that separation of lower size slacks through screening followed by crushing of
the higher size materials and their subsequent washing gives good result. Mixing of unwashed
lower ash natural slacks may effectively increase the overall yield and thus the desired beneficiated
product may be obtained at less cost and energy. Case studies from Kusmunda and Lajkura seam
coals have been presented in the paper show though washing of the whole coal crushed to desired
top size (barring -0.5 fraction) gives a slightly better result but cost and energy involved in
crushing, screening and actual washing through the alternative route is much less.

1. Introduction of combustion technology has opened up new

vista of the utility of these coals. Presently the
Son-Mahanadi valley coal basins are gifted with
vast resource of these coals have found their
a number of thick coal seams occurring near to
potential use in thermal power sector and
the surfac e within open c ast mining
gained a sobriquet – Power Coal.
proposition. Though on primary assessment the
These power coals, having enough reserves ,
coals are of very low grade and the present day
have lead to coming up of a number of power
mechanized mining methods lead to further
plants in the adjoining areas of coalfields of
deterioration of their quality, the advancement
lower Son- Mahanadi valley, viz. Talcher, Ib

348
 MPT-2013

river valley , Mand Raigarh and Korba. Since of ash in successive lower size fractions barring,
the coals occur in thick to very thick seams with sometimes, particles below 0.5 mm size which
wide variation in their quality along their show slightly upward trend of ash content than
thickness due to presence of a number of its immediate higher size. This may be owing
different quality dirt bands and partings, the to infiltration of out of the seam particles during
quality of the mine produc e also vary mining. Usually the dirt bands present in the
considerably. This leads to the necessity of their seam are harder than coal bands and therefore
beneficiation prior to use them as boiler feed. the later tend to break more easily leading to
Thus a number of coal washeries have also their progressively higher concentration in
come up in those areas to ensure consistent lower size fractions. The harder dirt materials
are concentrated in higher size fractions. The
supply of stipulated quality coal to the power
bigger pieces of coals also contain unliberated
plants.
dirt bands within them thereby increasing their
Before setting up a washery, it is necessary to
average ash content.
know the beneficiation potential of the coals
Detailed findings of broad screen analysis of a
concerned by generation of data through
number of ROM samples are presented in Table-
laboratory scale washing. These basic data are
1. The related ROM samples were collected from
of utmost importance for planning, designing
Talcher (seam-II), Ib river valley (Lajkura and
and selection of washer in the washing plant.
Rampur Seams) and Korba (Kusmunda group
Many such studies were undertaken at CSIR-
of seams) coalfields, mostly after the primary
CIMFR (erstwhile CFRI) Bilaspur Unit which
crusher at the Coal Handling Plants. Thus their
show some interesting findings related to
nominal top size of particles is +250 or +200
preparation of coal for washing. The present
mm which may technically be termed as ROM
study aims to highlight some such observations
size. After detailed screen analysis they have
and to suggest their potential use in the scheme
been classified in to 3 groups, viz., (+250/200-
of washing of these coals.
13) mm, (13- 0.5) mm and below 0.5mm. It can
2. Case Studies be seen from the table that (+250/200- 13) mm
It is well known that the concentration of fractions always show higher ash, ranging
mineral matter changes with change in the from 1.5 to4.1 percent (average 2.44) than the
particle size. The screen analyses of ROM coals ROM ash. The (13-0.5) mm fractions, on the
prior to washing almost always show decrease other hand, show consistently lower ash by 5.0
Broad size fractions of some ROM coals from thick seams are given below:
Name of Coalfield/ ROM (250/200 – 13)mm (13 -0.5)mm - 0.5 mm
seam Weight Dry ash Weight Dry Ash Weight Dry Ash Weight Dry Ash
% % % % % % % %
Talcher/ Seam-II 100 44.2 78.1 46.2 18.3 37.6 3.6 40.8
Korba/Lr. kusmunda 100 40.9 77.4 45.0 17.7 26.9 4.9 28.5
Korba/ Up. Kusmunda 100 48.6 73.6 51.8 20.5 36.7 5.9 50.1
Korba/Lr. kusmunda 100 36.4 67.5 39.3 26.3 29.0 6.2 36.5
Korba/Up. kusmunda 100 50.2 64.5 53.2 29.3 45.2 6.2 41.1
Ib valley/ Rampur 100 42.0 85.4 43.5 11.9 33.0 2.7 32.6
Korba/ Lr. kusmunda 100 42.3 71.3 45.5 24.4 34.7 4.3 31.5
Talcher/ Seam-II 100 48.7 83.4 50.4 13.4 39.7 3.2 42.8
Korba/ Lr. kusmunda 100 40.8 82.2 42.9 13.7 29.4 4.1 37.2
Ib valley/ Lajkura 100 41.2 79.0 42.7 18.3 32.8 2.7 51.2

349

to as high as 14.0 percent, averaging 8.62, with
respect to that of the ROM samples. The 0.5 mm
fractions, however, show variable result
probably because of contamination from loose
particles from roof or floor materials. The
relation between (13 – 0.5) mm and below 0.5
materials also vary due to the same reason.
The higher size fractions crushed and mixed
with natural size fraction result in increase of
ash content in lower size materials as the
higher ash containing materials are liberated
and allowed to be mixed with erstwhile low
ash containing size fractions. Thus different size
groups of washability head samples are
different from the natural size quality. It can be
postulated that if the higher size fractions are
washed and mixed with unwashed (13-0.5) mm
part, particularly where difference of ash
content between two groups are quite high, can
lead to similar end product with washing of
much less quantity of materials. Two cases are
presented here, one from Kusmunda seam ROM
with 48.6 percent dry ash and the other from
Lajkura seam with 41.2 percent dry ash, where
the clean product obtained from washing of
(100- 0.5) mm (Tables 1 and 2 respectively) are
compared with clean coal yield obtained
following selective washing (flow diagram 1
and 2 respec tively). The (13-0.5) mm
washability data for Kusmunda and Lajkura
ROM samples are given in table nos 3 and 4
respectively.
It can be seen from table-1, that is of Kusmunda
seam ROM, that a clean product with 31.3
percent dry ash can be obtained with 63.3
percent yield on ROM basis. If only the (100-
0.5) mm part of that coal is subjected to washing
and the cleans are mixed with unwashed (13-
0.5) mm slack the resultant yield becomes 67.5
with 34.8 percent dry ash (Flow diagram-1).
Here the yield increases by 4.2 percent with 3.5
percent increase in ash which is tolerable from
the point of view of its use in power sector. This
350
MPT-2013
reduces around 20 percent effort of washing
that can be proved to be much economic.
In the case of Lajkura seam ROM detailed in
table no. 2 it can be seen that 78.9 percent of the
ROM can be obtained as cleans with 36.5
percent dry ash. In the alternative way of
selective washing of (100-0.5) mm part, as
shown in Flow diagram-2, cleans of (100-0.5)
mm added to the unwashed (13-0.5)mm fraction
can produce a combined product of 82.3 percent
of the whole coal with 37.0 percent ash. Here
the ash is marginally higher with 3.4 percent
increase in clean product. Also the washing of
around 18 percent of the whole coal can be
averted.
3. Conclusion
It can be seen from the above study that the
power coals of thick seams of Son-Mahanadi
valley coalfields show characteristic difference
in concentration of mineral matter in different
size range of partic les and that c an be
judiciously utilized in selecting scheme of their
beneficiation. It can also be emphasized that
before setting up of washery for these coals, lab
scale study is of utmost importance for selection
of proper scheme of washing.
Acknowledgement
The authors are grateful to Director, CSIR-
CIMFR for his kind permission to undertake the
study and prepare the paper for presentation
in seminar.
References
Chattopadhyay A. K., Tatwadi. S. T., 1991.
Resource Potential of Power Coals in
Korba Coalfield, Proceedings of National
Workshop on Coal Exploration.
Indian Standards IS-6345, 1971
Raja Rao,C.S., Coalfields of India, vol.III (G.S.I.
Bull. A no.45)
 MPT-2013

Sarkar. G.G, An introduc tion to Coal Table 4: Washability Studies of Lajkura Seam
Preparation Practic e, Oxford & IBH IB Valley Coal Field
Publishing Co. Pvt. Ltd. Size (100-13) mm Wt%-79.0
Unpublished project reports of CFRI/CSIR- Cumulative Cumulative
CIMFR Bilaspur Unit, 2002-2012 Sp.Gr. Wt%
Dry Floats Sinks Ch. Mayer’s
Ash% Wt% pt. value
Whitaker. J. W. and Sarkar. G. G., Studies on Wt%
Ash
%
Wt%
Ash
%
Coal Washability, Parts 1-6 (CFRI >1.30 3.0 17.0 3.0 17.0 97.0 44.1 1.5 0.5
1.40 19.3 27.7 22.3 26.3 77.7 48.1 12.7 5.9
Publication, 1950-51) 1.50 23.3 35.7 45.6 31.1 54.4 53.5 34.0 14.2
1.60 18.5 42.7 64.1 34.4 35.9 59.0 54.9 22.1
Table 1: Washability Studies of Kusmunda 1.70 9.6 51.5 73.7 36.5 26.3 62.1 68.9 26.9
Seam Korba Coal Field 1.80 8.1 54.5 81.8 38.3 18.2 65.5 77.8 31.3

Size (100-0.5) mm Wt%-93.5 <1.80 18.2 65.5 100.0 43.2 90.9 43.2
100 43.2
Cumulative
Dry Cumulative Sinks Ch. Mayer’s
Sp.Gr. Wt% Floats
Ash% Wt% pt. value
Wt% Ash% Wt% Ash%
>1.30 5.0 4.7 5.0 4.7 95.0 49.2 2.5 0.2
1.40 13.1 15.4 18.1 12.5 81.9 54.6 11.6 2.2
1.50 18.1 26.7 36.2 19.6 63.8 62.5 27.1 7.1
1.60 11.3 36.9 47.5 23.7 52.5 68.1 41.8 11.3
1.70 10.1 44.0 57.6 27.3 42.4 73.8 52.6 15.7
1.80 6.2 51.6 63.9 29.6 36.1 77.6 60.7 18.9
1.90 3.9 58.0 67.7 31.3 32.3 80.0 65.8 21.2
<1.90 32.3 80.0 100 47.0 83.9 47.0
100.0 47.0
Clean coal yield: 63.3 percent on ROM basis.
Table 2: Washability Studies of Lajkura Seam
IB Valley Coal Field
Size (100-0.5) mm Wt%-97.3
Cumulative Floats Cumulative Sinks Mayer’s
Sp.Gr. Wt% Dry Ash% Ch. Wt% pt.
value
Wt% Ash% Wt% Ash%
>1.30 4.8 15.0 4.8 15.0 92.2 43.3 2.4 0.7
1.40 20.9 25.3 25.7 23.4 74.3 48.4 15.3 6.0
1.50 21.6 35.4 47.3 28.8 52.7 53.7 36.5 13.6
1.60 17.0 43.1 64.3 32.6 35.7 58.7 55.8 20.1
1.70 9.0 49.6 73.3 34.7 26.7 68.8 68.8 25.4
1.80 7.8 53.8 81.1 36.5 18.9 65.1 77.2 29.6
<1.80 18.9 65.1 100 41.9 90.6 41.9
100 41.9

Clean coal yield: 78.9 percent on ROM basis

Table 3: Washability Studies of Kusmunda
Seam Korba Coal Field
Size (100-13) mm Wt%-70.9
Cumulative Cumulative Mayer’s
Dry Floats Sinks Ch.
Sp.Gr. Wt% pt.
Ash% Wt%
value
Wt% Ash% Wt% Ash%
>1.30 1.6 7.1 1.6 7.1 98.4 51.6 0.8 0.1
1.40 11.3 16.6 12.9 15.4 87.1 56.2 7.3 2.0
1.50 19.2 27.0 32.1 22.4 67.9 64.4 22.5 7.2
1.60 12.0 36.5 44.1 26.2 55.9 70.4 38.1 11.6
1.70 11.4 44.2 55.5 29.9 44.5 77.1 49.8 16.6
1.80 6.8 52.2 62.3 32.3 37.7 81.6 58.9 20.1
1.90 4.0 58.7 66.3 33.9 33.7 84.4 64.3 22.5

33.7 84.4 100.0 50.9 83.2 50.9

<1.90
100.0 50.9

*******
351
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Chemical Beneficiation of Physically Treated Hingula Coal on

Laboratory Scale
Swati Pramanik, B.K. Purohit, PratimaMeshram*, S.K. Sahu and B.D. Pandey
Metal Extr.& Form. Div., CSIR- National Metallurgical Laboratory,Jamshedpur
Jamshedpur – 831 007, India

Abstract
Crude oil and coal are the backbone of energy chain for industrial growth, but limited production
of oil in India makes coal as the only reliable source of energy. Due to non-availability of good
quality coal, supply of high ash (15-55%) coal to power sector has increased over the years. Such
coals cause erosion, difficulty in pulverization, low flame temperature and affect efficiency of
thermal power station. Although coal is mostly beneficiated by physical method, but combining
it with chemical method may improve the quality and efficiency of boilers/plant capacity while
reducing the greenhouse gas emissions.
This study is based on the treatment of Hingula coal (29.6% ash) obtained from Talcher coal field,
Odisha. After physical beneficiation (prox. anal.: 13.3% ash, 49.0% FC, 37.7% VM and 11.8%
moisture) material was chemically treated with different alkali and acids to further reduce the
ash content. Process parameters such as alkali/acid concentration, time, temperature and pulp
density were optimised for de-ashing of coal. Bench scale treatment with Na2CO3 solution for 60
min at 85 oC and 60% pulp density followed by acid wash with dil. HCl, reduced ash content to
9.8%. Similar results were obtained when coal was treated with 10% H2SO4 for 60 min at room
temperature and 10% pulp density. Coal before and after chemical beneficiation was characterised
by XRD and EPMA. Experiments were carried out on kg scale to validate the bench scale data.
When physically beneficiated coal (~1.2 kg) was treated with 0.25N Na2CO3 solution for 60 min at
85 oC and 60% pulp density followed by acid wash with 1% HCl in an agitated reactor, ash content
was reduced to 8.98%. The product is being characterised to ascertaining the properties of the
demineralised coal.

Keywords: Coal, ash, beneficiation, de-ashing, demineralisation

1. Introduction to many other coal based power projects. The

The limited reserves of petroleum and natural
gas have made coal as the prime source of fuel
in the growing industries from metallurgical
* Correspending Author: Pratima Meshram, Metal Extr.&
Fo rm. Div., CSIR- Na tio nal Metallurgical Labora tory,
Jamshedpur Jamshedpur – 831 007, India
Email: pratima@nmlindia.org
Ministry of Coal, India, has reported (2013) the
demand of coal reaching upto 769.69 MT by
2013-14 against the domestic availability of
614.55 MT. In the upcoming years the demand
of coal may increase up to 1267 MT (Sahu et al.,
2011). It has also been found that today coal
holds about 70% of world’s fossil fuel resources.

352

Its demand has increased due to its low cost
and easy availability compared to other fuels
(Franco and Diaz, 2009). The coals obtained
today were generally formed from different
origin and contain many impurities and have
to be cleaned before its use in industries.
Therefore, coal washing has become important
from both economic and environmental point
of view. The raw coal contains organic matter,
moisture, impurities etc. The minerals usually
found in coals are silicates; clay minerals such
as kaolinite, illite, quartz, sandstone, pyrites
and carbonates such as siderites and ankerites,
etc. (Sharma and Gihar, 1991). Therefore, coal
beneficiation term involving de-mineralisation
and de-sulfurization has all such processes
carried on the ROMs to make it suitable for
application in industries without destroying
the physical identity (Sahu et al., 2011). The
effic ienc y of different methods of
demineralization and desulfurization depends
on the structure and composition of the
minerals and on the place and time of their
deposition and formation. Due to the scarcity
of coking coal worldwide and its high cost in
the international market, methods to improve
the low grade coals by reducing the ash and
sulfur contents have been developed. These
methods are classified as physical, chemical and
biological and their application has led to the
production of coal concentrates with low ash,
low sulfur and improved thermoplastic
properties (Mazumder and Sengupta, 1979).
Physical methods depend on the differences in
the physical properties of the minerals and the
carbonaceous part of the coal. The physical
treatment of coal involves separation and the
techniques like crushing and grinding to
decrease the mineral matter through coal
washing. Chemical methods are useful for
removing mineral matters which are finely
distributed and bound strongly to the
coal.Although chemical processes are slightly
expensive than physical methods, but the
353
MPT-2013
former methods are found to be more efficient
with respect to demineralisation efficiency. One
of the c hemic al methods is alkali-ac id
treatement(Adeleke et al., 2013). The common
alkalis used for demineralization include
NaOH, KOH, Na2CO3, NaHCO3 and Ca(OH)2 and
the acids used are HCl,H2SO4, HNO3, HF etc
either alone or in combination of the two. The
multistage de-ashing of coal with sodium
carbonate followed by acid leaching has also
been reported (Afonja, 1976; Adeleke et al., 2011;
Sharma and Gihar1991; Doymaz et al., 2007;
Yang et al., 1985). In the present study the
demineralisation of physically beneficiated
Hingula coal is reported using alkali treatment
with Na2CO3 followed by HCl washing. The
experiments have been carried out with the aim
of converting kaolinite and other such minerals
to its sodium derivatives using dilute to
moderately concentrated solutions of alkali and
removing the remaining minerals by treatment
with ac id leac hing/washing; results are
analysed and discussed in the text.
2. Experimental
2.1. Materials
In the present study Hingula coal- a non-coking
coal from Talcher coal fields, Odisha was used
for the c hemic al demineralization. The
proximate and ultimate analyses of the ROM,
and after physical treatment are presented in
Table-1. It can be seen that the ash in the coal is
reduc ed to a large extent by physic al
beneficiation. Therefore, to have a further
reduction in the ash content chemical treatment
was followed. The chemical analysis of the
physically beneficiated coal is given in Table-2.
The particle size of the sample for chemical
treatment was found to be -50 mm after
physical beneficiation. The experiments were
carried out in a three-necked glass reactor of
250 mL. A condenser was fitted to one of the
opening to overcome the evaporation at high
 MPT-2013

temperatures, a temperature sensor to maintain sample was first leached with 0.25 N sodium
the temperature of the reactants inside the carbonate solutions for 60 min at 85 oCand 60%
reactor and third neck for charging the material. pulp density. After alkali treatment the coal was
The reaction was carried over a hot plate and filtered, washed with 10% HCl and then with
was agitated with a magnetic stirrer. The effects distilled water. The sample was dried in oven
of various proc ess parameters like at 80 oC. This alkali treated coal was further
concentration, time, temperature and pulp
treated with 1% HCl for 60 min at 95oC and 10%
density were studied. The samples after
pulp density. The laboratory scale experiment
treatment was filtered, washed with acid and
was carried out with ~1.2 kg coal in a 3Lreactor
then with distilled water. The filtered coal
with the optimised process parameters. The
samples were dried in a hot air oven at 80 oC.
c oal before and after treatment was
Table 1: Proximate (dry-basis) and Ultimate characterised by XRD and EPMA.
analysis of Hingula Coal
3. Results and Discussion
Proximate Analysis
Coal Type Constituents
3.1. Effect of alkali concentration
Ash Volatile Matter Fixed Carbon Moisture The physically beneficiated sample was treated
ROM coal 29.6% 35.7% 34.7% 4.5% with different concentrations (0.1"5 N) of alkali
Physically beneficiated 13.3% 37.7% 49.0% 11.7%
coal (Na2CO3) at 95 oC for 60 min and pulp density of
Ultimate analysis 10% followed by leaching with 10% HCl in
Constituents Carbon Sulfur Hydrogen Nitrogen
second stage at same temperature and time. It
Physically beneficiated 57.58% 0.76% 5.18% 1.31%
coal was noticed that after Na2CO3 (0.25 - 5.0 N)
treatment, the ash content of Hingula coal was
For the laboratory scale, chemical treatment found to be in the range 13.3- 14.3% (Fig.1). The
was carried out in a thermostatically controlled inc rease in ash c ontent after the alkali
jacketed glass reactor (3L) while flowing the treatment may be due to formation of insoluble
water to maintain the temperature. The sodium alumino-silicates [Fan et al., 1985]. Upon
leaching reactor had arrangements of reflux further treatment of alkali treated coal with 10%
condenser, temperature sensor, and material/ HCl at 95 oC for 60 min, sodium alumino-
reactant charging port. The demineralization silicates present in the coal dissolved and ash
study was c arried out under agitated content of the coal was reduced to ~10.3%. At
conditions to validate the bench scale data. all concentrations of Na2CO3, followed by IInd
Table 2: Chemical analysis of the physically stage leaching with 10% HCl, the ash was
treated coal reduced to ~10.3%. The 0.25 N Na2CO3 was found
Chemical analysis to be the optimum concentration for treatment
Constituents (%) Al2 O3 SiO2 Fe TiO2 K2 O CaO Na 2 O MgO of coal for ash removal.
Physically treated 3.29 5.54 0.4 0.29 0.73 0.15 0.092 0.016
coal 3.2. Effect of contact time
2.2. Methods The physically treated Hingula coal was treated
with 0.25 N Na2CO3 at 95 oC and 10% pulp
A two-step alkali-acid leaching process was density for different time periods in the range
carried out to reduce the ash content after 15-300 min. The slurry was filtered, dried and
physical beneficiation. A known amount of coal
354
 MPT-2013

the alkali treated coal was further treated with was noticed (Fig. 3) that at temperatures
10% HCl at 95 oC for 60 min; results are given in between 25oC -75oC the ash content reduced to
Fig.2. It was observed that with 120 min of ~11% and on increasing the temperature from
alkali treatment followed by acid wash, the ash
85 oC-95 oC the ash was reduc ed to ~9.8%.
content reduced from 13.3% to ~10.3% and
Therefore, 85 oC was taken as the optimum
when coal was treated with alkali for more than
120 min followed by acid treatment, the ash temperature to carry out the demineralization
content decreased to ~9.8%. Fixed carbon also of caol.
increased from ~ 49% to ~54% at this stage.For
15
all time variations the ash removal was nearly
the same, therefore rest of the experiments were
10
carriedout for 60 min with 0.25 N Na2CO3 to %
sh
remove the impurities present in the coal. A
5
A f te r A lk a li T re atm en t A f te r A c id Tre a tme nt

15
0
15 25 35 45 55 65 75 85 95 105
T e m pe r a tur e( o C)
10

%
h
s
A Fig. 3: Effect of temperature on removal of ash
5
A f te r A lka li Treatm ent A f te r A c id Trea tme nt
from physically beneficiated Hingula coal.
Na2CO3: 0.25 N, Pulp density: 10%, Time: 60
0
0 1 2 3 4 5 6
min; in 2nd stage leaching HCl: 10%
N a 2 C O 3 C onc entr at ion (N )
3.4. Effect of pulp density
Fig.1: Effect of Na 2CO 3 concentration on After having optimised the conditions of
physically beneficiated Hingula Coal. Pulp concentration, time, temperature the coal
density: 10%, Temp: 95 oC, Time: 60 min; in 2nd sample was taken for different solid to liquid
stage leaching HCl: 10%
ratio of 5% - 80% and treated with 0.25 N
15 sodium carbonate solution for 60 min at 85 oC
followed by acid treatment. Fig. 4 shows that
%
10
increase in S/L ratio reduced the ash content
sh
A ~11% in the 1st stage leaching and ~9.8% in the
5
A f te r A lk a li T r e a tm e n t A f te r A c id T r e a tm e n t 2nd stage leaching.
0
0 60 120 180 240 300 360
T im e ( m in )

Fig.2: Effect of reaction time on ash reduction

from physically beneficiated coal
Na2CO3:0.25 N, Pulp density: 10%, Temp: 95
o
C; in 2nd stage leaching HCl: 10%
3.3. Effect of temperature
The reaction temperature was also varied in Fig. 4: Effect of pulp density in alkali treatment
the range 25oC - 95oC for treating the coal with with physically beneficiated Hingula
0.25 N sodium carbonate solutions for 60 min, coal.Na2CO 3: 0.25 N, Time: 60 min, Temp:
followed by acid treatment in the 2nd stage. It 95oC; in 2nd stage leaching HCl: 10%

355

3.5. Effect of acid concentration in the 2nd stage
leaching
After having treated the physically beneficiated
Hingula coal with 0.25 N sodium carbonate
solution for 60 min at 85 oC with 60% pulp
density, the HCl concentration in the 2nd stage
treatment was varied from 1- 30 (v/v)% . From
Fig-5, it was observed that inc rease in
concentration had no effect on the ash reduction.
Therefore, 1% HCl was enough for the treatment
of alkali treated coal in the 2nd stage. The GCV
and the sulfur content were found to be
increased after the chemical treatment, as given
in Table 3 .
Fig. 5: Effect of HCl Concentration after alkali
treatment. Na2CO3: 0.25 N, Time: 60 min,
Temp: 95oC, Pulp Density: 10%
Table 3: Ultimate analysis of Hingula Coal
after alkali and acid treatment on bench scale
Ultimate analysis
Constituents Carbon% Sulfur % Hydrogen% Nitrogen% GCV(cal/g)
Physically beneficiated coal 57.58 0.76
Alkali Treated coal 61.79 0.94
After Acid Treatment 63.56 0.99
3.6. Effect of different acid treatment
The physical beneficiated coal was treated with
various mineral acids like HCl, H2SO4, HNO3.
With 10% HCl at 95 oC the ash content was
reduced to 10.7% and the fixed carbon remained
unchanged (49.6%). When nitric acid was used
a lot of fumes were generated at all
temperatures, therefore experiments with
nitric acid were discontinued. Further it has
been reported in the literature that nitric acid
damages the coal structure and reduces the
carbon content. Physically beneficiated coal
MPT-2013
was treated with 10% sulphuric acid at 95 oC
for different time (15 - 240 min). It was observed
that 60 min leaching time was sufficient to
reduce the ash content of the coal from 13.3 to
~9.8% (Fig.6). Under this condition fixed carbon
also increased from ~49% to ~54%.
Fig. 6: Effect of 10% H2SO4 treatment time on
physically beneficiated Hingula coal.
H2SO4: 10%, Pulp density: 10% Temp: 95oC,
Pulp Density: 10%
3.7. XRD phase characterisation and EPMA-
EDS of the coal before and after chemical
treatment
The X-ray diffraction technique is preferably
suited for characterization and identification
of polycrystalline phases. The XRD was done
for characterisation to study the phase changed
in the coal minerals.Fig. 7 shows the XRD
profiles for physically beneficiated Hingula
coal, alkali treated coal and acid treated coal.
Quartz and Kaolinite (Al2Si2O5(OH)4) are the
dominant c rystalline phases and some
5.18 1.31 5355.867
4.67 1.47 5659.816
amounts of Illite [K1-1.5Al4[Si6-7Al1-1.5O20](OH)4],
4.84 1.57 5857.525 iron oxides are also present in the physically
beneficiated Hingula coal. The intensity of
Quartz and Kaolinite were reduced after the
treatment of alkali (0.25 N Na2CO3). These new
peaks correspond to sodium aluminium silicate
(Na8Al4Si4O18). This phase has a tendency to get
dissolved in acidic solutions as can be seen with
reduced peak in the XRD pattern of acid treated
coal.
Energy-dispersive X-ray analysis of the
physically treated Hingula coal, alkali and acid
treated coal was recorded to observe and
compare the leaching behaviour of ash in coal
356
 MPT-2013
001
2.0

in various media. The coal sample is mounted 1.8

CO
1.6

in epoxy resin and the mounted sample was 1.4

Ti

Counts[x1.E+3]
then polished with SiC paper. The polished
1.2

1.0

surface of the sample was then coated with 0.8 Al

Ti Si Cl
0.6 Na S
Fe
S
Fe Mg Ca

palladium. The EPMA images of physically 0.4

0.2
Cl KK FeKesc
Ca Ti Ti Fe Fe

beneficiated, alkali and acid treated Hingula coal 0.0

0.00 1.00 2.00 3.00 4.00 5.00
keV
6.00 7.00 8.00 9.00 10.00
001

are shown in Fig.8. It is clear from Fig.8(a) that 4.0

3.5 C

in the coal sample Al, Si is the main impurities. 3.0

O

Counts[x1.E+3]
2.5

In the chemically beneficiated coal ash content 2.0

Si

Ti

decreased to ~ 9.8% only (~ 26% ash reduction) 1.5

Fe
Fe Mg
Al
S
Cl
1.0 Ti Na S

which is clearly seen in the EPMA images. In Cl Ca FeKesc Fe

KK
Ca Ti Ti Fe
0.5

Fig. 8(b) and 8(c), impurities in the form of 0.0

0.00 1.00 2.00 3.00 4.00 5.00
keV
6.00 7.00 8.00 9.00 10.00

2.0 001
aluminum and silicon were still present. From 1.8
Ti
CO

the EDS analysis, the decrease in ash content of 1.6

1.4

Counts[x1.E+3]
the chemically treated sample is corroborated 1.2

1.0 Al
Ti

by lowering in the concentration of Al, Si, Ca

Si
0.8
Fe Mg Cl
0.6 Na S
Fe S

and Ti. Cl Ca
0.4 K K Ca FeKesc
Ti Ti Fe Fe
0.2

0.0
0.00 1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00
keV

Fig.8: EPMA study of Hingula coal (a)

Physically beneficiated Hingula coal, (b) Alkali
treated coal&(c) Acid treated coal
Laboratory scale demineralization study
A flow sheet is proposed to carry out the
experiment on laboratory scale (3L reactor).
Keeping in view the proposed flow-sheet
Fig.7: XRD pattern of Hingula coal before and further experiments were carried out using the
after chemical treatment optimised conditions to treat the coal on lab
Table 4: EPMA- elemental analysis for the coal scale (~1.2 kg) with alkali leaching followed by
HCl leaching. The physically beneficiated
Chemical Hingula Coal Alkali Acid leached Hingula coal was leached with 0.25 N Na2CO3
formula (Mass%) leached coal coal at 85 oC and 60% pulp density for 60 min. The
(Mass %) (Mass %) coal was filtered, washed with acid and finally
C 76.36 68.35 74.24
with distilled water and dried as reported
O 21.08 24.21 23.65
Na 0.24 ND 0.15 above. Then alkali treated coal was again
Mg ND* 0.05 ND* treated with 1% HCl at 95 oC for 60 min at 10%
Al 0.47 0.63 0.43 pulp density. The ash content of the coal was
Si 0.61 1.86 0.37
reduced to 9.48% with alkali treatment and
S 0.07 0.26 0.14
Cl 0.77 0.61 0.55
finally 8.98% ash after acid treatment. After
K 0.19 0.07 0.13 chemical treatment it was found that the
Ca 0.14 0.14 0.05 carbon and sulfur content of coal increased,
Ti 0.07 ND* 0.04 hydrogen content decreased, nitrogen was not
Fe ND* 3.83 0.26
found, and the gross calorific value also got
*ND: Not detected increased compared to that of the physically

357
 MPT-2013

beneficiated c oal [Table-5]. Petrography
analysis has to be studied for the coals of the
lab scale trial. XRD characterisation was done
for the large scale and the phases obtained were
similar to those of bench scale (Fig. 7).
ROM Coal
[Ash= 29.6%, VM= 35.7%, FC=34.7%]
Physical Beneficiation
Physically treated coal
[Ash= 13.3%, VM=37.7%, FC=49.0%]
Alkali Leaching
0.25N Na2 CO3
[60% PD,85o C,60 min]
Filtration,Washing with 10%
HCl and Distilled water
Leach residue
[Ash= 9.8%,VM= 39.9%, FC= 49.6%]
1% HCl Acid leaching
[10% PD, 95oC, 60 min]
Leach residue
[ Ash= 8.9%, VM= 38.7%, FC= 54.5%]
Fig. 9 :Flowsheet for chemical beneficiation
of Hingula Coal
4. Conclusions
In the present study on the beneficiation of
Hingula coal, it is concluded that chemical
treatment with 0.25N sodium c arbonate
solution at 85 oC for 60 min and 10% pulp
density followed by 1% HCl is more efficient
because of its low cost, less corrosive nature to
and ready available. The hot sodium carbonate
solution easily converts kaolinite into sodium
hydro-alumino-silicates whic h are acid-
soluble. Experiments also show that sodium
carbonate also removes quartz and converts
iron pyrite into hematite to some extent, but
not as readily as sodium hydroxide solutions.
The ash content can be reduced from 13% to
8.9% in the process of chemical treatment.
Acknowledgements
The authors are grateful to the Director, CSIR-
National Metallurgical Laboratory for his
continuous support and encouragement and
the permission to present the paper.
References
Adeleke, A. A., Ibitoye, S. A., Afonja, A. A. and
Chagga, M. M., 2011.Multistage Caustic
Deashing of Nigerian Lafia-Obi
coal.Petroleum & Coal. 54(4), 259-265.
Adeleke, A. A., Ibitoye, S. A., and Afonja, A. A.,
2013.Multistage Caustic Leac hing
Desulphurisation of a High Sulphur
Coal.Department of Materials Science and
Engineering, ObafemiAwolowo
University, Ile-Ife, Petroleum & Coal. 55(2),
112-117.
Afonja, A.A., 1976. Deashing and
Desulphurization of Nigerian c oals.
Research Report No.IFE/CHE/CP/06.
Doymaz, I., Gulen. J., Pisken, S., 2007.The Effect
of Aqueous Caustic and Various Acid
Treatments on the Removal of Mineral
Matter in Asphaltite.Yildiz Technical
University, Department of Chemical

Table 5 Ultimate analysis of Hingula Coal after alkali and acid treatment on bench and laboratory
scale Ultimate analysis
Bench Scale Laboratory Scale
Constituents Physically After After Acid Physically After Alkali After Acid
beneficiate Alkali Treatment beneficiate Treatment Treatment
d coal Treatment d coal
Carbon% 57.58 61.79 63.56 57.58 58.06 60.96
Sulfur % 0.76 0.94 0.99 0.76 0.97 1.12
Hydrogen% 5.18 4.67 4.84 5.18 4.06 3.79
Nitrogen% 1.31 1.47 1.57 1.31 1.11 Nf
GCV(cal/gm) 5355.867 5659.867 5857.816 5355.867 5255.6936 5554.525

358

Engg.Esenler-Istanbul.Turkry. Energy Sources,
Part A. 29, 337-346 .ISSN: 1556-7036.
Fan, C.W., Markuszewski, R., and Wheelock, T.
D., 1984.Chemical Behaviour of mineral
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American.Chemical.Society.Division.of
Fuel Chem. Preprints. 29(4), 319-325.
Franco, A. and Diaz, A.R., 2009. The future
challenges for “Clean Coal Technology”:
joining efficiency increase & pollutant
emission control. Energy. 34(3), 348-354.
Mazumder, B. K. and Sengupta, A. N.,
1979.Proceedings of the International
Symposium on Coal Sc ienc e and
Tec hnology for the Eighties.Vol.42;
Dhanbad, CFRI.
*******
359
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Sahu, H.B., Dash, S. and Swar, A.K., 2011.
Environmental Impac t of Coal
Beneficiation and Its Mitigation Measures,
National Institute of Tec hnology,
Department of Mining Engineering,
Rourkela Indian Journal Environmental
Protection. 31(B), 691-698.
Sharma, D. K. and Gihar, S.,1991.Chemical
cleaning of low grade coals through alkali-
acid leaching employing milder conditions
under ambient pressure.Fuel. 70, 663-665.
Yang, Ralph T., Das,Subho K. and Benjamin,
M.C.Tsai, 1985.Coal deminerilisation
using sodium hydroxide and ac id
solutions.Fuel, 64.
 MPT-2013
Proceedings of the XIII International Seminar on
Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

A Study on Pressure and Sp. Gravity inside Heavy Media

Cyclone to Optimize the Yield & Quality of Washed Coal

Mofid Hussain, S.P. Singh and Bidhan Ch. Dey*

Jindal Steel & Power Limited, Raigarh

Abstract
Heavy Media Cyclone is considered to be the heart of any heavy media cyclone based coal
preparation plant. Quantity as well as quality of washed coal depends upon the performance of
heavy media cyclone.There are different operational factors which directly or indirectly affects
the performance of heavy media cyclone. Among these factors pressure and sp.gravity inside a
heavy media cyclone are the two important parameters. Fluctuation in pressure and sp. gravity
inside a heavy media cyclone directly affects the quantity as well as quality of washed coal.
Coal preparation plant at Dongamahua of M/S Jindal Steel and Power Ltd. is a heavy media
cyclone based coal preparation plant. We have two units for coal preparation purpose. Both the
units are pump feeding heavy media cyclone plant. We have online pressure and specific gravity
motoring system installed in our coal preparation plant. In this paper we have studied the pressure
and sp.gravity inside heavy media cyclone installed at our plant,to optimize the yield and quality
of washed coal.

Keyword: Heavy media cyclone; operating factors; pressure and sp. gravity;yield and quality

1. Introduction contained low grade noncoking coal in seams

Jindal Steel & Power Ltd, a private sector
company is today’s world largest Coal based
Sponge Iron produc er through ‘Direc t
reduction’ process with installed capacity of
1.30 MTPA. In the beginning, Coal requirement
of the plant was met from South Eastern
Coalfields Ltd. Our visionary founder Late Shri
O. P. Jindal Ji, who in the quest of securing raw
material sufficiency for JSPL, acquired the coal
block IV/1 way back in 1996 which categorically
* Correspending Author: Bidhan Ch. Dey, Jr. Manager,
Co al Washery, JOCCM#1, Dong ama hua , Raigarh,
Chhattisgarh-496107 Contact no.: +91-9907197956; Email:
bidhan.dey@jspl.com
thickness varying from 1.5m to 5.5m.
Since then JSPL has traversed consummately
in the development of the coal block IV/1 in
conjunction with coal beneficiation plant; from
2mtpa to 6mtpa to utilize even ungraded coal
economically in the face of scarce coal reserve
of our nation and in true sense serving The Coal
Mines (Conservation & Development) Act.
These ungraded coal co-exist with all the four
major seams namely X, IX,VIII & VII(T&B),
which resulted in 4-6% upward movement in
ash% as analyzed in graded structure of coal
seams. VII(B) seam which majorly contained
ungraded c oal and was out rightly not
considered amenable to mining at the project

360

stage is being mined and benefic iated
ec onomic ally and giving overall c ost
advantage.
In the year 1996 JSPL commissioned its first jig
based coal washery at Raigarh. With jig
washery result were not satisfactory because
of various reasons and was phased out by 2.4
MTPA Heavy Media Cyclone Washery and was
commissioned successfully in August 2002
followed by commissioning of 1.1 MTPA
deshalling plant in January 2003 and then 3.6
MTPA two stage (High, Low) HM Bath & HM
cyclone based washery was commissioned in
April,2005.
The requirement of ash% in wash coal is 32-
33% for DRI production. We should maintain
the ash% according to the requirement. We have
tried to carryout a study that shows the trend
of variation between ash% of wash coal with
feed pressure and sp. Gravity to optimize yield
of wash coal.
2. Process
Washery II is a two-stage coal washing plant
with a capacity of 2.5 MTPA. The crushed coal
of lower ash seam is directly washed in the
dense medium Cyclones after desliming at
0.5mm. The deslimed coal + 0.5 - 25mm size coal
goes to the Heavy media tank for feeding to HM
Cyclones.
Crush coal(VII T & B seam) is first deslimed at
0.5mm# in Desliming screens and then fed to
the Heavy Medium Bath for separating Rejects
(of ash% >77%). The deshaled coal goes to the
Heavy media tank along with deslimed raw
coal of VIII, X & IX seam. Here after mixing with
heavy media of appropriate specific gravity fed
to HM Cyclones.
Washery III is a 3.5MTPA washery. It has three
independent circuits, Circuit I & II are two
stage-washing (HM bath & HM Cyclone)
circuits and circuit III is a single stage HM
Cyclone circuit. Feed from the main feed
conveyor is divided into three different circuits.
361
MPT-2013
The only difference between Washery-II & III is
that in Washery-III all coal is first deshaled and
then fed in the Heavy Media tank for onward
separation in Cyclones and in Washery-II 50%
coal is directly fed in Heavy Media tank and
50% coal is fed in Heavy Media tank after
deshaling. All other process is identicalto
Washery-II.
The desired quality parameters are clean coal
ash of 32-33% & middling ash 60-61%. The wash
coal is dewatered in a Centrifuge machine and
followed by Thermal Coal Drier so as to deliver
wash coal with 14 -16 % moisture. The wash
coal is finally screened to remove –3mm fraction
coal so that dispatched product contains about
14% of –3mm fraction.
The final products for the washeries, wash coal,
middling & Rejects are conveyed by belt
conveyors to overhead Bunkers for truck
loading. The wash Coal is dispatched to Raigarh
for the DRI operations. The middling coal is by
Powerplant.
Fine Coal Treatment: The deslimed material, -
0.5mm size coal goes to the fine coal tank from
where it is pumped to a battery of Classifying
Cyclones. The underflow of the classifying
cyclones (+150 ì) is dewatered in a high
frequenc y screen & mixed with process
middling. The –150 ì material is fed to
theThickener. The Thickened slurry from the
underflow of the thickener pumped to a mines
pond where a flocculent dosing system has been
incorporated for quick release of trapped water
from the slurry. This water is filtered through
a thick wall of rejects and we get sufficiently
clear water which is fed back to washery. This
has allowed us to maintain a close circuit.
2.1. Basic principle of dense media separation
Sinc e dense media cyclone works on the
principle of dense media separation, we have
to first understand the principle of dense media
separation.
In a medium, the velocity at which a spherical
coal particle sinks is given by the following
equation:
u  gdv  gDv  R (1)

where, d=density of the coal,v=volume of the
coal particle,D=density of the medium & R=
resistance that a coal particle encounters in
attempting to move downwards in a medium.
The forces governing the settling velocity in a
cyclone is given by the equation:
u 2vd U 2 vd
u  R (2)
r r
‘U’ is velocity of coal or grain
Eqn (1) is showing that stability can be
increased by having:
a) low v i.e for small particles
b) low d i.e. low relative density medium solids
c) high R i.e. high liquid resistance to particle
motion
The magnitude of ‘g’ in the Eqn (1) cannot be
altered or removed, but it can be reduced to a
negligible amount by replacing it with a much
larger force i.e. centrifugal force. The coal grain
when subjected to the effects of this new force
will move in the direction which the force is
applied. This concept is utilized in the dense-
medium cyclonic separators. Because the force
potential of this separator is great, it is possible
to treat relatively large quantities of raw coal
in a unit of small physical sized unit.
Eqn (2) shows that as the coal grain spirals
towards the centre of the cyclone, both the
settling velocity & forces causing it, become
greater i.e. the value of r is becoming smaller
and v is getting larger.
2.2. Medium used in our coal washery
Finely grounded magnetite powder with
magnetic content >88% used in our washery:
2.3. Type of feeding system in dense medium
cyclone at our washery
The coal washery of M/S JSPL is a pump-fed
dense medium cyclone washery.
Pump fed systems: Pump fed cyclones are
simpler in terms of plant layout and involve a
lower plant profile because the desliming screen
need not be installed above the level of the
cyclone. Although they are generally cheaper
362
MPT-2013
in capital cost , they may prove more expensive
to operate due to greater wear and tear on
pumps and pipeline and added power costs.
Also, any fluctuation in pump performance
may lead to lower operating pressure and
subsequent loss in efficiency.
Provided that feed conditions are maintained
as per the original design the c yc lone
performance will be the same in each case for a
given cyclone diameter.
3. Our areas of Interest
Effect of sp. gravity & pressure
We know as the sp. gravity inside the dense
medium c yc lone increases, c ut density
increases and ash% of the washed coal also
increases.
Increasing the pressure, to a certain limit,
increases efficiency .As the pressure energy is
converted into centrifugal force within the
cyclone, an increase in the centrifugal force
causes an increase in the radial displacement
of coal towards the cyclone wall. There is a
limiting condition where further increases in
pressure do not result loss in corresponding
increases in centrifugal force due to frictional
losses. Consequently, efficiency not improved.
Operating at higher than necessary pressure
also increases wear and, therefore, maintenance
costs. However, reducing pressure leads to an
almost exponential increase in cut density.
4. Results and Discussion
Data collected for sp. gravity, pressure of HMC
& ash% of wash coal represents the data for
two months. The data collected from online
pressure transmitter, online density gauge &
online ash analyzer systems which are installed
in our washery-III is given in Table 1.
The following data of pressure v/s ash% of wash
coal is showing that as the pressure increases,
ash% decreases. Feed rate is kept almost
constant during the period when data were
collected. The data is shown below:
 MPT-2013

Table 1: Collected data from Washery-2 Sp. gravity in the c yc lone is maintained
according to quality of the feed coal. Generally
HMC Pr. Ash% HMC Pr. Ash%
1.18 32.16 0.94 33.34 the Sp. Gravity is maintained around 1.51.The
1.19 32.22 0.95 33.47 relationship between sp. gravity and ash% of
1.22 31.93 1.05 33.08 wash coal is linear. The Sp. Gravity data for
1.19 32.2 1.10 32.54 HM cyclone & ash% of the wash coal is recorded
1.25 31.93 0.93 33.72
as shown in Table 2.
1.23 31.96 1.00 33.08
1.24 31.93 1.08 32.84 4.1. Graphical trend of the above recorded data
1.12 32.48 1.03 33.04
1.18 32.17 1.04 33.1 The relationship between ash% and pressure
1.22 31.85 1.10 32.54 is graphically presented in Fig. 1.
1.2 32.06 1.07 32.72
1.13 32.43 0.93 33.38
1.25 31.85 1.01 32.76
1.18 32.35 1.04 32.45
1.23 32 1.04 32.89
1.21 31.76 1.04 31.89
1.26 31.66
1.12 32.74
1.12 32.65
1.08 32.76
1.06 32.75
Fig. 1: Variation of ash% with pressure
1.01 32.92 The relationship between Sp. Gravity and ash%
Table 2: Sp. Gravity data for HM cyclone & of the above recorded data is graphically shown
ash% of the wash coal in Fig. 2.
Sp. gravity Ash%
1.61 33.47
1.61 33.34
1.60 33.72
1.61 33.55
1.54 32.76
1.54 32.84
1.58 33.29
1.56 33.21
1.55 33.08
1.54 32.68
1.55 32.91
1.55 32.87
1.55 32.74
1.57 33.19
1.53 32.71
1.52 32.54
1.51 32.54
1.54 32.86
1.54 32.83
1.53 32.83
1.51
1.52
32.52
32.68
Fig. 2: Variation of ash% with Sp. Gravity
1.52 32.45 The above relations show a downward trend
1.54 32.89
1.54 32.65 between ash% and HMC pressure and a linear
1.47 31.44
1.49 32.02 trend with a positive slope between ash% and
1.47 31.45
1.45 30.67
Sp. Gravity.
1.50 32.17
1.50 32.36 5. Conclusion
1.50 31.63
1.49 31.95
1.51 32.08 From the above study it is seen that to maintain
1.46 30.93
the desired ash% of the wash coal, the HMC

363

feed pressure should be kept in between 1.1 to
1.2 Kg/cm2 and the operating sp. Gravity
should be kept in between 1.50 to 1.53. The yield
of wash coal will be maintained & optimized
accordingly.
Acknowledgement
I want to acknowledge M/S Jindal Steel and
Power Limited for their continuous support
and help required to carry out this work.
*******
364
MPT-2013
References
Osborne, D. G., 1988. Coal preparation
Technology, Vol-1., first ed, Graham &
Trotman Limited, USA.
Sanders, G. J., 2007. The principles of coal
preparation, fourth ed, Australian coal
preparation society, Newcastle.
Imteyaz, S. M., 2013. Improvement of yield in
dense media bath by changing top size of
feed coal from 75mm to 25mm. Recent
trends and future needs in c oal
preparation, CPT 2013, CSIR-CIMFR. 31.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

A Study of Coal Washing Spirals Treating Indian Coals

K.M.K. Sinha, G.S. Jha, K.M.P. Singh, Nilesh Kumar, Pradeep Sahu and T. Gouri
Charan
Central Institute of Mining & Fuel Research (Digwadih Campus), Dhanbad

Abstract
A study of coal washing spiral operation treating Indian coals and its performance is under way
at CSIR-CIMFR. The purpose of the coal spirals is to take the samples on-line for the size -3 to 0.5
mm from 40 TPH coal washing pilot plant. The objective is to use the pilot plant data to develop a
fundamental understanding of the spiral separation process and to formulate of spiral performance
which can be subsequently validated and extended by the incorporation of field data.
A fundamental analysis was subsequently undertaken of the forces and mechanism occurring
during the spiral separation process and results from the current series of pilot plant tests
demonstrated the validity of this approach. Both the pulp behaviour (pulp profile and flow rate)
and coal particle position on spiral profile can be accurately predicted using this technique for the
spiral profile tested. For the spirals there was a strong correlation between solid feed rate and
clean coal ash content and yield at constant middlings setting.

1. Introduction Mikhail et al., 1988; Benusa et al. 2009). A high

A spiral concentrator or spiral consists of a
multiturn helical trough with a curved cross-
section. As the slurry flows down the trough,
the trajectory of the low-density particles (Coal)
is towards the outer periphery of the spiral,
and the trajectory of the high-density particles
(Shale/Stone) is towards the inner periphery of
the spiral. The slurry is split into two or three
product streams at the spiral discharge.
Spirals can operate over a wide range of flow
rates and solids c onc entrations and still
achieve acceptable separations. The volumetric
slurry flow rate typically ranges from 1.5 to 3.6
liters per second (L/s).A higher flow rate is
desired for larger heavier material, whereas
when cleaning fine coal particles, a low flow
rate is desired (Weale and Swanson, 1991;
flow rate would force the fine particles to the
outer rim with little or no separation.
However, a flow rate that is too low can result
in sluggish particles that will not flow and
ultimately not reach their intended stream. This
will result in a large amount of low-density
material in the high-density stream. In such
cases, the frictional forces will be more dominant
than the centrifugal forces, which will not be
able to move the particles to the outer rim. A
high flow rate can cause high-density, large
particles to move to the outer periphery of the
trough, resulting in misplaced high-density
material in the low-density stream. The feed
solids concentration of coal spirals are typically
in the range of 10%–35% by weight (Mikhail et

365
 MPT-2013

al., 1988; Benusa et al. 2009). Increasing the solids desired feed rate. The splitter position was
concentration will increase the tons per hour mea­sured from the outer rim to the tip of the
of material being proc essed but might splitter.
ultimately decrease the performance of the
spiral. In general, a high feed ash requires a
lower solids concentration (Benusa et al. 2009;
Honaker et al. 2007).
The feed rate of dry solids through a spiral
generally ranges from 1.8 to 2.7 tons per hour
(t/h). The dry feed rate is proportional to the
solids concentration, so the higher solids
concentration results in more tons per hour of
dry solids being processed.
Splitter position also gives significant impact Fig. 1 : Spiral set up
on beneficiation. In maximum opening, lower
density material is migrated towards higher Experimental Program
density material. In minimum opening, higher A statistically designed test program using
density material is migrated towards lower simple factorial design of experiments has been
density material. The fifty percent opening used where three levels of all variables are taken.
gives balanced distribution .But; finally it The formula used is
depends on liberation characteristics and N = 2k +3*
presence of free shale/stone.
Where N = number of trials
2. Experimental k = number of variables
3 * = Three number of replicate
Material
experiments carried out under base level
The fine coal was collected from the online
This is known as a factorial experiments and
underflow stream of a wet vibrating screen
(3mm) passing over a desliming screen all possible combination of the factor levels have
(0.5mm) in an operating 40 tph coal washing been executed during the experimentation.
pilot plant at CSIR-Central institute of Mining Actual and code variables are shown in
and Fuel research (CFRI Campus) Dhanbad Table1.Test results has been shown in Table
treat­ing coal extracted from Kathra Open Cast 2.The design matrix and results obtained are
Mines under Central Coalfield Limited. The shown in Table 3.
treated feed coal size was -3.0 + 0.5 mm.The Table 1: Code for spiral experiments
overall feed ash was 30.6 %. Pulp
Code Splitter position Code Flow rate Code
Density
Methods
( 7,14,21"), 21"≈0%,
(litter/
All experiments were conducted using a single- (%) X1 14"≈50%, 7 " = 100% X2 X3
minute)
start LD7 spiral (MDL, Australia). The spiral from outer rim

was operated in closed-circuit arrangement Upper Level 20 +1 100% +1 220 +1

Lower Level 10 -1 0% -1 200 -1
shown in Figure 1whereby the product and
Base Level 15 0 50% 0 210.0 0
reject streams were recycled back to the feed
tank. A valve located on the feed line controlled
3. Results and Discussion
the amount of slurry returned to the feed tank,
which, in turn, allowed the adjust­ment to the
366
 MPT-2013

Experimental Results Table 4: Experimental and Calculated RNA

The experimental programme provides a broad results
range of product ash values as shown in Table Actual Calculated
RNA RNA
2.The spiral concentrator provided a reduction
93.8 93.6
in ash content from 30.6 % to a minimum of 88.7 89.3
20.7 at the yield of 73.7 %. Yield varies from 85.7 86.7
82.5 83.4
73.1 to 89.5 % for different ash that varies 89.9 88.7
between 20.7 to 27.3 % as shown in Table 2. 84.2 83.4
Although it is less than theoretical value 93.2 93.6
90.2 89.3
determined from float and sink tests. However, 90.5 88.5
the simplicity and low cost characteristics of 89.0 88.5
89.4 88.5
the spiral compared to other alternatives may
override the inferior performance. Recovery of Model evaluation
Non-Ash material (RNA) was used by applying Table 3 is the design matrix and results obtained
the following formula to judge the efficiency of for recovery of non ash material (RNA). Table 4
process variables. is comparative experimental and calculated
RNA varies from 82.5 to 93.8 for the ash level
results obtained from model equation. It
that varies between 20.7 % to 27.3 %
indicates that the experiment and calculated
respectively. RNA values close to each other, the model
Table 2: Test results of clean coal and reject developed is valid over range of variation
ash%, yield% and RNA studied. Major statistics indicate that the
Cleans Reject models can be used for effectively describing
Expt .No. Ash % Ash % Yield % RNA the operating parameters effec ts on the
1 27.3 58.8 89.5 93.8
2 24.7 57.0 81.7 88.7 responsive variables. The models do not have a
3 22.9 56.6 77.2 85.7 significant lack of fit ( F-values less than
4 21.7 54.8 73.1 82.5 F0.05).The product RNA model has a lower
5 25.7 56.3 84.0 89.9
6 20.7 58.3 73.7 84.2
degree of freedom for model term ( 2 in stead of
7 26.6 60.4 88.2 93.2 7) due to the elimination of several insignificant
8 24.0 61.4 82.4 90.2 terms using ‘t’ test .Final regression equation
9 23.5 63.1 82.1 90.5
developed after eliminating the insignificant
10 23.5 60.3 80.7 89.0
11 23.3 61.5 80.9 89.4 coefficients through statistical test is as follows.

Table 3: Design Matrix of Experiments and results of Recovery of Non- Ash Material (RNA)
Expt.No X1 X2 X3 RNA X1*RNA X2*RNA X3*RNA X1*X2*RNA X1*X3*RNA X2*X3*RNA X1*X2*X3*RNA
1 +1 +1 +1 93.8 93.8 93.8 93.8 93.8 93.8 93.8 93.8
2 +1 +1 -1 88.7 88.7 88.7 -88.7 88.7 -88.7 -88.7 -88.7
3 +1 -1 +1 85.7 85.7 -85.7 85.7 -85.7 85.7 -85.7 -85.7
4 +1 -1 -1 82.5 82.5 -82.5 -82.5 -82.5 -82.5 82.5 82.5
5 -1 +1 +1 89.9 -89.9 89.9 89.9 -89.9 -89.9 89.9 -89.9
6 -1 +1 -1 84.2 -84.2 84.2 -84.2 -84.2 84.2 -84.2 84.2
7 -1 -1 +1 93.2 -93.2 -93.2 93.2 93.2 -93.2 -93.2 93.2
8 -1 -1 -1 90.2 -90.2 -90.2 -90.2 90.2 90.2 90.2 -90.2
9 0 0 0 90.5 0 0 0 0.0 0.0 0.0 0
10 0 0 0 89.0 0 0 0 0.0 0.0 0.0 0
11 0 0 0 89.4 0 0 0 0.0 0.0 0.0 0

367

RNA = 88.5+2.1X3+2.9X1*X2
From the final equation, it shows that
interactional effect of pulp density and splitter
position is more significant and positive than
flow rate.
4. Conclusion
In pilot plant studies, the spiral concentrator
was found to be an effective technology for
cleaning coal. The empirical models developed
from experimental data indicates that all three
parameters evaluated i.e. feed volumetric flow
rate ,feed solid concentration and splitter
position are significant in regards to achieve to
achieve the maximum yield possible to the
product stream over a range of product ash
content.
*******
368
MPT-2013
References
Benusa, Matthewc D., and Klima, Mark S., 2009
An Evaluation of a Two-stage spiral
proc essing anthrac ite refuse,
International Journal of Coal
Preparation and Utilization, 29: 49–67.
Honaker, R.Q., Jain, M., Parekh, B.K., Saracoglu,
M., 2007. Ultrafine coal cleaning using
spiral Conc entrators, Minerals
Engineering 20, 1315-1319.
Mikhail, M. W., Salama, A. I. A., Parsons, I. S.,
and Humeniuk, O. E. 1988.Evaluation
and Application of Spirals and Water-
Only Cyclones in Cleaning Fine Coal,
Coal Preparation, 6, 53–78.
Weale, W. G., Swanson, A. R., 1991. Some
Aspects of Spiral Plant Design and
Operation, Fifth Australian Coal
Preparation Conference, Newcastle,
Australia, May 13–16, 98–110.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Studies on Characterization and Assessment of Washing Potential

of a Low Volatile Coking Coal

DivyaJyoti, S. Bhattacharya, V.K. Saxena, Kunal Mathanker and Avinash Kumar

Indian School of Mines, Dhanbad, India, chem.divya@gmail.com,
bhattac.1957@yahoo.com, vksaxenaism@hotmail.com,
kunalmathnkar.1010@gmail.com
Abstract
Medium coking coal accounts for as much as 82% of the total coking coal reserves of India, atleast
27% of the medium coking coal reserves are of low volatile type. A representative of coal sample
was collected from combined seam of VI-IX of Ghodar collieries of Kusunda mines. Sampling is
done by Coning & Quartering. Proximate analysis of coal shows 32 % ash, 21.54 % VM, 2.20 %
moisture, 44.26 % Fixed carbon, 1.2 % sulfur and FSI is 2.5. About 50.55 % of ROM coal is above
25.4mm size. For Sink & Float test size fraction from -25.4mm to -3.175mm has been divided into
four size intervals. Washability analysis shows increase in clean coal yield from 40% for -25mm
fraction to 57.5 % for 3.175mm fraction with relative increase in cut density from 1.46 to 1.57
respectively at 17% ash. Washability Index also increases from 27.29 for -25mm fraction to 35.4
for 3.175mm particles respectively. Swelling properties improves as FSI increases upto 4.5 for
clean coal from 2.5 of feed coal. Also caking index improved upto 20 for clean coal from 11 for ROM
coal. Crushing to 6.35mm is found economical from washability test with 46.7 % clean coal yield
(17% ash) at 1.53 cut density.

Keywords: Washability; LVMC coal; clean coal yield; cut density

1. Introduction coal is estimated at 90.2Mt by 2016-17. This

Coal consumption in India is projected to
increase by 40% in next five years from the
production level of 539.94Mt in 2011-12.
Estimated resources including thermal and
coking coal is 286 Bt. About 35Bt of total reserve
is coking coal. Total coking coal production in
2011-12 was only 51.654Mt. 25Mt was
imported during the same period. In the current
plan periods, the projected production by 2016-
17 will be about 31Mt. Consumption of coking
* Correspending Author: DivyaJyoti, JRF, Indian School of
Mines, Dhanbad, India, E-mail: chem.divya@gmail.com
situation has led to augmentation of domestic
coal production by beneficiating Low volatile
medium coking coal(LVMC). This coal is not
linked to washeries and thus categorized as
non-linked washery c oal(NLW). Medium
coking coal account for as much as 82% of the
total coking coal of the country, 27% of the
medium coking coal is low volatile type. LVMC
coal is characterized by high raw coal ash
content to the extent of 46-47% and good coking
properties in general but vitrinite is below 20-
45% and inertinite as high as 70% with low
content of exinite. Due to greater involvement

369

of vitrinite and higher amount of finely
disseminated inter grown mineral matter, the
NGM at 1.45-1.65 cut density range are high
thus making the LVMC coals difficult to wash.
For long term security of supply greater use of
these c oals in steel plants, along with
indigenous prime and high volatile coking coals
can save huge foreign exchange provided
proper emphasis is given by setting up of
washeries to beneficiate these coals for use in
the steel plants after designing suitable flow
sheets. Coal India has planned to wash 19Mt of
LVMC coal in near future and is in the process
of installing 6 coal washeries for its LVMC coal
beneficiation on private-public cooperation
concept.
2. Experimental
2.1. Material
After surveying and observation of source of
low volatile medium coking coal, Godhar
collieries of BCCL (Kusunda area) has been taken
for present study. 400 kg coal sample collected
from combined seam (V-lX). ROM coal was
collected and staged crushed in a Jaw crusher
followed by Double roll crusher set at 50mm.
Bulk sampling, coning and quartering is done
to get representative samples for further tests.
2.2. Methods
Size analysis of sample was done by vibratory
screen in the size range of +50 to -3.15 mm and
ash analysis of each fraction by standard
method was done. For proximate and ultimate
analysis sample was further ground to -72
mesh. Sink- Float tests were performed for each
size fraction of size analysis in descending order
of specific gravities. Aqueous Zinc Chloride salt
was used as medium of varying density of 1.3
to 1.7. Proximate analysis, ultimate analysis,
free swelling index (FSI) and caking index (CI)
was determined for each fraction of Sink-Float
test. For ultimate analysis Vario EL
370
MPT-2013
ELEMENTAR ANALYSER was used. Fig. 7
shows the flowsheet of experimental work
carried out.
2.2.1. Sink-Float test
For the purpose of sink-float analysis, the feed
coal was divided into following five size
frac tions viz: (-25.4+19.05mm), (-
19.05+12.7mm), (-12.7+6.35mm), (-
6.35+3.175mm) and (-3.175mm). The sink float
test of the size fractions were carried out to
know the exact washability nature of the feed
coal. Fines of size fraction below 3.175mm are
discarded. Different baths of varying specific
gravities are prepared by dissolving ZnCl2 salt
in warm water. An air-dried sample of coal was
placed in small quantity at time in the highest
specific gravity bath and stirred well. The
material was allowed to settle. The float
obtained was transferred to next bath of lower
specific gravity. Sink was again stirred to
liberate any trapped light particles. This process
is repeated until lowest specific gravity. All sink
and floats were washed properly with warm
water for removal of ZnCl2. All fractions were
then dried and weighed. From the sink float test
data the washability curves of the different size
frac tions were drawn. The washability
characteristics of the different size fractions
were analyzed from the washability curves and
washability study was done to know the size
fraction to which the ROM coal is to be crushed.
3. Result and Discussion
3.1. Characterization
Proximate analysis of ROM shows it is a
medium coking coal and results are given in
table 1.
Table 1: Proximate analysis of ROM
Variables Values
Ash % 32.07
Volatile matter % 21.45
Moisture % 1.6
FSI 2.5
 MPT-2013

By size analysis it was observed that ROM

contains 50.55 % particles are above 25.4mm
with cumulative ash of 33.30 % (as received).
ROM was ground below 25.4mm for further
processing, and after crushing percentage of
fines increases by 14.45 by weight with approx
same ash composition of 20.32% (as received).
Rosin Rammler particle size distribution for
ROM and crushed coal is given in Fig.1. From
RRB plot it is found that partic le size
distribution is more uniform for crushed coal
than ROM coal. The value of distribution
constant (n) increased to 0.902 from 0.855 after
crushing. And the mean diameter for ROM and Fig. 3: Washability curve of (-25.4 +19.05mm)
c rushed c oal is 36.6mm and 11.6mm
3.2.2. Washability curves for (-19.05 +12.7mm)
respectively.
Washability curve drawn from sink-float test
data, shows that 34 %yield of clean coal at
standard ash of 17 % is achieved at cut
density of 1.46. Near gravity material (NGM)
32.5 and washability index 27.29, are found
for cut density 1.46.

Fig. 1: Rosin Rammler plot of size distribution

for ROM and crushed coal to size 25.4mm.
3.2. Sink-Float test
By sink-float tests data of all size fractions,
washability curves of each curves is drawn.
Fig. 4. Washability curve of (-19.05 +12.7) mm.
3.2.1. Washability curves for (-25.4 +19.05mm)
3.2.3. Washability curves for (-12.7+6.35mm)
Washability curve drawn from sink-float test
data, shows that 40.1 %yield of clean coal at Washability curve drawn from sink-float test
standard ash of 17 % is achieved at cut density data, shows that 41 %yield of clean coal at
of 1.46. Near gravity material (NGM) 32.5 and standard ash of 17 % is achieved at cut density
washability index 27.29, are found for cut of 1.49. Near gravity material (NGM) 41.1 and
density 1.46. washability index 27.67, are found for cut
density 1.49.

371
 MPT-2013

respectively. But little improvement in FSI and

CI is achieved for size fraction of (-19.05
+12.7mm) as FSI increase only 0.5 to reach 3
and CI remains same. This is because of less
amount of volatile matter present in the fraction
(-19.05 + 12.7mm) as compared to other size
fraction. Improvement in physical properties
of product of each size fraction is shown in
Table3.
Table 3: Effect of washing on clean coal and
reject for different size fractions.
Washability
Fig. 5: Washability curves of (-12.7 +6.35mm). Size,mm Y CC ACC NGMcc FSIcc CIcc
Index
YReject AReject

(-25.4+19.05) 40 1.49 32.5 4 20 27.29 23 1.76

3.2.4. Washability curves for (-6.35 +3.175mm) (-19.05+12.7) 38 1.49 32.5 3.5 19 27.29 54 1.55

(-12.7+6.35) 43 1.49 41.1 3 18 29.67 39 1.62

Washability curve drawn from sink-float test
(-6.35+3.175) 60 1.6 27.5 4.5 18 35.4 33 1.65
data, shows that 57.5 %yield of clean coal at
standard ash of 17 % is achieved at cut density Crushed to (-25.4mm) (+50mm)
ROM
of 1.57. Near gravity material (NGM) 27.5 and (-50+38.1mm)
Size analysis
washability index 35.4, are found for cut density Proximate analysis Size analysis
(-38.1+25.4mm)

(-25.4+19.05mm)
1.57. (-25.4+19.05mm) (-19.05+12.7mm) (-12.7+6.35mm) (-6.35+3.175mm) (-3.175mm) (-19.05+12.7mm)

(-12.7+6.35mm)
Sink -float test Sink -float test Sin k -float test Sink -float tes t S ink -float test
(-6.35+3.175mm)
Proximate analysis Pro xim ate analysis Prox imat e analysis Proximate analysis
(-3.175mm)

Pro xim ate analysi s

Fig. 7: Flowsheet of experimental work carried

Fig. 6: Washability curves of (-6.35+3.175mm).
3.3. Effect of washing on physical properties
of coal
For Size fraction (-25.4+19.05mm) improvement
in caking and swelling properties is found as
FSI increases upto 4 from 2.5 and CI upto 20
from 18 for ROM. FSI increases upto 3.5 and 4.5
and CI increases upto 19 and 20 for size fractions
(-12.7 +6.35mm) and (-6.35 + 3.175mm)
out.
4. Conclusions
Generally, washability of low volatile medium
coking coal can be improved by crushing it to
lower size bec ause difficult washability
characteristics of LVMC coal is due to fine
dissemination of mineral partic les with
macerals and ash% of marketable product can
further be improved making coal blendable
with prime coking coal, so that this coal can be
used in various steel plants.
On the basis of results obtained by conducting
different experiments and considering different
aspects of beneficiation, a complete cost-benefit
analysis is necessary prior to taking decision of

372
 MPT-2013

washing these coals. Since, crushing at lower References

size involves increased cost of size reduction,
CFRI Report, Coking potential of low volatile
cost beneficiation as well as handling cost of
medium coking coals of Jharia Coalfield.
size reduction, cost beneficiation as well as
India Coal Ministry, 2011-2012, Karvy stock
handling cost of material although there is
broking.
increase in yield of beneficiated coal.
India Energy Book, 2012, World Energy Council,
From the washability analysis, crushing of coal
1-12.
to less than 12.7mm is economical
Kumar, Rajiv, 2012, Coal is the next big problem,
From the washability data it is observed that
FICCI blog.
for coal crushed to d” 12.7mm at 17%±0.5 ash
Leonard J W; Mitc hell D R, 1997, Coal
the yield is 46.7 % at RD 1.53.
preparation, selly W. Mudd Series.
Utilization of LVMC c oals after suitable
Osborne, D.G vol.1
beneficiation can reduce the import of coking
coal, thereby saving considerable amount of
foreign exchange.

*******

373
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar
New Coal Preparation Plant Circuitry for Indian Metallurgical
Coal

S. Saurabh1, Z. Wang1, A. Mahapatra1 and S. Pal2

1
FLSmidth Salt Lake City, Inc., 7158 S. FLSmidth Drive, Midvale, UT 84047,· USA
2
FLSmidth India Pvt. Ltd., 34 Egatoor, Kelambakkam, Chennai, Tamil Nadu 603103,
India
Abstract
Coal preparation plant circuit selection and optimization for metallurgical coal has always been
a challenge in India. The commonly followed practice is to deslime the raw coal plant feed at
0.5mm and to send the oversize (+0.5 mm) to the heavy media (HM) cyclone circuit while the
undersize (-0.5mm) is directly fed to flotation. The HM cyclone circuits normally consist of a
primary stage, which provides 16-18% ash (dry-basis) metallurgical coal product and a secondary
stage, which provides 33-34% ash (dry-basis) middling as power station coal. Typically, the -
0.5mm final flotation product reports to the primary metallurgical coal product after dewatering.
This paper will highlight the results of a study performed by FLSmidth using Indian metallurgical
coal data. In this study, the plant circuits used in Indian metallurgical coal preparation plants is
compared to those used for the similar purpose internationally (particularly in North America).
The paper will show the results of desliming the raw coal at 1mm with the plus 1mm feeding the
HM cyclone circuit, the 1mm x 0.25mm reporting to a water-only gravity based circuit and the -
0.25mm going to flotation. The idea behind introducing these kind of circuits is to reduce the
amount of fines (-1mm) going to the HM cyclone, to improve the separation inefficiency of HM
circuit (Ep), to reduce magnetite loss and to reduce the product moisture. Furthermore, this
should also reduce required screen sizes and the magnetite recovery units, resulting in plant
capital cost reduction. Treating -0.5mm coal with froth flotation has been a concept followed
internationally since the 1970s. During the last two decades, it was proven that floating -0.25mm
(or even -0.15mm) was a better option with 1mm x 0.25mm or 0.15mm being cleaned in a water-
only gravity based circuit like water-only cyclones, spirals, teeter bed separators or reflux
classifiers™. Additionally, the smaller size distribution range (-0.25mm) going to flotation will
reduce the reagent consumption, lower the operating cost and improve the flotation performance.
The optimization of coal circuits was investigated using the equal incremental ash approach. This
new coal plant circuitry has been widely accepted and implemented internationally with proven
desirable results. This has the potential to reduce capital and operating cost of a coal preparation
plant. The results of this study will be the subject matter of discussion in this paper.

Keywords: Heavy media cyclone; reflux classifier; optimization; incremental ash.

* Correspending Author: Swadhin Saurabh, Sr. Process
Engineer, FLSmidth Salt Lak e City, Inc., Email:
swadhin.saurabh@flsmidth.com , Phone: +1-8015548286
1. Introduction
Designing and building a metallurgical coal
preparation plant in India based on the Indian
metallurgical coal data has always been a

374

difficult task. In India, preparation plant circuit
optimization is the key to ac hieving
metallurgical clean coal specification of 16-18%
ash (typical dry-basis) with the maximum
plant c lean c oal (metallurgic al) yield.
Optimization is a real challenge in India when
one has to deal with the Indian coal from
Gondwana origin, which has very high near
gravity materials (NGM) (>25%). The general
practice in India is to crush the Run-of-Mine
(ROM) coal to a top size of 13mm. It has been
widely accepted that crushing the coal to
smaller top size will provide better ash
liberation (Ryan et al., 1999). The conventional
Indian coal preparation plants are designed to
deslime the raw coal at 0.5mm and the 13mm x
0.5mm coarse coal reports to the HM Cyclone
circuits. The primary and secondary HM
Cyc lone c irc uits produc e the c lean
(metallurgical) coal and middling (power
station coal at around 33-34% ash). The -0.5mm
fine clean coal is obtained from the flotation
process.
In North America, the general practice is to
crush the ROM coal to approximately 50mm
top size and clean 50mm x 0 raw coal in a coal
preparation plant. The amount of NGM in the
coals mined in these regions is very low.
Moreover, this methodology also enables a
reduction in the amount of fines generated in
the preparation plant feed (crushing done at
much coarser size). These plants deslime at
1mm, with 50mm x 1mm going to the HM
Cyclone circuit and the 1mm x 0.25mm (or even
0.15mm) raw coal in water-based gravity
separation circuit (reflux classifier™, teeter bed
separator, spiral, water-only-cyclone etc.), with
the -0.25mm raw coal passing to flotation. The
plant circuitry in these regions are typically
optimized and designed based on the equal
incremental ash method (Abbott, 1982, Rayner,
1987, Bethell et al., 2006, Gupta et al., 2006,
Watters et al., 2010). More information on the
375
MPT-2013
equal incremental ash method is mentioned in
the Results and Discussion section.
This paper discusses a plant optimization
study performed based on three Indian coal
sample data from the Jharkhand area. Plant
simulations were performed using the equal
incremental ash method in LIMN™ flowsheet
processing software. The simulations were
performed and c ompared between the
conventional India plant circuitry (HM Cyclone
– Flotation) and the proposed plant circuitry
(HM Cyclone – Reflux Classifier™ – Flotation)
with a 13mm top size plant feed. The results of
these simulations have been discussed in this
paper.
2. Plant Feed Data Preparation for Simulation
Raw Coal data for 50mm x 0 size from three
different samples (1, 2 and 3) from Jharkhand
region were used for the coal quality analysis.
The intention of performing the coal quality
analysis was to form a representative plant feed
size distribution and washability data for
accurate simulations.
The original 50mm x 0 size distribution data in
all the three samples indicated that the dry
sc reening methodology was used. Dry
screening data do not represent the actual plant
feed. In dry sc reening, lots of fine c oal
agglomerate to the surface of the coarse coal
and report to the oversize material. This shows
less fines (-1mm or -0.5mm) in the size
distribution than in the actual plant feed. The
fines circuit could be under-designed if the dry
screening size distribution data is directly used
verbatim. Conversely, dry screening also
changes the washability of the coarse size
fractions due to the presence of fines in the
coarse coal.
A typical sampling methodology used in North
America is to use wet screening or sieving at
6mm and below and prepare the washability
data based on that. This method generates a
 MPT-2013

more ac c urate size distribution and Table 2: Predicted 50mm x 0 Size Distribution
washability data to be used for simulations and Data for Three Samples Based on Wet
plant process design. Table 1 shows the original Screening
dry screening size distribution data of the three
Sample 1 Sample 2 Sample 3
samples. Size (mm) Cumulative Cumulative Cumulative

Table 1: Original size distribution data for Top Bottom Wt. (%) Ash (%) Wt. (%) Ash (%) Wt. (%) Ash (%)
50 x 25 6.0 39.1 5.0 33.4 7.0 42.2
three samples based on dry screening 25 x 13 20.5 38.6 16.0 33.0 25.0 41.8
13 x 6 40.0 38.3 31.5 32.9 45.5 41.6
Sample 1 Sample 2 Sample 3
6 x 3 56.0 38.1 48.0 32.8 60.0 41.3
HGI*= 72 HGI = 84 HGI = 68
3 x 1 75.0 37.9 70.5 32.6 77.0 41.1
SIZE (mm) Cumulative Cumulative Cumulative
1 x 0.5 81.5 37.8 77.0 32.5 83.0 41.1
Top Bottom Wt. (%) Ash (%) Wt. (%) Ash (%) Wt. (%) Ash (%)
50 x 25 57.8 39.0 42.1 33.4 50.3 42.2 0.5 x 0.25 86.0 37.8 83.0 32.5 87.0 41.1

25 x 13 78.6 38.6 60.3
13 x 6 88.3 38.4 74.5
6 x 3 92.6 38.2 85.1
3 x 0.5 96.3 37.9 92.5
0.5 x 0 100.0 37.6 100.0
The following steps were taken to adjust the
50mm x 0 dry screening sizing and washability
data to form the 50mm x 0 wet screening sizing
and washability data. This 50mm x 0 wet
screening data was eventually used to form the
13mm x 0 wet screening plant feed data.
Step 1 - Size distribution and ash adjustment
of the 50mm x 0 dry screening data to determine
the 50mm x 0 wet screening data: From
historical data of the same HGI coals worldwide
with 50mm top size, an adjusted plant feed size
distribution for wet screening was assumed to
take degradation into considerations. These
predicted wet screening size distribution data
(50mm x 0) of the three samples showed more
fines (-1mm) than the dry screening data. The
fractional size ash contents were adjusted
acc ordingly while maintaining the same
sample head ash.
After plotting the new wet screening size
distribution in the Rosin-Rammler plot, the
weight percent of plus 1mm and plus 0.25mm
were determined. The washability of 3mm x
1mm and 1mm x 0.5mm were assumed to be
the same as that of 3mm x 0.5mm. Similarly,
the washability of the 0.5mm x 0.25mm and -
0.25mm were assumed to be the same as that of
-0.5mm. Table 2 shows the new wet screening
size distribution data for 50mm x 0 plant feed.
33.1 70.5 41.9 0.25 x 0 100.0 37.6 100.0 32.4 100.0 41.1
33.0 81.6 41.7
32.9 88.2 41.4
32.6 93.5 41.2 Step 2 - Washability Adjustment for the 50mm
32.4 100.0 41.1
x 0 wet screening from the 50mm x 0 dry
screening washability data to maintain the
same head ash:
The washability data of different weight
frac tions of dry screening sample were
adjusted to provide the predicted washability
data for the corresponding size fractions of the
new particle size distribution data. While
adjusting the washability, the ash of individual
specific gravity fractions were kept the same,
while the weight was adjusted to achieve the
new fractional ash of that size fraction. The
original dry screening sample provided the
washability data for the size down to 0.5mm.
There was no washability provided for the size
fractions smaller than 0.5mm. During this
study, the washability of 3mm x 0.5mm from
the dry screening data was assumed to be the
same as that for -0.5mm size fraction. This data
was then adjusted, using the same methodology
mentioned in the previous paragraph, to get
the washability of 0.5mm x 0.25mm. These new
predic ted plant feed wet sc reening size
distribution and adjusted washability for the
three samples were assumed to be the
representative 50mm x 0 plant feeds.
Step 3 – Size, ash and washability adjustment
to get 13mm x 0 wet screening plant feed from
the 50mm x 0 wet screening size and
washability data maintaining the same head
ash: The next step was to determine the 13mm

376
 MPT-2013

x 0 plant feed size and washability data. The 3. Results and Discussions
weight percents of the +13mm size fractions
Liberation comparison between 50mm x 0
from the predicted 50mm x 0 wet screening size
plant feed with 13mm x 0 plant feed in the
fraction data were assumed to be crushed and
proposed circuitry:
distributed in the same particle distribution as
Simulations were performed to evaluate
the -13mm size fractions in the original 50mm
whether changing 50mm x 0 plant feed to
x 0 wet screening data. To obtain the same head
13mm x 0 plant feed would show some increase
ash in 13mm x 0 as that in 50mm x 0, the percent
in the plant yield at the same product ash. This
ash values were adjusted using the same
would justify the effect of crushing the high
methodology as mentioned in Step 1. The
NGM coal for better ash liberation. Figures 1
washability data of the 50mm x 0 were adjusted
and 2 mention the circuits used to perform these
using the same methodology as that in Step 2.
simulations. The simulation results based on
This gave a new 13mm x 0 representative wet
these two circuitry options for the three
screening size and washability data for the
samples are shown in Figures 3, 4 and 5.
plant feed. Table 3 shows the new wet screening
size distribution for 13mm x 0 plant feed.
Table 3: Predicted 13mm x 0 size distribution
data for three samples based on wet screening
Sample 1 Sample 2 Sample 3
Size (mm) Cumulative Cumulative Cumulative
Top Bottom Wt. (%) Ash (%) Wt. (%) Ash (%) Wt. (%) Ash (%)
13 x 6 24.5 38.1 18.5 32.8 27.3 41.5
6 x 3 44.7 38.0 38.1 32.8 46.7 41.2
3 x 1 67.5 37.8 63.0 32.6 65.0 41.1
1 x 0.5 76.7 37.8 72.6 32.5 77.3 41.0
0.5 x 0.25 83.0 37.7 80.3 32.5 84.5 41.0
0.25 x 0 100.0 37.6 100.0 32.4 100.0 41.1

Step 4 – Flotation assumptions for -0.25mm

data using the -0.5mm flotation release analysis
data: In the original 50mm x 0 dry screening Figure 1: Simulation circuitry used for 50mm
data for the three samples, the flotation release x 0 wet screening plant feed data in proposed
analyses were given for the -0.5mm size new plant circuitry (Option 1)
fraction. There was no flotation kinetics data
provided in the original dry screening sample
data. A separate flotation release analysis data
for the -0.25mm size frac tion were not
provided. Assumptions had to be made for the
flotation product yield and ash for the -0.25mm
flotation using the -0.5mm release analysis
data. It was assumed that due to more ash
liberation and a narrower size range in the -
0.25mm size fraction than in the -0.5mm size
fraction, at the same yield, -0.25mm raw coal
flotation should give around 2-3% lower ash in Figure 2: Simulation circuitry used for 13mm
the flotation product than that from -0.5mm x 0 wet screening plant feed data in proposed
flotation. new plant circuitry (Option 2)

377

Figure 3: Simulation results of Sample 1 – Yield
Vs Ash for Option 1 and Option 2
Figure 4: Simulation results of Sample 2 – Yield
Vs Ash for Option 1 and Option 2
378
MPT-2013
Figure 5: Simulation results of Sample 3 – Yield
Vs Ash for Option 1 and Option 2
Figures 3, 4 and 5 clearly showed higher yield
at the same target metallurgical clean coal ash,
which was varied from 16% to 18% (dry-basis).
The simulations were performed using LIMN™
processing flowsheet software using equal
incremental ash approach.
Conventionally, in India the coal plant circuits
are often designed to produce the same product
quality as provided by the coarse coal circuit.
This approach rarely optimizes the plant yield
at a given target ash. A better approach is to
optimize the coarse, intermediate and fine
circuits by using the equal incremental ash
methodology. This concept states that the
maximum clean coal yield is obtained when all
the circuits cut at the same incremental ash,
instead of the same product ash. This concept
has been used worldwide for the plant yield
optimization and selection of the best circuitry
in a coal preparation plant.
Based on the simulation results in Figures 3, 4
and 5, the yields at the same target ash range
(16-18% dry-basis) were found to be higher in
the case of 13mm x 0 plant feed than the 50mm
x 0 feed. Clearly, this indicates that there is
significant ash liberation in the high NGM
Indian coal when the plant feed is crushed to
13mm x 0.
Simulation comparison with 13mm x 0 plant
feed in the proposed circuitry with the
conventional Indian plant circuitry:
The next set of simulations were performed to
c ompare the c irc uitry (c oarse and fine)
conventionally used in India to that used
internationally, particularly in North America.
The top size of the plant feed was kept constant
at 13mm and c irc uit optimization was
performed for the ash range of 16-18% (dry-
basis). Optimization was focused only on the
primary metallurgic al c oal produc t.
Simulations were performed based on the equal

incremental ash method in both the cases.
Figures 2 and 6 show the circuitry used for
simulations. The simulation results for the
three samples are shown in Figures 7, 8 and 9
Figure 6: Simulation circuitry used for 13mm
x 0 wet screening plant feed data in
conventional Indian plant circuitry (Option 3)
Figure 7: Simulation results of Sample 1 – Yield
Vs Ash for Option 2 and Option 3
Figure 8: Simulation results of Sample 2 – Yield
Vs Ash for Option 2 and Option 3
379
MPT-2013
Figure 9: Simulation results of Sample 3 – Yield
Vs Ash for Option 2 and Option 3
From Figures 7, 8 and 9, it can be clearly seen
that the metallurgical clean coal overall plant
yield at the target ash range was higher in the
case of the proposed circuit in option 2. The
overall yield in the proposed circuit is 3-5%
higher at around 16% target ash and 1-2% at
around 18% target ash in all the three samples.
The following are the reasons for desliming coal
at 1mm (not at 0.5mm) and treating 13mm x
1mm (not 13mm x 0.5mm) in HM Cyclone
circuit:
1. The 0.5mm desliming adds fine coal (1mm
x 0.5mm) to the coarse coal (13mm x 1mm)
in the HM Cyclone circuit. This increases
the solids (coal) loading going to the HM
Cyclone circuit, which typically requires
higher media (magnetite and water) flow
to maintain a certain media to coal ratio
(M/C). The inc rease in magnetite
recirculation and the decrease in Mean
Grain Size (MGS) of coal in the HM Cyclone
would typically incur higher magnetite
loss either from the drain and rinse screens
or from the magnetic separators. Therefore,
1mm desliming should reduc e the
operating c ost as c ompared to the
conventional circuitry (Option 3).

2. The coarser coal (13mm x 1mm) in HM
Cyclone circuit increases the MGS of coal.
This increases the drainage capacity of
drain and rinse screens and also increases
the solids dewatering capacity. This tends
to potentially reduce the deslime and drain
& rinse screen sizes and hence helps in
reducing the capital cost of this circuit.
3. For the same size HM Cyclone, a decrease
in solids (coal) in the HM Cyclone feed also
results in increasing the M/C, and this could
be beneficial in improving the cyclone
efficiency for the difficult-to-wash coal.
The following are the reasons for using water-
only gravity separation c irc uit (Reflux
Classifier™) for 1mm x 0.25mm coal:
1. Reflux Classifier ™ is a fluidized bed system
with parallel inc line c hannels above
(Galvin, 2012). The higher-density particles
suspension by base fluidization acts as a
dense medium for gravity separation. The
main advantage of this equipment for this
size fraction is that it is able to separate at
low cut point (1.50 SG50 typical) for this
size range (1mm x 0.25mm) at a very low
Ep (Ecart Probable), which enables a lower
ash product for this size range. This
typic ally allows the HM Cyc lone to
separate at high cut point (SG50) to match
the same incremental ash. This increases the
overall plant yield. This also increases the
coarse coal (13mm x 1mm) product in the
overall clean coal product, which should
help in lowering the overall produc t
moisture.
2. The presenc e of water-based gravity
separation device for 1mm x 0.25mm
reduces the usage of magnetite (because of
1mm x 0.5mm in HM Cyclone and 0.5mm x
0.25mm in flotation in option 3). This helps
reduc e the operating c ost of the coal
preparation plant.
The following are the reasons for using 0.25mm
x 0 in flotation:
380
MPT-2013
1. Flotation is normally a “fixed” process in a
coal processing plant, which means that
there is not much room and time to vary
the parameters to change the yield and ash
during operation bec ause of the
complications of surface chemistry and
flotation kinetics. In option 3, once the
flotation is fixed, the yield optimization
would be difficult to realize in a single HM
Cyclone for 13mm x 0.5mm raw coal. In the
option 2, there are two gravity based
separation circuits: HM Cyclone and Reflux
Classifier™. These two circuits give more
flexibility to adjust the cut points (SG50s)
for different size fractions quickly in a plant
to match the same incremental ash, hence
providing an optimized yield.
2. In the -0.5mm flotation, the recovery of
particles greater than 0.25mm is not easy
to accomplish. It can rarely be done being
very difficult to maintain the yields and
recoveries on a consistent basis. The
princ ipal reason is the buoyanc y
restrictions. It is difficult for the coarse
particles (due to its mass) to make transfer
from the flotation feed slurry to the froth.
In addition, turbulence is much more
pronounc ed at the c oarse size c lass.
Additionally, the froth is much coarser and
sensitive to chemical fluctuations. Lastly,
trying to optimize the flotation for wide
range size distribution is not easy.
Therefore, it is not advised to run both
coarse (0.5mm x 0.25mm) and fine (-
0.25mm) in the same flotation cell.
3. There is relatively more ash liberation in
the -0.25mm size fraction than that is the -
0.5mm size fraction (Yoon et al., 2002). More
liberation should provide lower ash
product in the -0.25mm flotation at the same
yield than in the -0.5mm flotation. This in
turn should allow the HM Cyclone and
Reflux Classifier™ circuit to cut at higher

SG50 and assists in increasing the overall yield
at the same product ash.
4. Since the -0.25mm size fraction in flotation
brings less solids in the flotation circuit
than the -0.5mm size fraction, the reagent
consumption for flotation should decrease
considerably thus reducing the operating
cost.
4. Conclusion
Based on the simulation results, 13mm x 1mm
in HM Cyclone, 1mm x 0.25mm in Reflux
Classifier™ and 0.25mm x 0 (option 2) in
Flotation is the optimized (higher yield at the
target ash) circuitry for Indian metallurgical
coal as compared to the conventional circuitry
(13mm x 0.5mm in HM Cyclone and 0.5mm x 0
in Flotation – option 3) followed in coal
preparation plants in India. The overall plant
yields are 1-5% higher than the conventional
plant circuitry at 16-18% product ash. This new
plant circuitry should also help in reducing the
overall operating costs in regard to magnetite
and flotation reagent consumption by inserting
a water-based gravity separation circuitry for
intermediate coal (1mm x 0.25mm).
Acknowledgement
The authors would like to express gratitude to
David Bingham, David Meadows, Vishal
Gupta, Asa Weber and Philip Thompson (all
from FLSmidth USA) for their valuable
suggestions and support in writing and
reviewing this paper.
References
Abbott, J., 1982. The optimization of process
parameters to maximize the profitability
from a three-c omponent blend, 1 st
Australian Coal Preparation Conference,
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381
MPT-2013
April 6-10, Newcastle, Australia, pp. 87-
105
Bethell, P.J., Luttrell, G.H., Firth, B., 2006.
Comparison of Preparation Plant Design
Practices for Metallurgical and Stream
Coal Applications, XV International Coal
Preparation Conference and Exhibition,
Beijing, China, October 17–20, 2006, pp.
98–110.
Galvin, G., 2012. Development of Reflux
Classifier, Challenges in Fine Coal
Processing, Dewatering and Disposal,
Soc iety of Mining, Metallurgy and
Exploration, Colorado, USA.
Gupta, V., Mohanty, M.K., 2006. Coal
preparation plant optimization: A critical
review of the existing methods,
International Journal of Mineral
Processing, 79(1), pp. 9–17.
Rayner, J.G., 1987. Direct Determination of
Washing Parameters to Maximize Yield at
a Given Ash, Bull. Proc. Australia Inst.
Mining and Metallurgy, 292(8), pp. 67–70.
Ryan, B., Leeder, R., Price, J.T. , Gransden, J.F.,
1999. The effect of coal preparation on the
quality of clean coal and coke, British
Columbia Geological Survey Geological
Fieldwork, 1998, pp.247–275.
Watters, L.A., Dynys, A., Keles, S., Ali, Z.,
Luttrell, G., 2010. Identific ation of
Optimum Strategies for Process of Fine
Coal Streams, XVI International Coal
Preparation Congress 2010 Conference
Proceedings, Lexington, USA, April 25–29,
pp. 30–36.
Yoon, R.H., Luttrell, G.H. , Asmatulu, R., 2002.
Extending the upper particle size limit for
coal flotation, The Journal of the South
Afric an Institute of Mining and
Metallurgy, October 2002, pp.411–416.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Suitability of Froth Flotation in comparison to Spiral Washer for

an existing Coking Coal Washery – A Case Study for its
Improvement in Respect to Yield% at Desired Ash Level
Sanjay Chaudhuri, S.K. Kabiraj, U.S. Chattopadyay, S.C. Maji and T.Gouri
Charan
Coal Preparation Division, CSIR-CIMFR, Digwadih Campus, Dhanbad

Abstract
An operating Coking Coal Washery is presently feeding coal from nine different sources having
varying feed ash contents. The coal fines varies in ash content ranging from 19.5% - 43.6%. For
treating the coal fines, the washery is operating Spiral for last few years. Under operating
conditions the samples were collected from the Washery as Feed to the spiral and products as
well. Detailed investigations were carried out along with Froth Flotation study to compare with
the existing Spiral washer. It was found that Froth Flotation is much better and efficient option to
replace the Spiral Washer in respect to an improvement for the said washery on the basis of
enhancement of yield% at the desired ash level.

Keywords: Coking coal washery; spiral washer; froth flotation.

1. Introduction
The introduction of mechanized, high-
pr oductivity extraction methods has
resulted in run-of-mine coals that are finer
and dirtier than in the past and has given
rise to an increasing need to develop
appropriate cleaning technology. These fines
contain a substantial amount of carbonaceous
matter. Several methods have been proposed
to beneficiate suc h c oal fines. Sp ir al
concentration is a convenient technique for
beneficiating coal fines in the size range 0.5 to
0.15 mm and froth flotation is practiced
worldwide providing good results.
A study was offered to CIMFR, to evaluate the
possibilities for a coking coal washery to
enhance the yield at the desired ash level. The
washery consist of Heavy Medium Bath and
Batac jig for beneficiation of coarse coal, while
for coal fines are fed to a Spiral for recovery of
clean coal. In the existing fine coal circuit, the
Spiral Washer, where the feed coal of size 0.5mm
to 0.15mm (15%) and the unwashed fraction
below 0.15mm(1%) after dewatering directly
mix with clean product. As per the circuit of
the washery expected yield of cleans of the
Spiral is 8% at 18% ash level where as the
unwashed below 0.15mm fraction yields 1% at
18% ash level. Hence the combined clean
product expects a yield of 9% at 18% ash level.
But after detailed investigation it was found
that the efficiency of the Spiral is poor and if
these are treated by flotation an improvement
in the overall recovery may be possible. The
present paper highlights the details on the
improvement of the fine coal circuit through
incorporation of flotation technology.
2. Experimental
The coking coal washery is generating about
16.7% coal fines and the ash content being
40%and this coal fines are being classified in a

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 MPT-2013

hydro cyclone. The underflow of the hydro The coal fines was classified into two sizes viz.,
cyclone is presently being fed to the spirals and -0.5 + 0.15 mm and -0.15mm. Laboratory
the overflow being screened in high frequency flotation tests were carried out on the overall
screens and used separately. coal fines and on the fractions -0.5 + 0.15 mm
Table 1: Size analysis of coal fines and -0.15mm using a Denver D-12 sub-aeration
Size (mm) Wt% Total% Ash% flotation machine with a 2.5 litre capacity cell.
0.5-0.25 48.8 8.1 41.8 Diesel Oil and MIBC are used collector and
0.25-0.15 13.0 2.2 38.8
0.15-0.074 10.2 1.7 33.4
frother respectively. Impeller speed was
-0.074 28.0 4.7 41.6 maintained at 1500 rpm for all the experiments
Total 100.0 16.7 40.6 and the air flow rate is 2.07 meter cube / meter
The raw coal fines generated from feed to the square/minute. The flotation data is shown in
washery was collected. Samples were also Tables 4, 5 & 6 respectively.
collected from feed to the spiral, Spiral cleans
and Spiral rejects when the Washery was under
operational condition. The size analysis of the
coal fines sample was carried out and the data
is presented in Table- 1. The coal fines were
also subjected to float & sink test and the Mayers
Curve was plotted and is depicted in Figure – 1.

Figure 2: Tromp Curve

3. Results and Discussions

The overall ash content of the Feed to washery

was noted to be 36.2%. The quantity of coal fines
-0.5mm is about 16.7% and ash content being
Figure 1: Mayer cruve 40% which is on higher side. From Table 1 it is
To understand the performance of the spiral clear that the sieve analysis of coal fines shows
detailed size analysis and float & sink tests of that it contains ultrafines (below 0.15mm) to
Spiral Feed, Spiral Cleans and Spiral Rejects was the tune of 38.2% ( 6.4% ) with ash content of
carried out. The size analysis data is presented 39.4% and the contribution of + 0.15 fraction as
in Tables – 2. The float & sink data of spiral 61.8% ( 10.3% ) with 41.2% ash.
cleans and rejects was used for plotting the Table 4: Froth Flotation Tests of Raw Coal fines
tromp curve and the same is shown in Figure – (below 0.5mm)
2.
Table 2: Size analysis of Spiral feed and Flotatio Collector1.25kg/t, Collector2.25kg/t, Collector2.75
n Frother 0.25kg/t kg/t, Frother
Products Results Frother 0.42kg/t 0.50kg/t
Wt% Ash% Wt% Ash% Wt% Ash
Size (mm) Spiral Feed Spiral Cleans Spiral Rejects
%
Wt% Ash% Wt% Ash% Wt% Ash%
Conc 34.5 11.1 58.9 14.5 68.1 16.5
+3 0.8 26.5 0.4 17.8 1.5 46.5 Tailing 65.5 54.8 41.1 76.5 31.9 89.9
3-1 3.3 21.8 1.2 16.9 2.6 39.7 Total 100 39.7 100 40 100 39.9
1-0.5 10.7 16.3 5.2 15.4 7.4 36.2
0.5-0.25 29 20.6 23.9 12.7 23.7 41.5
0.25-0.15 19.8 32.3 20.9 18.4 20.2 48.1
0.15-0.074 15.6 47.4 17 26.7 17.3 52.6 The float and sink tests on the coal fines
-0.074 20.8 62.1 31.4 45.7 27.3 62.8
Total 100 38.3 100 26.8 100 49.5 indicated that the theoretical yield% at 18% ash

383
 MPT-2013

content is about 60%, which is depicted in
Figure 1. The coal fines are classified into two
sizes viz., -0.5 + 0.15mm and below 0.15mm.
The fraction 0.5 + 0.15mm was subjected to float
& sink test and it indicates that the theoretical
yield at 18.0% ash level is about 58.8% (6.1%)
and the corresponding rejects being 41.2%
(4.2%) and ash contents 69.7%.
It may be noticed from Table -2 size analysis of
the feed to the spiral, that the below 0.074mm
fraction is to the tune of 20.8% and below
0.15mm is of 36.4% indic ating that the
classification is improper as a result these fines
reporting to the spiral and thereby reducing
the separation efficiency. From the ash balance
of cleans and rejects it may be noted the yield of
cleans in the spiral is about 66.7% and the ash
content being 27.0%, while the rejects is about
33.3% and ash content being 50.1%.
Table 5: Froth Flotation Tests of Raw (0.5
mm to 0.15mm fraction)
The flotation studies on the coal fines (below
0.5mm) indicated that it is possible to recover
about 34.5% (5.8%) clean coal as concentrate at
an ash c ontent of 11.1% under normal
conditions, however the yield% of clean coal
may be increased to 58.9% (9.8%) at ash content
of 14.5% and c lean c oal may be further
augmented to 68.1% (11.4%) at an ash content
of 16.5%, when the collector dosage and frother
dosage was increased.
The coal fines was split into two fractions viz.,
- 0.5 + 0.15 mm and – 0.15mm and the flotation
studies on 0.5 + 0.15mm fraction shows that it
is possible to recover 69.7% (7.2%) clean coal as
concentrate at an ash content of 16.4%. Whereas
when the ultrafines -0.15mm was subjected to
laboratory flotation tests, it was found that it
is possible to achieve flotation concentrate of
73.2% (4.7%) at an ash content of 20.5%.
4. Conclusions

Flotation Collector1.90k Collector2.27k

The coal washery is generating high percentage
Results g/t, Frother g/t, Frother of coal fines and at relatively high ash content.
0.42kg/t 0.50kg/t
Wt% Ash% Wt% Ash% The washery is presently operating spiral for
Conc 63.2 13.4 69.7 16.4 enriching the coal fines. The detailed studies
Tailing 36.8 81.3 30.3 90.2
Total 100 38.4 100 38.8 showed that the performance of the spiral is
poor, whereby it was noticed that good amount
Table- 6: Froth Flotation Tests of Raw Coal of coal is lost in the tailings. The laboratory
fines Coal fines ( - 0.15mm)
flotation studies on the coal fines (below 0.5mm)
Flotation Collector1.14kg/t, Collector1.90kg/t
indicated that it is possible to recover 68.1%
Results Frother 0.25kg/t , Frother 0.42kg/t (11.4%) at an ash content of 16.5%. Hence it
Wt% Ash% Wt% Ash% may be concluded that Froth Flotation is the
Conc 37.1 18.3 73.2 20.5 suitable and efficient replacement of the Spiral
Tailing 62.9 50.7 26.8 86
Total 100 38.7 100 38.1 which can beneficiate the whole below 0.5mm
fraction of substantial quantity (16.7%) of high
Using the washability data of cleans and rejects ash content more proficiently than the spiral
the Efficiency of the Spiral was calculated by as well as enhances the yield of clean coal to the
plotting the Tromp Curve, which is depicted in tune about 4 - 5% at desired ash level whereas
Figure-2 where the Ep was found to be 0.31, d50 Spiral neither beneficiate the whole 0.5mm
being 1.97 and the Organic Efficiency of the spiral fraction particularly the ultrafines nor the coal
being 75.2%. It is clear that the performance of fraction 0.5 - 0.15mm as per the present circuit
the spiral is poor and good quality coal is being properly.
wasted.

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384
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

High Ash Non-Coking Coal from India: Beneficiation and

Implications

A. Vidyadhar*, Renuka and M. Sharma

Mineral Processing Division, CSIR-National Metallurgical Laboratory, Jamshedpur,
India

Abstract
In the entire spectrum of industrialization from global perspective, coal as the primary source of
energy is the fulcrum of major developmental factors on which hinges the growth of economy at
macro level. This supposedly happens to be vital for improvement in quality of living conditions,
thereby, impacting the lives of millions across the world. The International Energy Agency (IEA)
as well as national/regional energy agencies have projected coal to be the key component of energy
mix, well into the future. The primacy of coal as source of energy is factually expected to surpass
the significance of oil as a typical and primary source of energy in next 4-5 years or even earlier.
Indian coal has been observed to be of low quality on account of its high ash content attribute and
the high ash non coking category coal constitutes sizeable quantity of near-gravity materials
(NGM), which entails beneficiation to suit end-user or application specific qualitative level. The
present manuscript demonstrates the beneficiation of high ash non-coking coal from Vasundhara
mines, Odhisa, with 57% ash content intended for scaling down the ash content to 25% in obtaining
clean coal at a reasonable yield, deploying physical beneficiation techniques. The coal was
characterised thoroughly in terms of petrographic characteristics, size analysis, washability,
chemical composition and the gross calorific value of the coal was observed to be 3221 Kcal/kg.
The beneficiation process was initiated at a top size of 6.3 mm after initial deshaling of the ROM
coal. Tactical combination of gravity separation and flotation techniques yielded clean coal with
25% ash at 40% yield and an intermediate clean product with 49% ash at 12% yield. Low ash
content in the final clean coal is possibly achievable from the combined clean coal with 25% ash
content adopting chemical beneficiation route.
Keywords: Non-coking coal; beneficiation; washability; gravity separation; flotation

macro-economic development of the country

1. Introduction
Coal is the vital energy fuel world-over,
statistically contributing to 55% of installed
energy generation capacity during the calendar
year 2011 and it plays a pivotal role in the
* Correspending Author: E-mail: ari@nmlindia.org
(Indian Minerals Year Book, 2011). Indian coal
has been observed to be of low quality on
account of its high ash content attribute and
the high ash non coking c ategory c oal
constitutes sizeable quantity of near-gravity
materials (NGM), which entails beneficiation to
suit end-user or application specific qualitative

385
 MPT-2013

level. The beneficiated coal has immense The mineral matters (mainly the argillites and
potential for being used as a blendable mix for carbonate minerals) occur in dark colour either
metallurgical applications (Reddy and Biswal, as cavity filling or in disseminated form and
2006; Haldar, 2010; Sahu et al. 2011; Gouri contribute 52.7% (Table 1). The gross calorific
Charan et al. 2011) and such blend formulation value of the coal was found to be 3221 kcal/kg.
of clean coal facilities maximising the infusion Table 1: Maceral constituents present in
of non-coking coal with scarce coking coal for Vasundhara coal sample
catering to metallurgical industries, enabling
Petrographic constituents Vol. % Vol. % (Vmmf basis)
lesser dependence on import of high-rank low Normal Vitrinite 14.7 31.1
ash content coke. Vitrinite Oxidised 1.2 2.5

The present study demonstrates the physical Inertinite 25.2 53.3

beneficiation of high ash non-coking coal from Liptinite 6.2 13.1

Mineral matter 52.7 -
Vasundhara mines of Odhisa with 57% ash
content intended for scaling down the ash
content to 25% for sponge iron in obtaining
c lean c oal at a reasonable yield and the
middlings for power generation.

2. Experimental
2.1. Raw material
High-ash non-c oking c oal sample from (a) Photomicrograph showing mineral matter
Vasundhra mines, Odhisa was taken up for the (black and brown) under reflected light.
present investigation.
2.2. Petrographic Studies
Coal petrography was done though Advanced
Polarizing Mic roscope DM 4500 (Leic a,
Germany) following IS-9127. Petrographic
investigation on polished grains (16 #) of
Vasundhara coals unravelled vitrinite maceral (b) Photomic rograph showing inertinite
is 14.7% (31.1% Vmmf) while oxidised vitrinite mac eral (white) and vitrinite (grey) and
content is 1.2% (2.5% vmmf), thus, reveals mineral matter (brown) under reflected light.
deficiency of overall vitrinite maceral. Oxidised
vitrinite shows oxidation cracks. Inertinites are
dominant and are represented by semifusinites
with small cellular structures and brighter
colour, fusinites with prominent cell cavities
and bright colour, inertodetrinites in bright
fragmental form, contributing 25.2% (53.3%
vmmf), while liptinite macerals occur with (c) Photomicrograph showing vitrinite grain
thread like appearance in dark colour 6.2 % (grey) inertodetrinites (white) and mineral
(13.1% vmmf). matter (dark) under reflected light.
386
 MPT-2013

Size (mm) Wt % Ash %

 50 + 25 44.13 57.51
 25 + 20 15.30 58.04
 20 + 15 1.18 57.62
 15 + 10 13.04 56.49
 10 + 8 1.24 60.38
 8 + 6.3 3.87 60.18
 6.3 + 3 5.71 59.84
(d) Photomicrograph showing vitrinite grain  3 + 2.81 0.21 60.66
 2.81 + 1.68 5.07 59.29
(grey) inertinite (white) and mineral matter
 1.68 + 1.20 1.30 58.02
(dark) under reflected light.  1.20 + 0.85 1.06 56.84
Fig. 1: Photomicrographs of macerals and  0.85 + 0.50 1.43 53.74
 0.50 + 0.42 0.61 56.26
mineral matter studied under DM4500
 0.42 + 0.30 0.95 53.74
polarizing coal petrological microscope  0.30 + 0.21 0.46 52.44
(studied under oil immersion using 20 X  0.21 + 0.15 0.38 54.79
 0.15 + 0.10 0.35 55.65
objective).
 0.10 + 0.075 0.30 58.43
Chemical constituents through proximate  0.075 + 0.063 0.10 48.94
analysis of raw coal are shown in Table 2.  0.063 + 0.045 0.29 58.02
Table 2: Proximate analysis of the coal sample  0.045 3.01 62.01
Total 100.00 57.82

Moisture Content % Volatile Matter% Ash Content% Fixed Carbon%

22.4
3.8 57.4
2.3. Size Analysis
The size analysis of non-coking coal, as received
from Vasundhara mines, Odhisa was carried
out by dry sieving techniques to identify the
percentage of ash, volatile matter and moisture
content at various size fractions. The raw coal
was initially screened at 50 mm; the plus 50
mm fraction was crushed in a single roll
crusher. The overall combined fraction of the
product below 50 mm was subjected to screen
analysis. The size distribution of coal crushed
to 50 mm is shown in Table 3. It is seen that
about 73% of the crushed material was above
10 mm. The  0.5 mm fraction was about 6%,
and its ash percentage varied from 49%.
Table 3: Size and chemical analysis of raw coal
crushed to 50 mm
2.4. Washability Studies
20.2
In order to study the feasibility of deploying
gravity based techniques for coal cleaning,
washability studies were carried out on the
Vasundhara coal sample. Considering the high
ash content of this c oal, the washability
characteristics were determined at a top size of
6.3 mm first. The size fractions - 6.3 + 3 mm, - 3
+ 1 mm, - 1 + 0.5 mm and - 0.5 mm were
subjected to float and sink tests, and the relative
density range was observed to be 1.40 to 2.00.
The generated data was used for plotting
washability curve to establish the washability
characteristics. The theoretical maximum yield
at 25% ash level was observed to be around
20%. Not much improvement was observed in
washability characteristics when crushed to a
top size of 3 mm, however, quite a bit of
improvement is observed when the same
crushed to 1.18 mm top size. The washability
characteristics are shown in Fig. 2.

387

Fig. 2: Washability characteristics of
vasundhara coal
3. Results and discussion
3.1. Physical beneficiation
This coal (ROM) had very high ash content
(~57%). Initially, it was targeted to obtain a clean
coal with around 25% ash at a reasonable yield
through physical beneficiation and then adopt
chemical route to achieve low ash target. The
washability data indicated that over 30% yield
is achievable in the clean coal through gravity
concentration at a target ash level of 25% when
the coal is crushed to - 1.18 mm size. The
maximum yield drops below 20% when
crushed to a top size of 6.3 mm. However,
considering the high ash of the feed, it was
decided to deshale the feed ROM coal and then
initiate the processing at a top size of 6.3 mm.
The following Table 4 gives the deshaling data
reveals that around 20% of the material is
rejected at an ash level of 77%. The deshaled
feed still contains nearly 53% ash and this
material is c onsidered the raw feed for
subsequent processing.
Table 4: Deshaling data of raw coal
Products Wt% Ash%
ROM Coal 100 57.5
Rejects 20.2 77.2
Deshaled Feed 79.8 52.7
388
MPT-2013
Processing was initiated at 6.3 mm top size for
this coal. The coal was crushed and the size
analysis of the crushed feed is shown in the
following table. Table 5 illustrates the ash
distribution in the size classes as indicated for
the process feed.
Table 5: Ash distribution of process feed in
different size classes
Size (mm) Wt% Ash%
 6.3 + 3 34.7 53.8
3 + 1.18 34.6 52.6
 1.18 + 0.5 14.3 51.4
 0.5 16.4 50.2
Tota l 100.0 52.5
The deshaled feed material was crushed to a
top size of 6.3 mm and was fractionated into -
6.3 + 1.18, - 1.18 + 0.5 and - 0.5 mm size classes.
The coarse fraction was treated in jigging
operation to recover a relatively cleaner
product with 42% ash. The jig concentrate was
crushed to - 1.18 mm size and the - 1.18 + 0.5
mm fraction was treated in a spiral-floatex
circ uit, while the - 0.5 mm frac tion was
subjected to flotation. The spiral-floatex circuit
produced a clean coal with 24.6% ash at a mass
yield of 10.4%. The tailings streams were mixed
with the original intermediate size fraction. The
jig tails had 69% ash and this product was
crushed to - 0.5 mm size for flotation.
The combined - 1.18 + 0.5 mm fraction was
treated in a separate spiral-floatex circuit which
generated clean coal with 26.5% ash at 10%
yield. One of the tailings from this circuit had
79% ash which was considered a reject. The
other tailing stream had 60% ash and was
crushed to - 0.5 mm size for flotation.
The combined - 0.5 mm material was treated in
flotation through a rougher-cleaner-recleaner
circuit. The rougher tailing was a reject with
80% ash and 24% yield, while the cleaner tailing
with 68% ash content was also considered a
reject. The re-cleaner tailing with 49% ash can
 MPT-2013

be recycled as cleaner feed. The concentrate of
the re-cleaner contains 25% ash with a mass
yield of ~20%. All the clean coal streams with
around 25% ash are combined to give a mass
yield of 40%. The process flowsheet is shown in
Fig. 3 and the product streams of physical
beneficiation are summarized as follows:
Clean coal with 25% ash is generated at a mass
yield of 34%. The reject stream (rougher tailing)
has 80% ash content and 31% yield. The re-
cleaner tailing (40% ash and ~15% yield) is
intended for recycling as cleaner feed. The
cleaner tailing (66% ash at 21% yield) may also
be considered as a reject stream. This coal has
poorer floatability, thus, unsustainable for
being treated by flotation alone.

4. Conclusions

Indian coals in general are of drift origin. Most

of the non-coking coals have high ash content
which is not suitable for direct utilization. The
high ash non-coking coal from Vasundhara
mines of Odhisa was characterised thoroughly
in terms of petrography, size analysis,
washability and chemical composition and the
gross calorific value of the coal was observed
to be 3221 Kcal/kg. The coal was initially
deshaled and subsequently processed at a top
Fig. 3: Physical processing flowsheet of size of 6.3 mm. Tactical combination of gravity
Vasundhara coal separation and flotation techniques yielded
1. Clean coal with 25% ash at 40% yield clean coal with 25% ash at 40% yield and an
2. Intermediate clean product with 49% ash intermediate clean product with 49% ash at
at 12% yield 12% yield. A suitable flow sc heme for
3. Intermediate reject product with 68% ash beneficiation of high ash non-coking coal was
at 18% yield suggested. Low ash content in the final clean
4. Reject stream with 80% ash at 30% yield coal is possibly achievable from product mix of
In view of the fact that nearly 73% of the raw clean coal with 25% ash content, adopting
material is ending up being treated in flotation chemical beneficiation route.
circuit, exploring the possibility of treating the
Acknowledgements
entire deshaled coal by flotation alone was felt
desirable. The raw material was crushed to - The financial support from Ministry of Steel,
0.5 mm and was treated in a rougher-cleaner- Government of India under the project titled
recleaner circuit. The following Table 6 gives “Development of technology to produce clean
the flotation data. coal from high ash and high sulphur Indian
Table 6: Flotation results of raw coal crushed coals” (GAP-0243) is gratefully acknowledged.
to - 0.5 mm References
Rougher Wt% Ash% Cleaner Wt% Ash% Re-cleaner Wt% Ash% Gouri Charan, T.R., Chattopadhyay, U.S., Singh,
Conc. 69.2 40.7 Conc. 48.4 29.7 Conc. 33.8 25.3
Tails 30.8 79.6 Tails 20.8 66.3 Tails 14.6 39.9 K.M.P., Kabiraj, S.K., Haldar, D.D., 2011.
Feed 100.0 52.7 Feed 69.2 40.7 Feed 48.4 29.7
Beneficiation of high-ash, Indian non-

389

c oking c oal by dry jigging. Minerals &
Metallurgical Processing 28 (1), 21-23.
Haldar, D.D., 2010. Beneficiation of non-coking
coals: Basic concepts and technology
routes. Proc. XI International Seminar on
Mineral Processing Technology (MPT-
2010)., R. Singh., A. Das., P.K. Banerjee., K.K.
Bhattacharyya., N.G. Goswami (Eds.),
NML Jamshedpur, pp. 419-427.
Indian Minerals Year Book., 2011. Coal & Lignite.
Indian Bureau of Mines., Chapter 24.
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390
MPT-2013
Reddy, P.S.R., Biswal, S.K., 2006. Beneficiation
of non-c oking c oal for metallurgic al
purpose. Proc. International Seminar on
Mineral Processing Technology (MPT-
2006)., G. Bhaskar Raju, S. Prabhakar, S.
Subba Rao, D.S. Rao and T.V.V. Kumar
(Eds.), pp. 595-604.
Sahu, A.K., Tripathy, A., Biswal, S.K., Parida, A.,
2011. Stability study of an air dense
medium fluidized bed separator for
beneficiation of high-ash Indian coal. Int.
J. Coal Preparation and Utilization. 31 (3-
4), 127-148.
 MPT-2013

Proceedings of the XIII International Seminar on

Mineral Processing Technology (MPT-2013)

©CSIR-IMMT, Bhubaneswar

Recovery of Settling Pond Coal Fines through Physico-Chemical

Techniques for Optimum Utilization

U.S. Chattopadhyay1, T. Gouri Charan1 and R. Venugopal2

1
CSIR-Central Institute of Mining & Fuel Research, Dhanbad
2
Indian School of Mines, Dhanbad

Abstract
The coking coal fines (-0.5mm) generated from various coal washeries are lying in the lagoons/
settling ponds for decades long which is to the tune of around 3.5 million tonnes. In addition to
these a huge quantity are bled every month to these waste basins on a regular basis. These fines
are basically vitrinite enriched coking material which can be utilized properly if beneficiated in a
judicious manner. Beneficiation of this coal slurry by physico chemical techniques is assuming
increasing importance in India. The present study of beneficiation of these waste settling pond
fines can recover fine cleans (ash <15%) which if used suitably can improve the coking property of
the coke oven blend for coke making. The present paper highlights the work carried out on coal
samples collected from the ponds nearby the washeries. The results indicated that good amount
of coking coal with less than 15% ash may be recovered and used for metallurgical purposes.

Keywords: Settling pond; coal slurry; physico- chemical process.

1. Introduction beneficiated could have augmented the supply

The coal beneficiation process adopted by
central coal washeries produce approximately
1.6 million tones of slurry annually. This slurry
is yet to be beneficiated in large scale flotation
units, which are still to be made operational.
This results in the accumulation of slurry/fines
and creates tremendous problem for the
existing washeries. Moreover, due to its high
ash content (more than 25%), such fines cannot
be mixed with clean coal and are sold for
domestic coke making, brick making and other
non metallurgical uses. Thus huge quantity of
potentially enriched coking coal material is
virtually wasted, whic h, if properly
of scarce coking coal to the steel industry. CFRI
through dec ade long R&D efforts have
developed an improved process technology
that can recover finest cleans (ash less tan 15%)
from the said high ash coal slurry with an
overall yield of approximately 50% at less than
20% moisture.
The flotation plant for beneficiation of coking
coal fines can recover fines clean (ash <15%)
which can improve the quality and value of coke
made in blend with inferior raw coal in suitable
proportion. The present study has been carried
out in a min flotation plant for beneficiation of
coking coal fines. The study has been carried
out to develop an empirical model for

391

optimizing the reagent doses for maximizing
yield at clean coal of 15% or less.
Thus by application of the optimization
tec hnique it may be possible to suggest
desirable level of yield and ash content values
of finer size fractions of c oal treated in
washeries. The problem confines to selection of
conditions for flotation of fine coal slurries
which will produce the desired result.
The continuous technique in studying the rate
of coal flotation was established by Brown et al
(1952) wherein a simple proportionality
between rate and cell concentration for a
limited pulp density. Sublik et al (1983)
attempted to explain the influence of ultrafine
coal particles (below 0.06 mm) on the floatability
of three phase system constituting solid, liquid
and gas (normally air). Aeration and bubble
characteristic for the recovery of fine particles
were studied by Jameson (1983). It is observed
by Tarhar (1981) that by the use of sufficient
quantity of collector to effectively coal the
surface area developed by the increase in fines
content can reduce the ash content of the
concentrate to a reasonable extent. Kalyan Sen
et al (1984) studied the effect of varying both
the collector and frother doses on the flotation
products which was significant to optimize the
flotation circuit. A recent published report by
Yoon (1984) said that coal particles below
(approximately) 38 micron in diameter are
difficult to float and consume more quantity of
reagents.
2. Experimental Procedure
For each Flotation test required amount of
slurry sample collected from a Commercial Coal
washing Plant was taken in a beaker and made
into slurry with a known volume of water and
kept 30 minutes for proper wetting. Then the
slurry was transferred into a 2.5 lit cell of
Denver -12 machine and the rest of the water
was added to maintain required pulp density.
392
MPT-2013
The slurry then conditioned for 2 min. at an
impeller speed 1500 r.p.m. The conditioning
time of pre-wetted sample (at 33% solid content)
with calculated diesel oil for 2 min. and mixing
time of frother was 0.5min, after dilution to fill
the cell upto 25mm from overflow brim. Then
the air inlet valve was opened and the
c oncentrate was collec ted in a tray. The
concentrate and tailings were filtered, dried and
analyzed for ash c ontent. After some
exploratory tests a set of 13 experiments were
carried out to study the selection of the process
and operating variables and ash content of the
products considering the collector and frother
doses as mentioned in Table 1.
Laboratory flotation tests were carried out to
study under the following conditions:
Size of the feed particle : -0.5mm
Impeller speed : 1500 r.p.m
pH of the Slurry : Neutral
Conditioning time : 2 min.
Solid content during Conditioning : 33% by wt.
Air rate (m3/m2/min.) : 2.07
Table 1: Level of Collector and Frother doses
Diesel Oil(Kg/t) Frother(Kg/t)
Principle Level 1.25-1.75 0.25-0.36
Incremental Size 0.25 0.50
The Process
The process adopted for the production of low
ash good quality coking coal in mini coal
beneficiation plant is a specially designed Froth
flotation system.
The fine coal particles of size below 0.5mm are
conditioned in a conditioner by using water
and collector (like, diesel oil). Conditioned coal
slurry is then fed into a series of flotation cells
where air bubbles are generated by the rotation
of high-speed impellers of special design, with
the help of a frother.
Thus the coaly particles float on to the surface
of the cell as froth. The ash forming mineral
matter remains in the pulp and is discharged
 MPT-2013

from cell as tailings. The froth containing low Table 3: Optimum doses of Collector and
ash coal is dewatered and separated as cake Frother
used as coking blend for metallurgical coke
Collector Frother Yield% Ash%
making.
Dose(kg/t) Dose(kg/t)
The objective of a flotation cell is to operate at a 1.55 0.35 75.5 14.0
high yield while producing low ash clean coal.
In order to achieve these objective, optimal 3. Results and Discussion
operating c onditions is essential. Henc e Regression model equation has been developed
optimization procedure depends upon complex considering collector dosage and frother dosage.
interaction between the structural variables, The complete design matrix together with the
response values obtained from the
which define the inter-connection between the experimental works is given in Table - 4 . The
process parameters such as pulp density, centre runs (0 and 0) were repeated five times
aeration rate, reagent dose etc. which affect the as they contribute to the estimation of the
flotation performance of the individual cell. quadratic terms in the model. Based upon the
Designed experiments were carried out under design of experiment the following equations
have been developed.
predetermined condition using Box Hunter
Conc.(Wt%) = 73.24-
Method with the frother and collector as 1.75(CD)+4.24(FD)+2.73(CD)2-
variables to find out the maximum yield at 3.15(FD)2+5.83(CD)(FD)
desired ash level. The coded and natural form Conc.(Ash%) = 14.26-0.33(CD)-
of the design matrix is depicted in Table: 2. The 0.0004(FD)+0.56(CD)2-0.37(FD)2+0.78(CD)(FD)
optimum doses for collector and frother is Where , CD = Collector dose
FD = Frother dose
shown in Table 3.
Table 4: Response values from Design of
Table 2: Coded and natural form of Design
Experiments
Matrix
Expt.
No Collector Frother Concentrate Tailings
No of Coded Form Natural Form
Kg/t Kg/t Wt% Ash% Wt% Ash%
Observation X1 X2 Z1 Z2 1 1.75 0.35 79.9 15.5 20.1 65.1
1 +1 +1 1.75 0.35 2 1.25 0.35 71.2 13.6 28.8 54.2
3 1.75 0.25 65.0 14.2 38.8 44.1
2 -1 +1 1.25 0.35
4 1.25 0.25 79.4 16.1 22.9 56.8
3 +1 -1 1.75 0.25 5 1.15 0.30 80.6 15.9 19.4 65.5
4 -1 -1 1.25 0.25 6 1.85 0.30 74.6 14.4 25.4 61.2
7 1.50 0.23 56.3 12.7 40.7 42.8
5 -1.412 0 1.147 0.3 8 1.50 0.37 75.4 13.9 24.6 58.1
6 +1.412 0 1.853 0.3 9 1.50 0.30 75.1 14.7 24.9 58.6
10 1.50 0.30 71.2 14.0 28.8 57.0
7 0 -1.412 1.5 0.229
11 1.50 0.30 73.1 14.2 26.9 56.2
8 0 +1.412 1.5 0.37 12 1.50 0.30 74.0 13.9 26.0 58.7
9 0 0 1.5 0.3 13 1.50 0.30 72.8 14.6 27.2 58.1

10 0 0 1.5 0.3
11 0 0 1.5 0.3
The detailed kinetic study at 15 sec, 30 sec, 60 sec,
12 0 0 1.5 0.3
120 sec, and 240 sec has been carried out after
optimization of the process parameters like
13 0 0 1.5 0.3
reagent doses. It was observed that within 60 sec,
around 75% of the concentrate with average ash
of 14.5% is possible from the present sample as
depicted in Table 5.
Table 5: Kinetic Study
Sam Feed.
. No Ash% 15 Sec 30 Sec 60 Sec 120 Sec 240 Sec Tailings
Ash
Wt% Ash% Wt% Ash% Wt% Ash% Wt% Ash% Wt% Ash% Wt% %
1 26 50 14.4 15 14.7 10.2 15 1.2 35.5 0.8 47.5 22.8 60.2

393

4. Conclusions
The regression equation for the flotation yield
and ash obtained from the data generated
through the designed of experiment was used
to predict the maximum yield at 14% ash level.
Constrained non linear optimization
programme (ROSENBROCK) was used to get
the values of the frother and collector dose for
the maximum yield of cleans at desired ash level
of 14%. The maximum yield was 75.7%. The feed
ash of slurry used for the optimization is 26.0%.
It was observed from the material balancing of
the plant data that the yield of cleans at 14%
ash level is about 69%, whereas in the
optimization of the laboratory data shows that
the yield at 14% ash level is 75.7%. To obtain
the maximum yield of clean coal at desired ash
level (i.e.14% ash), optimization of other
structural variables namely pulp density,
aeration rate, RPM etc should be considered.
From the detailed kinetic study was observed
that within 60 sec, around 75% of the
concentrate with average ash of 14.5% is
possible from the present sample.
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