Minerals Engineering xxx (2012) xxx–xxx

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Minerals Engineering
journal homepage: www.elsevier.com/locate/mineng

Prediction of flotation behavior of sulphide ores by oxidation index

Ozlem Bicak ⇑, Zafir Ekmekci
Hacettepe University, Mining Engineering Department, 06800 Beytepe, Ankara, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: In addition to size, density, composition and mineralogy (mineral type, texture, liberation, etc.), surface
Available online xxxx characteristics of sulphide minerals affects flotation behavior of sulphide ores considerably. The variations
in surface characteristics of sulphide minerals can be related to the variations to the degree of surface
Keywords: oxidation which is known to influence the flotation performance. Surface oxidation affects dissolution
Froth flotation behavior of sulphide minerals, activation/depression and adsorption of collectors, i.e. their flotation behav-
Oxidation ior. Therefore, a methodology, called ‘‘Oxidation Index’’ was developed to measure surface oxidation of
Sulphide ores
sulphide minerals quantitatively and predict flotation behavior of different ore types. The methodology
is based on derivation of an ore specific calibration curve and prediction of flotation performance of differ-
ent ore types from the same deposit by using the calibration curve. The results of the test works performed
using a complex Cu–Zn sulphide ore from Çayeli Bakır Is _ßletmeleri A.Sß., Turkey are discussed in this paper.
Ó 2012 Published by Elsevier Ltd.

1. Introduction determine the degree of oxidation which are basically Eh (Baker

Mineralization in sulphide ore deposits is generally not homog-
enous. In the same ore deposit, it is likely to observe ore types with
different mineralization, different degree of liberation and also sur-
face oxidation (Ekmekci et al., 2010; Bojcevski et al., 1998; Vink,
1997; Jones, 1987). These variations affect flotation performance
significantly depending on the structure of ore. In most of the sul-
phide ore flotation plants, chemical and mineralogical properties of
the flotation feed are periodically measured to control the flotation
process. However, it is likely to observe drastic changes in the flo-
tation response with the same chemical and mineralogical charac-
teristics. This is generally attributed to the changes in surface
properties of the sulphide minerals in the ore due to surface oxida-
tion. Therefore, measurement of surface oxidation of sulphide min-
erals has a crucial importance for plant control. Flotation of
sulphide ores are strongly affected by chemical parameters like
pH, Eh, dissolved ions and surface oxidation. Low degree of surface
oxidation may enhance the flotation of sulphide minerals by form-
ing surface coatings of metal deficient sulphides (Buckley and
Walker, 1988), elemental sulphur (Trahar, 1984) or polysulphides
(Luttrell and Yoon, 1984). However, extensive surface oxidation
generally reduces flotation recovery and selectivity (Senior and
Trahar, 1991; Smart, 1991) by coating the surface of the minerals
with hydrophilic and stable metal oxide/hydroxide species.
Oxidation of sulphide ores may occur due to weathering process
during formation, mining, stockpiling, crushing, milling or flota-
tion. In literature there has been many techniques used to
⇑ Corresponding author. Tel.: +90 3122977600/145; fax: +90 312992155.
E-mail address: obicak@hacettepe.edu.tr (O. Bicak).
et al., 1991), dissolved oxygen demand test (Houot and Duhamet,
1990), EDTA extraction technique (Rumball and Richmond, 1996;
Kant et al., 1994), XPS and Auger surface analysis (Smart, 1991),
optical mineralogy, infrared spectroscopy, flotation, contact angle
and zeta potential. However, most of these techniques have some
limitations particularly in plant scale applications.
Ethylene diamine tetra acetic acid, widely abbreviated as EDTA
is a polyamino carboxylic acid and a colorless, water-soluble solid
acetate. EDTA has the ability to dissolve and form complex with
the oxidation products of sulphide minerals, however does not
react with metal sulphides (Shannon and Trahar, 1986; Grano
et al., 1988; Rumball and Richmond, 1996). EDTA extraction was
found to be the most suitable method for measurement of surface
oxidation both in laboratory and plant scale applications (Bicak
et al., 2008).
Therefore, the aim of this work was to develop a new measure
based on EDTA extraction technique to determine the degree of
oxidation of sulphide ores quantitatively. The surface oxidation
as measured by the new methodology was then related to the
changes in flotation performance.
2. Materials and methods
2.1. Material
In this paper, a copper–zinc massive sulphide complex sulphide
_ßletmeleri A.S
ore from Çayeli Bakır Is ß ., Turkey, containing about 70%
sulphide minerals is used. The average composition of the ore are
given in Table 1.

0892-6875/$ - see front matter Ó 2012 Published by Elsevier Ltd.

http://dx.doi.org/10.1016/j.mineng.2012.05.012

Please cite this article in press as: Bicak, O., Ekmekci, Z. Prediction of flotation behavior of sulphide ores by oxidation index. Miner. Eng. (2012), http://
dx.doi.org/10.1016/j.mineng.2012.05.012
2 O. Bicak, Z. Ekmekci / Minerals Engineering xxx (2012) xxx–xxx
In Çayeli ore, chalcopyrite, pyrite and sphalerite are the main
sulphide ore minerals. In addition to that bornite, galena and chal-
cocite are found in variable proportions in different ore types in the
same deposit.
2.2. Experimental methods
2.2.1. EDTA extraction test
There are many techniques to measure degree of oxidation in
literature but among these techniques, EDTA extraction was found
to be the most suitable for plant applications (Bicak, 2011).
In the EDTA extraction technique, 10–20 g of dry sample is
added into a beaker containing 200 ml of 3% EDTA solution at pH
7.5 and stirred vigorously for 30 min. The beaker is sealed during
extraction to prevent contact with atmosphere. After the extrac-
tion, the pulp is filtered to separate the solution and the solid for
chemical analysis. 3% EDTA solution was used as a standard
solution in all of the tests. pH of the solution was adjusted to 7.5
with NaOH to prevent the formation of metal–EDTA precipitates
(Rumball and Richmond, 1996).
Degree of oxidation is evaluated based on two methods of cal-
culation, Es and Em. Es (Kant et al., 1994) represents the amount
of metal oxidized on the mineral surface which is accepted as an
indication for mineral oxidation, whereas Em (Eq. (1)) value repre-
sents oxidation degree of the ore in total. In this paper, all evalua-
tions are made on the basis of Em Total values.
Amount of metal in solution ðmgÞðCu;Zn;FeÞ
EmðCu;Zm;FeÞ ¼
Amount of solid ðgÞ
2.2.2. Flotation tests
Flotation tests are conducted in a 3 l modified Leeds type flota-
tion machine. Flotation feed is ground at 60% w/w pulp density for
15 min to obtain particle size 80% passing 38 lm. Aerophine
(3418A) and MIBC obtained from Çayeli flotation plant were used
as collector and frother respectively. The flotation tests were per-
formed at 30% w/w pulp density and pH 11.5 by adding CaO to
the mill.
The flotation products were assayed for Cu, Zn and Fe using AAS.
Flotation rate constants calculated by using first order flotation
rate equation.
3. Optimization of EDTA extraction test
Factorial design was used to test the influence of different
parameters in the optimization tests and the results were evalu-
ated by using Design Expert 7.1.5. Surface area of the different size
fractions was measured using BET technique.
Fig. 1 shows the change of Em Total (mg/g) values according to
the changes in extraction time and P80 passing size of material. Em
Total values changes as a function of extraction time and particle
size. The results of EDTA extraction tests showed that the particle
size (surface area) was a significant parameter determining the
amount of extracted metal from the mineral surface (Bicak,
Table 1
Mineralogical and chemical characteristics of a typical Çayeli ore.
Mineral (%) Element (%)
Chalcopyrite 7 Cu 3.5–4
Bornite 0.4 Zn 5–7
Sphalerite 12.72 Fe 28–30
Pyrite 60 Pb 0.5–1.2
Galena 0.6
Others 19.28
Please cite this article in press as: Bicak, O., Ekmekci, Z. Prediction of flotation behavior of sulphide ores by oxidation index. Miner. Eng. (2012), http://
dx.doi.org/10.1016/j.mineng.2012.05.012
6
106 Micron
5 75 Micron
Em Total (mg/g)
38 Micron
4
3
2
1
0
0 50 100 150
Extraction Time (min)
Fig. 1. The changes in Em Total values with extraction time and P80 values of solid
used. (P80: 80% of material passing size).
2011). Therefore, the equations used to calculate Es Cu and Em to-
tal were modified to include surface area (Eqs. (2)–(4)).
Cu Extracted ðmgÞ
Es Cp ðmg=m2 Þ ¼ ð2Þ
Cp ðmgÞ  BET ðm2 =gÞ
Emtotal ¼ EmCu þ EmZn þ EmFe ð3Þ
EmTotal
Em TotalBET ¼ ð4Þ
BET surface area ðm2 =gÞ
In the calculation of Es Cp, chalcopyrite was assumed as the
ð1Þ only copper mineral in the ore. Similar calculations can be done
for the other minerals (sphalerite, galena, pyrite, etc.) by using
the concentrations of the other metals (Zn, Pb, Fe, etc.). Em Total
can be calculated as the ratio of total amount of dissolved metal
by EDTA to the amount of ore used in the extraction and unit sur-
face area (Eq. (4)).
Another significant parameter for extraction is the time of
extraction. Fig. 1 shows clearly that even after two hours, the Em
Total values continue to increase linearly. Similar finding is com-
patible with literature. According to Rumball and Richmond
(1996), complete dissolution of iron takes eight hour. Therefore
for practical reasons, the extraction time was taken as 30 min
and kept constant for all experiments. Particle size which is 80%
38 lm (also flotation size in the plant) were also kept constant
in all tests.
4. Derivation of Oxidation Index
There has been many research works in the literature investi-
gating the effects of surface oxidation on flotation performance.
Some of these techniques are qualitative or at best semi-quantita-
tive and does not give a quantitative index representing the degree
of oxidation of a sulphide ore. Therefore, a quantitative measure-
ments method is required to establish the relationship between
oxidation and flotation performance of a given ore.
Flotation tests were conducted in a 3 lt modified Leeds flotation
machine. The flotation tests were performed at pH 11.5 and 30% w/
w pulp density. 15 g/t MIBC was used in the experiments, the col-
lector dosage was determined according to the copper content of
the feed. Air rate is adjusted to 3 lt/min and the flotation time is
0.5–1.5 – 7 min. The products of the flotation tests were analyzed
for Cu, Zn and Fe. Flotation rate constants calculated by using first
order flotation rate equation (Eq. (5)).
R ¼ R1 xð1  ekt Þ ð5Þ
where, R is the Flotation Recovery (%), R1 the Flotation Recovery at
infinity (%), k the Flotation rate constant (1/min), t is the Flotation
Time (min).
 O. Bicak, Z. Ekmekci / Minerals Engineering xxx (2012) xxx–xxx 3

For this purpose, ‘‘Oxidation Index (OI)’’ is developed to deter- 100 2.0
mine the degree of oxidation of an ore in terms of percentage (%)

Cu Recovery (%)
as given in the following equation. 80 Kümülatif
CumulativeBakır Verimi
Cu Rec. (%)(%)
1.5

k cu (min-1)
Em TotalBET  Em TotalBETmin 60 kkCu
Cu
OI ð%Þ ¼  100 ð6Þ 1.0
Em TotalBETmax  Em TotalBETmin 40

where; Em TotalBET is the Em Total value of a studied ore that has a 0.5
20
random oxidation degree, Em TotalBETmin the Em Total value of ore
that has minimum oxidation degree, Em TotalBETmax is the Em Total 0 0.0
0 20 40 60 80 100
value of ore that has maximum oxidation degree.
Em total values for min and max oxidation conditions are re- Peroxide Concentration (%)
quired to derive an oxidation index and calculate oxidation degree
Fig. 3. The variations in recovery and flotation rate constant of the copper minerals
in percentage. For this purpose, a calibration curve is derived by as a function of peroxide concentration.
oxidizing the ore to different levels artificially using hydrogen
peroxide.
For derivation of the calibration curve, an ore sample with good 100
flotation response was selected from the Çayeli ore deposit. The

Copper Recovery (%)

representative samples from the ore were ground in a ring mill
to obtain a product of 80% 38 lm, which is also flotation particle
size for Çayeli ore. Then, the ore was treated in different concentra-
tions of peroxide solutions (0%, 1%, 5%, 10%, 25%, 50%, 75% and
100%) overnight to obtain ore samples having different degree of
surface oxidation. In order to obtain EDTA extraction result of an
unoxidized sample, a fresh ore sample was subjected to EDTA
washing prior to flotation test acid washing or ultrasonic treatment
can also be used as an alternative method to remove the oxidized
species from the surface of the minerals.
The variation of Oxidation Index (OI) is given in Fig. 2 as a func-
tion of peroxide concentration for both copper minerals and the to-
tal sulphide minerals in the ore. The change in the degree of
oxidation was small up to 10% peroxide concentration, and in-
creased rapidly up to 50% peroxide treatment which gave 80% OI.
Higher concentrations of peroxide oxidized the sulphide minerals
completely.
5. Prediction of flotation performance using Oxidation Index
The relationship between cumulative copper recovery, flotation
rate constant and peroxide concentration is given in Fig. 3. Both the
recovery and flotation rate of the copper minerals decrease expo-
nentially with the peroxide concentration. However, the flotation
recovery decreased to values lower than 5% after 50% peroxide
concentration. This shows that the ore is oxidized almost com-
pletely at this concentration. The relationships between Oxidation
Index and copper recovery and flotation rate of the copper miner-
als in Çayeli ore are illustrated in Figs. 3 and 4 respectively. In these
figures, the legend ‘‘Cp’’ represents the oxidation index based on
surface oxidation of the copper minerals, ‘‘Ore’’ represents the oxi-
dation index based on surface oxidation of all of the sulphide min-
erals in the ore. The results showed that copper recovery decreased
Cp
80
Ore
60
40
20
0
0 20 40 60 80 100
OI
Fig. 4. The relationship between oxidation index and copper recovery on mineral
and ore basis.
exponentially as a function of oxidation index. However, the flota-
tion rate constant of the copper minerals changes linearly as
shown in Fig. 5 Flotation response of the copper minerals was af-
fected slightly up to a certain degree of surface oxidation, which
was about 10% in terms of oxidation index value. Higher values
the flotation performance decreased drastically and the sulphide
minerals in the ore were almost completely depressed at OI values
greater than 75%. The results showed that, the variation in flotation
response of the Çayeli ore could be demonstrated as a function of
oxidation index and the suggested curves represented in Figs. 3
and 4 could be used as the calibration curves to estimate flotation
performance of ore samples from different parts of the ore body.
5.1. Prediction of ore variability
In order to test the flotation performance prediction capability
of the Oxidation Index methodology, ten different ore types having
different mineralogy and chemical composition were obtained

2.0
100
Cp
Cp
80 1.5 Cevher
Ore
k Cu (min-1)

60
OI (%)

1.0

40
Cp 0.5
20 Ore
Cevher
0.0
0 0 20 40 60 80 100
0 20 40 60 80 100 OI (%)
Peroxide Concentration (%)
Fig. 5. The relationship between oxidation index and flotation rate constant on
Fig. 2. The relationship between oxidation index (OI) and peroxide concentration. mineral and ore basis.

Please cite this article in press as: Bicak, O., Ekmekci, Z. Prediction of flotation behavior of sulphide ores by oxidation index. Miner. Eng. (2012), http://
dx.doi.org/10.1016/j.mineng.2012.05.012
4 O. Bicak, Z. Ekmekci / Minerals Engineering xxx (2012) xxx–xxx

from Çayeli mine. The chemical composition of the ore samples are 100 0.30

% Distribution of Cp, Sp, Bn, Py

given in Table 2. 90

% Distribution of Chalcocite
Chemical and mineralogical composition of the ores were very 0.25
80
different from each other. Mineralogical analysis of the ores was
70
performed using the optical microscopy equipped with Clemex im- 0.20
age analysis system. The results showed that the main copper min- 60
eral was chalcopyrite (Fig. 6) for the ores with low copper content, 50 0.15
and in addition to chalcopyrite the secondary copper minerals 40
mostly bornite and chalcocite were found in the ores with high 0.10
30
copper content. The other important sulphide minerals were sphal-
20
erite and pyrite. 0.05
Degree of oxidation of each ore was determined by the EDTA 10
extraction tests as described in Section 2.2. The samples for EDTA 0 0.00
Ore 1 Ore 2 Ore 3 Ore 4 Ore 5 Ore 6 Ore 7 Ore 8 Ore 9 Ore 10
extraction tests were prepared by dry grinding in a ring mill to ob-
Bornite Sphalerite Chalcopyrite Pyrite Chalcocite
tain the flotation particle size (P80:38 micron) and surface area val-
ues were determined, accordingly. Degree of oxidation of the ores Fig. 6. Mineralogical distribution of sulphide minerals.
was determined based on the oxidation index derived from Em val-
ues, i.e. on ore basis. The results showed that the oxidation index of
the ores was different from each other, changing between 3% and
72% (Figs. 7 and 8). This was attributed to both the differences in 100
surface oxidation and also their mineralogical characteristics. 90

Cu Recovery (%)
80
Batch flotation tests were conducted to determine the flotation 70
performance of each ore type and establish the relationship be- 60
tween the oxidation index and flotation performance. As it was 50
40
shown in Table 2, Cu content of the ores varies from 1.47% to 30
16.30%. Hence, the collector dosage for the copper flotation was 20
added according to their copper contents. Ores divided into three 10
0
groups according to their copper contents and the collector dos- 0 20 40 60 80 100
ages added accordingly at 30, 60 and 90 g/t (Bicak, 2011). The rela- OI (%)
tionship between the oxidation index and flotation recovery and
rate constant of copper are illustrated in Figs. 7 and 8, respectively. Fig. 7. The relationship between cumulative copper recovery and oxidation index
The solid curves given in the figures represent the calibration curve for the ore samples from Çayeli.
derived for Çayeli ore as described in the previous section.
Both flotation recovery and rate of the copper minerals de-
creases with oxidation index. The results showed that the oxida-
tion index derived for Çayeli copper ore can be used successfully 2
to predict flotation response of different ore types from the same
deposit. This suggests, it will be possible to predict the flotation 1.5
(min-1)

performance by performing an EDTA extraction test using ore sam-

ples from flotation feed, stock piles or from drill cores to determine
1
degree of oxidation quantitatively. This would help the plant met-
kCu

allurgist to plan the blending strategy and take necessary precau-

tions for plant performance optimization. 0.5

5.2. Plant scale studies in Çayeli flotation plant 0

0 20 40 60 80
As it was explained in the previous sections, it is possible to pre- OI (%)
dict floatability of sulphide ores by using the Oxidation Index
methodology. Hence, the methodology was tested using the sam- Fig. 8. The relationship between flotation rate constant (k) and oxidation index for
the ores from Çayeli.
ples taken from the stockpile and also flotation feed of the plant
for five days. The calibration curve derived for Çayeli ore was used
to predict the flotation performance.
100
Copper Recovery (%)

Table 2
80
Chemical analysis of the ore samples from Çayeli Cu–Zn ore deposit.
April 2009
Sample code %Cu %Zn %Pb %Fe 60
June 2010
Ore 1 15.55 5.47 0.18 29.29 40 Calibration Curve
Ore 2 16.30 5.25 0.14 24.48
Ore 3 2.59 5.40 0.10 24.74 20
Ore 4 1.47 8.39 0.41 31.46
Ore 5 1.89 9.09 0.32 42.63
0
Ore 6 14.92 6.55 0.16 31.15 0 20 40 60 80 100
Ore 7 7.11 7.38 0.02 28.38
Ore 8 2.56 3.76 0.12 27.09
OI (%)
Ore 9 10.42 5.68 0.07 30.69
Ore 10 8.56 8.77 0.07 40.70 Fig. 9. Compatibility of the calibration curve with the results of the EDTA tests
conducted in the plant by Çayeli staff.

Please cite this article in press as: Bicak, O., Ekmekci, Z. Prediction of flotation behavior of sulphide ores by oxidation index. Miner. Eng. (2012), http://
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 O. Bicak, Z. Ekmekci / Minerals Engineering xxx (2012) xxx–xxx 5

Table 3 tation conditions can be modified according to the OI values deter-

Chemical composition of the seven ores from different stockpiles that compose the mined by a simple and quick test.
flotation feed and the flotation feed in Çayeli flotation plant.
The ‘‘Oxidation Index’’ methodology was tested by using Çayeli
Date Stockpile No. Chemical composition Cu–Zn complex sulphide ore (high sulphide mineral content). It
Cu% Zn% Pb% was possible to predict flotation response of different ore types
21.04.2009 Flotation feed 3.60 3.11 0.07
with an acceptable accuracy.
22.04.2009 1ÇT 4.22 2.33 0.07 This work proved that the Oxidation Index methodology is an
23.04.2009 3ÇT 2.88 5.88 0.18 effective tool to predict flotation response of different ore types
24.04.2009 7ÇT 1.87 0.64 0.03 in plant operation. However, more work is required to improve
24.04.2009 7KP 1.79 1.84 0.04
the methodology for prediction of floatability on a size by mineral
15.06.2010 Primary ball mill feed 3.41 7.36 0.36
15.06.2010 3ÇT 3.15 13.83 0.81 basis. So that the ‘‘Oxidation Index’’ can be included as an ore
15.06.2010 8ÇT 0.82 12.20 0.30 parameter to the ‘‘Floatability Component Model’’.
15.06.2010 5ÇT 3.25 14.38 0.89 A patent (Application Number: PCT/IB11/052707) application
18.06.2010 Primary ball mill feed 3.49 6.65 0.35
for Oxidation Index methodology has been applied and Cayeli Cop-
18.06.2010 1KP 4.42 2.27 0.05
18.06.2010 3KP 3.56 10.75 0.63
per Mine has started to use this technique as a standard diagnostic
18.06.2010 6KP 4.50 6.50 0.25 tool.
18.06.2010 7KP 2.47 9.00 0.50
Acknowledgments

Fig. 9 shows the results of the Oxidation Index tests with the
calibration curve for Çayeli ore. It is clearly shown that the results
of the EDTA extraction tests performed in the plant are in good cor-
relation with the calibration curve. These results proves that it is
possible to predict flotation performance of sulphide ores by using
‘‘oxidation index’’ methodology within an acceptable accuracy as
expected.
A similar study was conducted by the plant metallurgists for
longer period. Ore samples were collected between 15 and 18 June
2010 from different ore types in the stockpile and flotation feed to
validate the methodology and test the compatibility of the calibra-
tion curve and the measured degree of oxidation values. The chem-
ical analysis of the ores used in this study are given in Table 3.
The oxidation index derived for the Çayeli copper ore can be
used successfully to predict the flotation response of different ore
types from the same deposit.
6. Conclusions and recommendations
Effects of surface area (particle size) and extraction time were
found to be as important parameters for the EDTA extraction.
The amount of oxidized material on mineral surfaces increases
proportional with the increases in the surface area and extraction
time. Therefore, the equations were modified to include surface
area at constant extraction time.
‘‘Oxidation Index’’ methodology was developed to express de-
gree of oxidation quantitatively. In this methodology, the ore is
oxidized artificially to different degree of oxidation by using hydro-
gen peroxide solutions. Based on the EDTA extraction tests applied
to the artificially oxidized samples, the degree of oxidation is ex-
pressed in terms of percentage (oxidation index, %) and related
to flotation performance. The relationship between oxidation index
and flotation recovery and rate is used as the calibration curve for
prediction of flotation performance of an unknown ore sample
from the same deposit. Therefore, the ‘‘Oxidation Index’’ methodol-
ogy can be used to predict flotation performance of the ore types
before they are fed to the flotation plant. Ore blending and also flo-
The authors gratefully acknowledge technical and financial sup-
_ßletmeleri A.S
port of Çayeli Bakır Is ß . and financial support of The Sci-
entific and Technological Council of Turkey (TÜBITAK) _ Project No:
107M275.
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