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Pozzolanic Characteristics of Palm Oil Waste

Ash (POWA) and Treated Palm Oil Fuel Ash
(TPOFA)

Conference Paper November 2012

DOI: 10.1201/b13165-31

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Pozzolanic Characteristics of Palm Oil Waste Ash (POWA) and Treated
Palm Oil Fuel Ash (TPOFA)
*
Nurdeen M. Altwair1, 2 , M. A. Megat Johari1 & A.M. Zeyad1,3
1
School of Civil Engineering, Engineering Campus, Universiti Sains Malaysia, Nibong Tebal, Malaysia
2
Civil Engineering Department, Faculty of Engineering, Al-Merghab University, Al-Khums, Libya
3
Department of Civil Engineering, University of Sciences and Technology, Sana'a, Yemen
S. F. Saiyid Hashim
School of Materials and Mineral Resources Engineering, Engineering Campus,Universiti Sains Malaysia

ABSTRACT: This work presents the results of the processing of palm oil waste ash (POWA) under controlled
burring conditions in order to obtain materials with pozzolanic properties. Palm oil waste samples were burnt
in an aired electric oven at 800 and 1000 for 6 and 2 h, respectively. Furthermore, treatment of palm oil fuel
ash is also discussed. Ground palm oil fuel ash (GPOFA) was treated by heating at 450 C for 90 min. For both
methods, either ash production from raw materials or ash treatment, pozzolanic characteristics was character-
ized by using chemical analysis, X-ray diffraction (XRD), scanning electron microscopy (SEM) and strength
activity index (SAI). Results obtained conrm that POWA burned at 800 and 1000 C have properties indica-
tive of very high pozzolanic activity. Moreover, no inuence of heat treatment on the pozzolanic properties of
treated POFA.

1 INTRODUCTION en that the ash continuous to increase, therefore

more ash lead to potential environmental problem
Palm oil industry plays a major role in the eco-
when it is disposed as landfill materials due to the
nomic development of several tropical countries.
limitation of its utilization (Safiuddin et al., 2011).
Malaysia was the second largest producer of palm oil
To get a solution for this potential environmental
with around 40% and 41 % of the total world supply
problem, many research studies have been carried
in years 2008-2009 and 2009-2010 respectively.
out to examine the feasibility of using the ash as
(Chandara, 2011). Based on the statistics of Malay-
mineral admixture in blended cement. The beginning
sian Palm Oil Board (MPOB), the fresh fruit bunch
was by Tay (1990), ash from palm oil mills was used
yield is around 20.18 and 19.2 tons per hectare in
to replace Portland cement and showed that it had
year 2010 and 2011 respectively with the total pro-
low pozzolanic property. Later many researchers
duction of fresh fruit bunch around 90,566,927 tons
showed that POFA can be successfully used as a
and 90,070,272, tons in the year 2010 and 2011 re-
supplementary cementitious material in mortar or
spectively (MPOB, 2010). Generally, for every 100
concrete (Megat Johari et al., 2012; Jaturapitakkul et
tons of fresh fruit bunches processed, there were
al., 2007; Rukzon & Chindaprasirt, 2009; Safiuddin
around 20 tons of nut shells, 7 tons of fibers, and 25
et al., 2011; Sata et al., 2004; Sata, Jaturapitakkul, &
tons of empty bunches discharged from the mill (Tay
Rattanashotinunt, 2010). The partial replacement of
& Show, 1995).
Portland cement with POFA can lower the produc-
As the oil price increases, it becomes costly to
tion costs and improve the engineering properties
continue relying on diesel generators to provide
and durability of concrete. Furthermore, POFA can
power supply. For this concern, the shell, fiber and
increase the ecological properties of concrete, con-
empty fruit bunch of palm tree are used extensively
tributing to a healthier and more sustainable envi-
as a fuel to heat the steam for electricity generation
ronment.
and during the palm oil extraction process (Sheng &
This paper presents the research conducted at
Kwang, 2010). After combustion in the steam boiler,
Universiti Sains Malaysia, aimed to determine the
there is around 5% of ash, known as palm oil fuel
characteristics of palm oil waste ash produced under
ash (POFA), being produced (Sata et al., 2004). Giv-
controlled condition at 800 C and 1000 C for 6 and
2 h, respectively. The treatment of palm oil fuel ash
* which was taken directly from the plant boiler was
Corresponding author.
also addressed.
E-mail address: cemamj@eng.usm.my
2 EXPERIMENTAL
2.1 Experimental production of POWA
Palm oil waste (POW) (Fig. 1) was collected
from a near-by palm oil mill and it was first dried in
an oven at 105 C for 24 h. POW was crushed using
the crusher machine followed by milling to the aver-
age particle size of 600m.The ground POW was
burnt at 800 C and 1000 C for 6 and 2 hours, re-
spectively, in an aired electric furnace.
Figure 1. Palm oil waste (POW) before crushing.
Before testing chemical characteristics of palm oil
waste ash (POWA), the samples were subjected to
dry grinding followed by sieving in sieve No.200 (75
m). X-ray Fluorescence (XRF) was used to verify
the chemical compositions of ash. The X-ray diffrac-
tion (XRD) analysis was performed to identify dif-
ferences in the formation of amorphous or crystalline
silica. Morphologies, particle shapes, and particle
agglomeration were studied using a scanning elec-
tron microscope (SEM).A laser diffraction particle
size analyzer was used to measure particle size dis-
tribution and specific surface area. The ash samples
were labeled with appropriate combination of sym-
bols i.e. T and t which correspond to burning tem-
perature (C) and burning time (hour), respectively.
For example, the ash sample prepared by grinding
raw materials at 800 C with a burn time of 6 h was
designated as POWA8006 with T = 800 and t = 4.
As well as the ash which was grinded after burning
was designed as GPOWA8006 with G= ground.
2.2 Experimental treatment of POFA
Un-treated POFA was produced from the burning
palm oil waste (shell, husk and organic fiber) in
boiler at temperature ranging between 800 C to
1000 C. This ash was black in color because it was
contained an unburned different materials such as fi-
bers and nutshells as well as unburned carbon as the
major constituent. For discarding of these materials,
the POFA was dried in the oven at 100C for 24 h
and then sieved using a set of sieves (3 mm, 600
m and 300 m) to remove unburned materials
which are coarser than 300 m. The ash was ground
in a ball mill to reduce the particle size for improv-
ing the reactivity. The mean particle size of POFA
before milling was about 74.29 m with the specific
surface area around 0.054 m2/g. For differentiating
the ground palm oil fuel ash it was designated as
GPOFA. To remove unburned carbon, GPOFA was
heated by low heat treatment at temperature of 450
C for 90 minutes, here in designated as treated
ground palm oil fuel ash (TGPOFA).
2.3 Pozzolanic activity index of ash (SAI)
Pozzolanic activity of POWA has been deter-
mined based on compressive strength according to
ASTM C311 (2005). The test mixture, replaced 20
% of the mass of the amount of cement used in the
control mixture by the same mass of the test sample.
The control mixture was prepared with 1500 g of
Portland cement, 4125 g of graded sand and 726 ml
of water. The test mixture was prepared with 1200 g
of cement, 300 g of ash, 4125 g of graded sand and
requisite quantity of water required for flow of 110%
to 115% of control mixture. Fifty-millimeter cubes
were casted for this experiment. After molding, the
molds were placed in a moist room at27 2 C. Af-
ter 24 h, the specimens were stored in saturated lime
water. The compressive strength was determined for
the three specimens of the control and the test mix-
ture at ages of 3, 7, 14 and 28 days.
3 RESULTS AND DISCUSSION
3.1 POWA characterization
The ash color sometimes depends on the impuri-
ties and chemical composition of the ash. In this
study, it was observed that the temperature and burn
time affected the optical properties of ash. Burning
the ground raw materials to a temperature of 800C
for 6 hours, the ash color became light gray to brown
with earthy texture. The same observations could be
seen for the burning temperature of 1000C, the ash
color became light black and dark brown for 2 hours.
The ash texture changed from coarsely to earthy tex-
ture. However, at burning temperature of 800C and
1000 C for 6 and 2 hours resulted in POWA8006
and POWA10002 with low loss on ignition of 4.02
% and 6.2 %, respectively.
The XRD patterns of POWA samples are shown
in Figure 2. There was no significant crystalline
phase could be detected by the XRD.
Figure 2. XRD patterns of POWA: Q- quartz, S- amorphous sil-
ica, P- potassium gallium silicate, I- Iron chromium oxide, H-
hematite.
 The POWA8006 showed that the main peaks served. The grinding process reduced not only the
were represented by -quartz at peaks of 2 of 21.7, particle size but also the porosity of POWA. In addi-
27.1, 35.9 and 68.5. Iron chromium oxide was de- tion, the grinding led to the increase of specific sur-
tected at peaks of 2 of 49.7and 63.4. While amor- face area from 0.45 to about 8.5 m2/g. The present
phous silica was detected between 2 of 22.3 to results indicate that the amount retained on 45 m
30.2 and 37.5 to 48.8. The XRD pattern of sieve were less than15% and 5 % for Un-ground
POWA10002 showed that the small peak of -quartz POWA and ground POFA respectively (Fig 4).
was detected at two peaks of 2 of 27.1 and 42.3. It
was clear that the majority of the main phases were
represented by amorphous silica which was detected
from 17.5 to 70.2.
Table 1 shows the chemical composition of stud-
ied ash. The activated products were mainly formed
by silica, alumina, and iron oxide. The chemical
composition of POWA samples was limited under
the conditions required for the specification of fly
ash; where all POWA presented in Table 1 were
found to be under the Class F as specified in Figure 4. Particle size distribution of POWA samples.
ASTMC618 (2005).The total main oxides of
POWA8006 and POWA10002 were up to 82.3 and 3.2 Treated POFA characterization
83.4% respectively. The color of treated ground palm oil fuel ash
Table 1. Chemical compositions of ash. (TGPOFA) was light brown to grayish red due to
Ox- Chemical compositions (%) most of the unburned residual has been removed.
ides Palm oil waste ash Palm oil fuel ash
comp. Table 1 shows the chemical compositions of
POWA-8006 POWA-10002 GPOFA TGPOFA
SiO2 50.6 51.9 62.74 66.9 GPOFA and TGPOFA which exhibit that it contains
Al2O3 16.2 17.1 5.32 6.44 10.13% of the LOI before the heat treatment but af-
Fe2O3 15.5 14.4 4.87 5.72 ter the treatment the LOI decreased to around 2.3%.
CaO 1.4 1.5 4.94 5.56 The decrease in LOI value for TGPOFA is compen-
MgO 2.3 2.01 2.51 3.13
Na2O 0.19 0.2 0.15 0.19
sated by the increase in mass percentage of other
K2O 5.5 4.8 4.69 5.20 component. The difference in chemical composition
SO3 0.41 0.14 0.26 0.33 between GPOFA and TGPOFA is due to the differ-
LOI 4.02 6.2 10.13 2.3 ence in their unburned carbon. The main oxides of
treated ash are complied with the specifications of
ASTM C618 class F, with SiO2 + Al2O3 + Fe2O3 of
79.07 %.
Mineral composition of the TGPOFA did not
change much due to the heat treatment. XRD proles
showed that the agglomeration and crystallization of
glassy phase of POFA particles which influence the
pozzolanic property did not take place during the
treatment (Fig.5).
Figure 3. SEM of POWA samples; (a) before grinding (b) after
grinding.

Figure 3 shows SEM photograph of un-ground

POWA and ground POWA. It was found that un-
ground POWA at both temperatures had angular and
irregular particles with median size of about 20 m
and most particles had a porous texture. Further-
more, small particles of carbon were observed with Figure 5. XRD patterns of POFA before and after treatment (Q-
Quartz; C- Cristobalite; S-Amorphous silica; K- potassium
the average particle sizes of about 15m. aluminum phosphate.
Un-ground POWA contained very low carbon
particles of irregular shape. There were no agglom-
eration of particles in the unground POWA photo- GPOFA particles were irregular in shape with a
graph, thus it seems that agglomeration did not occur porous texture. The unburned carbon particles were
during the burn period. After grinding, irregular par- irregular in shape. The unburned particles were ob-
ticles with a smaller, crushed size and free of carbon served in the GPOFA photograph but were absent
with the average particle size of 0.5 m were ob- from the TGPOFA photo. This indicates that the un-
burned carbon had been removed by heat treatment
of GPOFA (Fig. 6).
Figure 6. Scanning electron microscopy (SEM); (a) GPOFA (b)
TPOFA.
Figure 7. Cumulative particle size distribution curves of
GPOFA and TGPOFA.
The average particle size of GPOFA and
TGPOFA were about 2.87 m and 2.96 m, respec-
tively, indicating that there was no signicant change
in the average particle sizes of POFA before and af-
ter treatment. This also proves that the heat treat-
ment did not result in the agglomeration particles
(Fig. 7). The specific surface area of GPOFA and
TGPOFA were around 1.683 m2/ g and 1.521 m2/g,
respectively.
3.3 Strength activity index of GPOWA and TGPOFA
Strength activity index for all mortars containing
TGPOFA and GPOWA are shown in Fig. 8.
Figure 8. Strength activity index of GPOWA and TGPOFA
mortars at 3, 7, 14 and 28 days.
It can be observed that the SAI of TGPOFA-
cement mortar at all ages were higher than the min-
imum requirement of 75% as specified in ASTM C
618. At the early ages of 3 and 7 days, replacing
OPC with 20% TGPOFA was found to improve the
compressive strength by pure cement hydration;
hence, the compressive strength was less than the
reference. At the early ages of TGPOFA-cement
mortar, only the high fineness of POFA particles
plays a role in strength development filling the voids
between the pates and the sand. At 28 days, the
compressive strength of TGPOFA-cement mortar
was higher than the reference cement strength.
At later ages, the silicates or aluminates in amor-
phous react with Ca(OH)2 generated by the hydration
process of cement to produce product of mainly cal-
cium silicate hydrate (C-S-H), thereby improving the
compressive strength.
GPOWA mortars gave higher SAI than control at
all ages. The SAI for mortars with GPOWA8006
and GPOWA10002 at age of 28 days increased to be
117.61% and 118.75%, respectively. This may due
to their high surface area, smaller particle size and
amorphous conditions. The compressive strengths of
mortar with GPOWA10002 developed comparative-
ly slight higher strength compared to mortar contain-
ing GPOWA8006 at all ages. This could be due to
difference in the amount and type of amorphous
phase. GPOWA10002 containing a greater amount
of SiO2 and Al3O2 in amorphous. Both of these ox-
ides play a very important role in the pozzolanic re-
action because they can react with calcium hydrox-
ide, which is released from the hydration of OPC, to
produce mainly products of calcium silicate hydrate
(C-S-H) and calcium aluminium hydrate (C-A-H)
The SAI of mortar containing GPOWA is more than
TGPOFA at all storage ages. This may be attributed
to the GPOWAs have been produced under con-
trolled conditions. In addition, raw materials of
GPOWAs did not contain strange organic materials.
Based on ASTM C618, the chemical and physical
requirements of chosen GPOWA samples were su-
perior compared to TGPOFA sample. The total main
oxides of TGPOFA, GPOWA8006 and
GPOWA10002 were 79.07%, 82.30% and 83.40%,
respectively. The average particle size of TGPOFA,
GPOWA8006 and GPOWA10002 were 2.99, 0.29
and 0.3 m. The specific surface areas were 1521,
8399 and 8121 m2/kg, respectively. From that, it
can be indicated that the pozzolanic reactivity of
GPOWA is higher than TGPOFA.
4 CONCLUSIONS
(1) The palm oil waste can be an important raw ma-
terial for the pozzolan production. POWA
burned at 800 C and 1000 C for 6 and 2 h has
good pozzolanic properties, suggesting suitabil-
ity for use in the manufacture of blended ce-
ments. Specifically, an amorphous ash with high
specific surface area and reduced loss on ignition
 can be produced with burning at these tempera-
tures.
(2) After 28 days, up to 117% of SAI can be
achieved when burning the POW at a tempera-
ture of 1000 C and 800C for 2 and 6 h, respec-
tively. This indicates the presence of the required
properties that characterize the pozzolanic mate-
rials. In addition, at all storage ages, the SAI of
POWA mortars was higher than that of OPC
mortars.
(3) POFA obtained by heating at 450C for 90 min
resulted in loss on ignition significantly lower
than that of the untreated POFA. Hence, the
treated POFA was free from carbon and other
organic matter. In addition, the treatment process
yielded POFA with high specific surface area,
preserving the amorphous characteristic related
to pozzolanic activity of POFA and free from
particle agglomeration.
(4) SAI of POFA-cement mortar fulfilled the re-
quirements of pozzolanic materials as per ASTM
C 618. SAI confirmed that after 28-day curing
time, the strength of treated POFA was greater
than that of the reference cement (100.7%).
Hence, strength increased as curing time pro-
gressed because of the consumption of Ca(OH)2
by the TGPOFA.
(5) At all storage ages, the SAI in the case of
GPOWA mortars were higher than that of
TGPOFA.
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ACKNOWLEDGMENT
The authors gratefully acknowledge the Universiti
Sains Malaysia for providing the financial support
through the Research University
(1001/PAWAM/814103) and Short-Term Grant
Schemes for undertaking the research work. Special
thanks are due to United Palm Oil Industries for
providing the materials.

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