J. Anal. Appl.

Pyrolysis 82 (2008) 205–211

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Journal of Analytical and Applied Pyrolysis

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Oil spill sorption using carbonized pith bagasse

1. Preparation and characterization of carbonized pith bagasse
M. Hussein a, A.A. Amer b,*, I.I. Sawsan a
a
Alexandria University, Faculty of Engineering, Chemical Department, Alexandria, Egypt
b
Alexandria Petroleum Company, Alexandria, Egypt

A R T I C L E I N F O A B S T R A C T

Article history: Treatment of oil spills remains a challenge to environmental scientists and technologists. Among all the
Received 30 August 2007 existing techniques used for oil treatment, sorption is a popular technique because it is cheap, simple and
Accepted 10 March 2008 effective. Among the various sorbents used pith bagasse appears to be the most attractive material in
Available online 22 March 2008
terms of cost, versatility and abundance. In the present work, the efficiency of surface modification of pith
bagasse by carbonization is demonstrated. Pith bagasse was carbonized in a stainless steel tube for
Keywords:
different temperatures ranging from 200 to 600 8C and for different heating periods from 1 to 3 h. The
Pith bagasse
carbonized pith bagasse was tested using gas oil; 1- and 7-day weathered heavy Arabian crude oil. It was
Hydrophobicity
Oleophilicity
found that carbonization of pith bagasse improves the oleophilic and hydrophobic properties. The best
Carbonization carbonization conditions were established at 300 8C for 2 h.
Oil spill ß 2008 Elsevier B.V. All rights reserved.
Sorbent

1. Introduction on a simple energy basis; however, from a comprehensively

Bagasse is the residue fiber remaining when sugar cane is
pressed to extract the sugar. Some bagasse is burned to supply heat
to the sugar refining operation. Some are returned to the fields, and
some finds it way into various board products. Bagasse is
composed of fiber and pith. The fiber is thick walled and relatively
long (1–4 mm) [1]. According to Paturau [2] most of sucrose
together with bundles of small fibers is found in the inner pith. The
outer rind contains longer and finer fibers, in a random
arrangement throughout the stem and bound together by lignin
and hemicellulose.
The oil adsorption properties of untreated and treated pith
bagasse are an interesting research subject in an industrial and
environmental context. Pith bagasse is biodegradable and recy-
cling bagasse that is treated as agricultural waste, for example as a
material used in the cleanup of oil spills, would provide both
economic and environmental benefits. It is expected that
carbonization rather than combustion both imparts and enhances
the oil adsorption capacity of pith bagasse.
More energies are consumed in the carbonization of pith
bagasse requiring a heated oven and inert conditions than
incineration. The carbonization process is by no means economical
* Corresponding author. Tel.: +20 1224 93520/002033571885.
E-mail address: amer_abdelrazik@yahoo.com (A.A. Amer).
environmental viewpoint, carbonization that transfers pith
bagasse into an oil adsorbent can provide both economic and
social benefits.
Activated carbon is one of the most important types of
adsorbents widely used as a tool in environmental protection in
various industrial applications. Each application requires activated
carbon of specific characteristics such as surface area, pore size and
pores distribution and adsorption characteristics [3]. Usually the
production of activated carbons involves two stages; the carbo-
nization of the raw materials followed by high temperature
activation, at 800–1000 8C, of the resulting chars [4]. The
carbonization of any carbonaceous material in absence of air
involves decomposition of organic molecules, evolution of tarry
and gaseous products, and finally in a solid porous carbon mass.
The selection of a suitable activated carbon is an integral part of the
design of a carbon treatment plant. A primary characterization of
the product before its application in adsorption process shows the
primary sign of versatility in a convinced manner. The adsorptive
properties of any activated carbon is highly dependent on active
surface sites incorporating functional groups, specific surface area,
particle size, pore volume, pretreatment if any, etc. These factors
have remarkable effects on the adsorption capacity and, hence play
important role in examining the suitability of the adsorbent for a
system [3].
The properties of activated carbons are determined to a large
extent by nature of precursor and carbonization conditions [3,5].

0165-2370/$ – see front matter ß 2008 Elsevier B.V. All rights reserved.
doi:10.1016/j.jaap.2008.03.010
206 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211

In the present study, the oil adsorption capacity, the physical

properties of carbonized pith bagasse are examined. The
water adsorption properties of the carbonized pith bagasse
were also examined to explore their practical applications in
treating oil spills within water. A procedure is described that
enhances the oil adsorption capacity of pith bagasse. The
dominant mechanism of oil adsorption by the bagasse is then
discussed.

2. Experimental methods

2.1. Materials

2.1.1. Sorbent material

The pith bagasse used in this study was a waste produced from
sugar industry. Its moisture content was found to be about 40%.
The fresh bagasse was thoroughly washed with water to remove
soil and other foreign materials. The big part of pith was separated
from the tough (hard walled) dried for 7 days under sunlight, dried
at 105 8C for 2 h, crushed in a Willey mill and sieved. The particle
size fraction between 1 and 0.8 mm was selected and then
subjected to a carbonization process.

2.1.1.1.Characterization of pith bagasse. Scanning electronic micro-

scope model (SEM JEOL JSM 6360 LA made by JEOL, Japan) was
used to study the fiber surface morphology. Before examination,
the fiber samples were sputtered coated with a thin layer of gold in
a vacuum chamber.
Thermo gravimetric analyzer: used for determining thermal
stability of bagasse (TGA-50 Shimadzu) Japan.
The range of temperature used was between 0 and 600 8C with a
temperature increase rate of 5 8C/min. A TGA thermo balance was Fig. 1. Procedure for preparing carbonized pith bagasse.
used and the size of the sample was around 7 mg.

2.1.2. Tested oils
Different kinds of oil to represent a wide variety were tested in
the application of sorbents. Gas oil has a specific gravity of 0.82 at
T = 15 8C a flash point of 55 8C obtained from benzene station; and
heavy Arabian crude oil which has kinematics viscosity of 11.2 cSt
at 40 8C and a specific gravity of 0.8825 at (60/60) was obtained
from Medore Refining Company. The gas oil was used without
modification.
In early stages of an oil spill lighter hydrocarbons do evaporate
and consequently the oil viscosity increase before any possible
cleanup operation can take place [14]. So to simulate this situation
of oil spill and to minimize experimental variation, crude oil
samples were put on a tray where oil formed a layer of a 5-mm
thick and was situated in open air for 1 and 7 days [6].
Three types of oils namely, gas oil, 1- and 7-day weathered
heavy Arabian crude oil, were employed to investigate the oil
sorption characteristics of pith bagasse. Gas oil represents low
viscosity (74.6118 cSt at 25 8C) oils such as light crude oil, kerosene
and gasoline. One day weathered heavy Arabian crude oil is a good
surrogate for oils with intermediate viscosity (181.360 cSt at 25 8C)
such as heavy crude oil and vegetable oils. Seven day weathered
heavy Arabian crude oil represents highly viscous oils (512.79 cSt
at 25 8C) such as lubricating oils. These oils were investigated in
favor of the crude oils or lightweight hydrocarbon oils because they
were less volatile and had better compositional uniformity, which
minimized the transient change in their chemical and physical
characteristics during experiments.
2.2. Sample preparation
Fig. 1 represents the procedure for making carbonized pith
bagasse. The samples were in a closed carbonized stainless steel
tube (with a length of 12.5 cm, inner diameter of 2.5 cm and a small
hole at the top for the ventilation of the gases produced during
carbonization) and heated in a muffle furnace.
The tubes were heated to 200, 300, 400, 500 and 600 8C and
maintained at the selected temperature for different periods of
time (1, 2 and 3 h). The tubes were then left to cool at the furnace to
ambient temperature. The collected carbonized solid product was
tested for the influence of the carbonization conditions (tempera-
ture and period of carbonization) on the product characteristics
(oleophilic and hydrophobic properties).
2.3. Methodologies of oil sorption experiments
The tests used in this study to determine the sorption capacity
and the sorption characteristics were done according to:
 The American Society for Testing Materials ASTM standards [7].
Absorbency expressed in weight of oil adsorbed per unit weight
of sorbent.
 Environmental Canada Protection Services EPS manufacture
standard sorption capacity [15], which is also a measure of the oil
sorbed per unit weight of sorbent.
2.3.1. Sorption capacity determination for pure oil (oil only) under
static condition
This test gives ideal size laboratory method which compares
one absorbent’s oil capacity with another. The objective of this test
is to determine the optimum sorbent capacity without the
competing presence of water. The test is done as follows according
to ASTM [7].
One gram of sorbent was placed in a 1-l beaker filled with a
layer of 7.5 mm of oil sample where a net was lowered at the
 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211 207

Fig. 2. Scanning electron micrographs of the longitudinal and cross-section of pith bagasse before carbonization.

bottom before adding the oil. After 15 min the sorbent was
removed with the net and let to drain over the cell for 5 min where
a clean empty weighted watch glass was placed under the sorbent
sample to catch any additional drips and immediately the
saturated oil sorbent was transferred to the watch glass. The
sample weight was determined and the oil sorption capacity was
calculated. The quantity of oil sorbed by the sorbent was
determined by subtracting the initial sorbent weight from the
total weight of saturated sorbent.
test cell. After 15 min the sorbent with the net was removed from
the beaker and let to drain over the beaker for 5 min. The net was
placed over a clean empty weighted watch glass to catch any
additional drips and immediately the saturated oil sorbent was
transferred to the watch glass and the weight was recorded [8].
3. Results and discussions
3.1. Electro scanning of pith bagasse

2.3.2. Static water test Pith bagasse is a three-dimensional, biopolymer composite

This procedure was designed to test for water pickup under
stagnant condition (hydrophobic characteristic). The test was
performed at room temperature (22–25 8C).
The test cell (1 l glass beaker) was filled with a layer of 80 mm
water of salt water containing 3.5% by weight NaCl. One gram of
the sorbent sample was placed in a net which is lowered into the
anisotropic, amorphous, porous, has a high aspect ratio (length/
width) and a rough surface. The fiber structure is hollow tubular
structure (or lumen) with external diameter of 111.764 mm,
internal diameter of 88.23 mm, and length of 220 mm, laminated,
randomly oriented, with molecular layers and an integrated matrix
as seen from the electronic scanning microscope in Fig. 2A and B.

Fig. 3. Thermal gravimetric analysis of the bagasse sample.

208 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211

The figure also shows the roughness of the surface and the
projections which enhance the adsorption properties of pith
bagasse; also they show the anisotropic structure of pith bagasse,
the amorphous orientation of the fibbers, and the big fiber lumen
that enhance the capillary action and the diffusion of oil through
the cuticle to the inner fibers; finally, they show the hollow tubular
structure (or lumen) which enhance the absorption properties of
pith bagasse.

3.2. Studying the thermal gravimetric analysis of pith bagasse

The thermal gravimetric analysis of the bagasse sample is Fig. 5. Effect of carbonization temperature on the % yield of carbonized pith bagasse
shown in Fig. 3. The fiber mass decreased from about 97.242% (at at t = 1.5 h.
100 8C) to 51.939% (at 250 8C) and to 28.153% (at 350 8C). Different
regions can be associated with the loss of retained water at 100 8C, Table 1
hemicellulose degradation in the 200–260 8C regions, cellulose Sieve analysis
degradation at 240–350 8C and lignin degradation at 280–500 8C. Particle size (mm) Carbonization temperature (8C)
Between 100 and 250 8C, degradation turns the lignocellulosic
200 300 400 500
fiber into a brownish color material, losing its strength, although
this was not quantified. At higher temperatures, up to 500 8C, Mass fraction
carbonization occurs with accentuated loss of material. 0.8 0.392 0.356 0.218 0.261
0.63 0.435 0.353 0.400 0.351
Being one of the oldest thermal analytical procedures used for
0.4 0.117 0.158 0.164 0.156
the study of polymeric systems, the thermogravimetry analysis is a 0.315 0.036 0.088 0.131 0.054
technique of evaluating the thermal decomposition kinetics of 0.2 0.015 0.032 0.048 0.091
materials by monitoring the weight loss of the sample in a chosen 0.1 0.005 0.013 0.039 0.087
atmosphere (usually nitrogen or air) as a function of temperature
[9]. Not all thermal events result in a change of the sample mass:
melting, crystallization, and glass transition do not exhibit a mass sorption capacity decreases with increasing the carbonization
change; whereas desorption, absorption, sublimation, vaporiza- temperature.
tion, oxidation, reduction and decomposition do. TGA is best By further increasing in the carbonization temperature the
known for its ability to provide information on the bulk sorption capacity decreases except for a temperature of carboniza-
composition of compounds. The usefulness of TGA for analyzing tion of 500 8C.
complex systems is greatly enhanced by the ability to record Fig. 5 shows the influences of temperature of carbonization on
simultaneously the first derivative of the weight loss, that is, the the yield. The figure shows that as the carbonization temperature
derivative of the thermo gravimetric curve. increases the yield decreases till it reaches a minimum value of
(34%) at 600 8C at 1.5 h due to intensified gasification.
3.3. Study the sorption capacity of carbonized pith bagasse
At higher temperature over 300 8C the substances which stays
deeply in particle has the chance to disintegrate and explode by
1. The effect of carbonization temperature.
increasing the carbonization temperature the particle size
2. The effect of carbonization time and temperature.
decreases as shown in Table 1. Table 2 shows the distribution of
bagasse products during the carbonization at different tempera-
3.3.1. Effect of carbonization temperature tures [10].
The effect of carbonization temperature of pith bagasse varied The variation of the sorption behavior of 1- and 7-day
from 200, 300, 400, 500 and 600 8C and heated at a constant time of weathered Arabian crude oil and gas oil is due to their viscosity.
1.5 h. Choi and Cloud [11] have studied the effect of oil viscosity on oil
Fig. 4 shows the influences of temperature of carbonization on sorption capacity. They suggested that the sorption capacity of the
oil sorption capacity of 1- and 7-day weathered heavy Arabian oil is inversely proportional to the oil viscosity and directly
crude oil, gas oil and water. The figure shows that the sorption proportional to the capillary radius. At the same time, the viscosity
capacity increases with increasing the carbonization temperature increases the adherence of oil onto the surface of the fiber and
until it reaches a maximum of 300 8C in the same time water within the capillary during drainage.

Fig. 4. Effect of carbonization temperature on sorption capacity of oil and water. Fig. 6. Effect of carbonization time on the sorption capacity of 1-day weathered oil.
 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211 209

Table 2
Distribution of bagasse products

Biomass Treatment conditions Yield of products Ash (wt.% mf) Moisture (wt.%)

T (8C) Time (h) Solid yield (wt.% maf) Liquid yield (wt.% maf) Gas yield (wt.% maf)

Bagasse 230 1 87.5 9.9 2.6 2.41 2.5

Bagasse 230 2 85 10 5 2.66 2.2
Bagasse 230 3 83.7 10.3 6 2.46 2
Bagasse 250 1 78.9 10.7 10.4 2.84 1.9
Bagasse 250 2 77.5 10.9 11.6 2.89 1.7
Bagasse 250 3 75.4 12.6 12 2.97 1.6
Bagasse 280 1 68.6 18.5 12.9 3.27 1.8
Bagasse 280 2 64.7 20.5 14.8 3.46 1.7
Bagasse 280 3 63.8 21 15.2 3.51 1

T: temperature, time: residence time; duration of the treatment at the final temperature, maf: moisture and ash free, mf: moisture free.

temperature increases the oil sorption capacity increases till it

Fig. 7. Effect of carbonization time on the sorption capacity of 7-day weathered oil.
These results agree with Kumagai et al. [12] the recorded
changes in composition show that the hydrogen content decreases
with increasing carbonization temperature, while variation in the
carbon content is minimal.
Also these results agree with Vitidsant et al. [4] increasing the
temperature of carbonization, decreases the % yield. This can be
attributed to remove light volatile matter first following by big
molecules with the increasing of the temperature or partial
combustion.
reaches a maximum value of 25.5 g oil/g fiber at 300 8C at 2 h.
However, further increases in the carbonization time lead to
decrease in the sorption capacity of the 7-day weathered Arabian
crude oil.
Fig. 8 shows the influences of time of carbonization on oil
sorption capacity of gas oil. As shown in the figure for gas oil as the
carbonization temperature increases the oil sorption capacity
increases till it reaches a maximum value of 23.86 g oil/g fiber at
300 8C at 2 h.
However, further increases in the carbonization temperature
lead to decreases in the sorption capacity of gas oil.
Fig. 9 shows the influences of time of carbonization on water
sorption capacity. As shown in the figure water pickup as the
carbonization temperature increases the water sorption capacity
decreases till it reaches a minimum value of 0.89 g water/g fiber at
200 8C at 3 h.
However, with further increases in the carbonization tempera-
ture lead to increase in the sorption capacity of water.
Fig. 10 shows the influences of time of carbonization on the
yield. As shown in the figure as the carbonization temperature time

3.3.2. Effect of carbonization time and temperature

Fig. 6 shows the influences of time of carbonization (1, 1.5, 2 and
3 h) on oil sorption capacity of 1-day weathered heavy Arabian
crude oil. As shown in the figure for 1-day weathered oil as the
carbonization time increases the oil sorption capacity increases till
it reaches a maximum value of (24.5 g oil/g fiber) at 300 8C at 2 h.
Further increases in the carbonization time leads to a drop in
sorption capacity.
Fig. 7 shows the influences of time of carbonization on oil
sorption capacity of 7-day weathered heavy Arabian crude oil. As
shown in the figure for 7-day weathered oil as the carbonization Fig. 9. Effect of carbonization time on the sorption capacity of water.

Fig. 8. Effect of carbonization time on the sorption capacity of gas oil. Fig. 10. Effect of carbonization time on the % yield of carbonized pith bagasse.
210 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211
Fig. 11. Effect of soaking time on raw and carbonized pith bagasse.
the yield decreases till it reaches a minimum value of 33.2% at
600 8C at 3 h.
The increase in oil sorption capacity may be due to some
volatile compounds which were in the inner part of particle could
evaporate more with time and surface area increased while
increasing carbonization time as it leads to deformation in fiber
structure, resulting in reduction in oil sorption capacity.
It is commonly recognized that the following mechanisms work
solely or in combination during fluid adsorption on fabrics as
reported by Kumagai et al. [12]:
1. Interaction with oleophilic compounds and/or functional groups
on the fiber surface.
2. Physical trapping on the fiber surface related to the fiber density,
fineness, and irregularity.
3. Capillary action via oil diffusion into pores on the fiber surface.
The viscosity of 7-day weathered oil is higher than that of 1-day
weathered oil which are 512.79 cSt at 25 8C and 181.360 cSt at
25 8C for 7-day weathered oil and 1-day weathered oil, respec-
tively. If capillary action had been dominant, the carbonized pith
bagasse would thus have adsorbed more 1-day weathered oil;
however, the carbonized pith bagasse adsorbed more 7-day
weathered oil than 1 day. The high viscosity of the oil reinforces
adhesion between the fibers within the carbonized pith bagasse
and the oil during the dripping of excess oil.
The results agree with Amer and Hussein [13]. The increase in
oil sorption may be due to some volatile compounds which in the
inner part of the particle could evaporate more with time and
surface area increases as seen in the electro scanning micrographs
after carbonization. However, increasing carbonization times leads
to deformation in fiber structure results in reduction oil sorption
capacity.
Fig. 12. Scanning electron micrographs of the longitudinal and cross-section of pith bagasse after carbonization.
It is clear from the above results that the best condition for
carbonization at which the carbonized pith bagasse showed its
maximum oil sorption capacity was at 300 8C for 2 h.
3.4. Hydrophobic characteristic
This procedure was designed to test water pickup and
the buoyancy behavior of sorbents in water for a period of
about 1 week. This also helped to simulate field conditions
where the sorbent may be left for several days before being
collected.
The hydrophobic properties of carbonized pith bagasse were
tested and compared with raw pith bagasse by determining the
water pickup.
Fig. 11 shows that raw pith bagasse have a great affinity for
water and picks it quickly when the fibers comes in contact with
water. The quantity of water pickup after 15 min is about 9.87 g
H2O. This increases with time of contact and reaches about 12.13 g
water/g fiber in 168 h (7 days). This shows that the hydrophobic
properties of pith bagasse must be improved. The poor hydro-
phobic properties of the pith bagasse are due to the presence of free
hydroxyl groups in the cellulose structure which have a strong
affinity for water. Comparing these results with the results of the
soaking time of carbonized pith bagasse, good improvement in the
hydrophobic properties can be noticed. The water pickup
decreases from 12.13 g water/g raw fiber to 0.62 g water/g
carbonized fiber in 168 h (7 days).
3.5. Electro scanning of carbonized pith bagasse
It was found from Fig. 12 that the porosity increased and the
carbonization enhance the production of carbonized material with
well-developed pore structure, high specific surface area, the
structure consists of a distorted three-dimensional array of
aromatic sheets and strips of primary hexagonal graphic crystal-
lites. This structure creates angular pores between the sheets of
molecular dimensions which cause many of the useful absorption
properties of activated carbon. So physical trapping on the fiber
surface as reported by Manocha [14] is related to fiber density,
fineness, and irregularity also pores on the fiber surface is
inescapable. The carbonized pith bagasse fiber has a hollow
tubular structure (or lumen).
In actual sense, the adsorption capacity of any activated carbon
depends not only on the available surface area, but also on the
surface morphology of the activated carbon. The crystalline
structure, fractures, surface edges, nature and distribution of
pores regulate the adsorption efficiency.
 M. Hussein et al. / J. Anal. Appl. Pyrolysis 82 (2008) 205–211
Nature of raw material and its method of activation are mostly
affecting the pores development and distribution. As indicated
from the electro scanning that the sorption capacity will increase
by the carbonization process.
4. Conclusions
The experiments carried out involved treatment of raw pith
bagasse by thermal carbonization, where their sorption capacity (g
oil/g fiber) and water pickup were examined and taken as a
measure to determine the potential of using bagasse in oil spill
treatment in sea water.
Sorption capacity and porosity of any activated carbon depends
largely on carbonization conditions, morphology and physical
state of precursor, i.e. pith bagasse.
Carbonization plays the major role in porosity development of
any type of raw material as proved from the results of SEM
micrographs and adsorption properties of carbonized pith bagasse.
The increasing in the oil sorption capacity as temperature increases
is attributed to the formation of many small pores in which oil is
sorbed as seen in the electro scanning micrographs.
Thermal carbonization of pith bagasse enhances the oil sorption
capacity of gas oil, 1- and 7-day weathered crude oil and the best
condition was established at 300 8C for 2 h where the % yield is
good and sorption capacity increased. In the selected conditions a
high surface area and a relatively high yield of activated carbon has
been obtained at 300 8C with an activation time of 2 h. Higher
temperature decreases the yield of activated carbon.
211
Thermal carbonization reduces the water pickup from 12.13 g
water/g fiber to 0.62 g water/g carbonized fiber.
In summary carbonization is a good treatment for pith bagasse
as it increases the sorption capacity of raw pith bagasse and
decreases its water pickup which enhances the use of pith bagasse
in oil spill cleanup as sorbent material.
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