Carbon 45 (2007) 330336

www.elsevier.com/locate/carbon

Adsorption of hydrogen sulphide (H2S) by activated carbons

derived from oil-palm shell
Jia Guo
a

a,*

, Ye Luo b, Aik Chong Lua c, Ru-an Chi a, Yan-lin Chen a,

Xiu-ting Bao a, Shou-xin Xiang a

Hubei Key Laboratory of Novel Reactor and Green Chemical Technology, School of Chemical and Pharmaceutical Engineering,
Wuhan Institute of Technology, Wuhan 430073, PR China
b
School of Physical Science, Wuhan Institute of Technology, Wuhan 430073, PR China
c
School of Mechanical and Aerospace Engineering, Nanyang Technological University, Singapore 639798, Singapore
Received 17 January 2006; accepted 14 September 2006
Available online 28 November 2006

Abstract
Adsorption of hydrogen sulphide (H2S) onto activated carbons derived from oil palm shell, an abundant solid waste from palm oil
processing mills, by thermal or chemical activation method was investigated in this paper. Dynamic adsorption in a xed bed conguration showed that the palm-shell activated carbons prepared by chemical activation (KOH or H2SO4 impregnation) performed better
than the palm-shell activated carbon by thermal activation and a coconut-shell-based commercial activated carbon. Static equilibrium
adsorption studies conrmed this experimental result. An intra-particle Knudsen diusion model based on a Freundlich isotherm was
developed for predicting the amount of H2S adsorbed. Desorption tests at the same temperature as adsorption (298 K) and at an elevated
temperature (473 K) were carried out to conrm the occurrence of chemisorption and oxidation of H2S on the activated carbon. Surface
chemistries of the palm-shell activated carbons were characterized by Fourier transform infrared spectroscopy and Boehm titration. It
was found that uptaking H2S onto the palm-shell activated carbons was due to dierent mechanisms, e.g. physisorption, chemisorption
and/or H2S oxidation, depending on the activation agent and activation method.
 2006 Elsevier Ltd. All rights reserved.

1. Introduction
Hydrogen sulphide (H2S), a rotten-egg smell gas produced by anaerobic digestion in acid condition from
organic and inorganic compounds containing sulphur, presents dual problems of its toxicity and foul odour. H2S can
be detected by most people as low as 0.0047 ppm [1].
Although no signicant physical harm may be caused in
such a low concentration, the exposure to this nuisance
can lead to nausea, loss of appetite, and other negative
eects. From the point of view of engineering design of a
purication system, the odour threshold of H2S is

Corresponding author. Tel.: +86 27 87194980; fax: +86 27 87194465.

E-mail address: guojia@mail.wit.edu.cn (J. Guo).

0008-6223/$ - see front matter  2006 Elsevier Ltd. All rights reserved.
doi:10.1016/j.carbon.2006.09.016

0.18 ppm [2]. Various measures can be applied to reduce

or eliminate H2S emissions from dierent sources, particularly sewage treatment facilities. Among these measures,
the use of activated carbon is most successful and widespread due to its safety and eectiveness of the operation
process [3]. Usually, activated carbons used for H2S
adsorption are those activated carbons modied with caustic chemicals such as KOH and NaOH [4] or oxidative
agents KI and KMnO4 [5] which promote oxidation of
H2S to elemental sulphur. All of these carbon modications, however, create the hazard of xed-bed self-ignition
owing to the high heat released by the reactions [6]. Moreover, the adsorptive capacity of the activated carbon may
be signicantly decreased by the modication process since
the micropores are not accessible due to the blockage of
pore entrances [7]. For these reasons the use of activated

J. Guo et al. / Carbon 45 (2007) 330336

331

Nomenclature
C
Dk
F
L
LMTZ
m
Ms
M1
r
R

gas-phase adsorbate concentration (mol m3)

Knudsen diusion coecient (m2 s1)
constant in Freundlich isotherm (dimensionless)
length of the xed bed (m)
length of the mass transfer zone (m)
constant in Freundlich isotherm (dimensionless)
mass of the adsorbate entered the particle (g)
mass adsorbed after innite time (g)
radial coordinate of the spherical particle of the
adsorbent (m)
radius of the adsorbent particle (m)

Greek letters
e
total porosity of the adsorbent (%)
s
time elapsed (s)

carbons prepared by chemical activation, particularly from

carbon-enriched lignocellulosic precursors, as H2S adsorbents would be benecial for environment as well as for
municipal facilities.
In present work, dynamic and static adsorption of H2S
on oil-palm-shell activated carbons by dierent activation
methods as well as on a coconut-shell-based commercial
activated carbon was studied. Oil-palm shell (also called
endocarp) is a cheap and abundant agricultural solid waste
in tropical countries such as Malaysia and Thailand. Palm
shells have been successfully converted into well-developed
activated carbons used for removal of various gaseous pollutants [8,9]. However, there are few publications in the scientic literature that report on the preparation of activated
carbon from palm shell impregnated with KOH and H2SO4
and even far fewer on use of such adsorbents for H2S
removal. The objective of the study is to reveal the reaction
mechanisms (e.g. physisorption, chemisorption and/or H2S
oxidation) between H2S and the palm-shell activated carbons prepared by various activation methods.

2. Experimental
2.1. Adsorbent preparation
Palm shells from a palm-oil mill in Selangor, Malaysia were dried,
crushed and sieved to a particle size fraction of 1.02.0 mm. 10 g of this
processed starting material was impregnated with 200 ml of H2SO4
(40%) or KOH (30%) at room temperature (298 K) for 24 hours and then
dried at 383 K overnight. The mixture was activated in a stainless-steel
reactor (550 mm length and 38 mm i.d.) under a stream of nitrogen (N2)
gas owing at 150 cm3/min. The reactor was heated in a vertical tube furnace (818 P, Lenton) from room temperature to a pre-set temperature
(973 K) for 2 h. After cooling to room temperature, the resulting products
were taken out and leached with distilled water. In another comparative
study, the preparation of activated carbons by thermal activation with carbon dioxide (CO2) gas (100 cm3/min) at 1173 K for 2 h was carried out. A
coconut-shell-based commercial activated carbon by steam (H2O) activa-

s0.05

s0.95

breakthrough time, dened as the time when the

outlet concentration at 5% of the inlet concentration (s)
exhaustion time, dened as the time when the
outlet concentration at 95% of the inlet concentration (s)
tortuosity factor related to the path of the molecule (dimensionless)

Subscripts
e
eective value of corresponding diusivity
i
serial number
0
initial state

tion (CAC, Damao Chemicals and Chemical Apparatus, Tanjin) was also
used for testing. The physical properties of the palm-shell and coconutshell activated carbons are given in Table 1.

2.2. Characterizations
Proximate analysis and ultimate analysis were carried out by a thermogravimetric analyzer (TGA-50, Shimadzu) and an elemental analyzer
(CHN-932, LECO) respectively. Textural characteristics of samples were
determined by N2 adsorption at 77 K with an accelerated surface area
and porosimeter (ASAP-2000, Micromeritics). The specic surface area
was calculated from the isotherms by the Brunauer-Emmett-Teller
(BET) equation [10]. The DubininRadushkevich (DR) equation was used
to calculate the micropore volume from the N2 adsorption data [11].

2.3. Chemical characterization

Boehm titration with sodium hydroxide, sodium carbonate, sodium
bicarbonate, and sodium methoxide solutions was carried out to determine the oxygenated surface functional groups under the assumption that
NaOH neutralizes carboxyl, phenolic and lactonic groups; Na2CO3 neutralizes carboxyl and lactonic; and NaHCO3 only carboxyl groups. For
general surface functional groups, the samples were studied by a Fourier
transform infrared spectrometer (FTIR-2000, Perkin Elmer). The spectra
were recorded from 4000 to 400 cm1. By comparing to the standard frequency patterns, various characteristic chemical bonds (or stretchings)
were determined, from which certain surface functional groups could be
derived. X-ray photoelectron spectroscopy (MK-II, Vacuum Generator)
was used to examine the change of surface chemistry. It was measured
using Mg Ka radiation generated at 12.5 kV and 250 W. The 1 s core-level
scan spectra were taken for the surfaces of the activated carbon before and
after adsorption process.

2.4. Adsorption and desorption of H2S

Dynamic adsorption of H2S was conducted in a copper column
(10.0 mm i.d. and 20 cm long) lled with pre-dried activated carbons,
which were retained on a metal mesh at the bottom of the column. The
column was operated in the up-ow mode. H2S adsorbate of 2000 ppm
(balanced by pure He gas) from a gas cylinder was introduced to the inlet
of the adsorption column at a certain volumetric ow rate (90 cm3/min).
The ow rate was controlled by a rotameter (MVIP804, MDA Scientic),
which was calibrated carefully with the soaplm burette method [12]. All

332

J. Guo et al. / Carbon 45 (2007) 330336

Table 1
Physical properties of the coconut shell and palm shell activated carbons
Sample

Nitrogen adsorption
Porosity (%)
BET surface area (m2/g)
Micropore volume (cm3/g)
Proximate analysis (wt.%)
Volatile matter
Fixed carbon
Ash
Ultimate analysis (wt.%)
Carbon
Hydrogen
Nitrogen
Oxygen (by dierence)

Palm shell activated

carbon by CO2
activation

Coconut shell activated

carbon by H2O
activation

Palm shell activated

carbon by KOH
activation

Palm shell activated

carbon by H2SO4
activation

58.4
1062
0.26

67.4
1183
0.35

56.3
1148
0.25

59.5
1014
0.28

6.4
86.1
7.5

4.5
91.9
3.6

10.6
83.0
6.4

14.2
82.0
3.8

87.1
1.0
1.1
10.8

87.5
0.9
2.0
9.6

84.1
0.8
0.6
14.5

83.3
0.4
0.2
16.1

the runs were carried out at the laboratory temperature of 298 K and an
ambient pressure of 1.0 bar. The time-dependent concentration at the
exit of the column was continually monitored by a ame photometric
detector (FPD, Fisher-Rosemount). The column was operated until saturation, that is, when the outlet concentration became equal to that of the
inlet.
Static adsorption of H2S was also carried out in the TGA. H2S
(1000 ppm, balanced by He) was introduced into the analyzer chamber,
where a platinum pan with about 20 mg of adsorbent was suspended.
At room temperature of 298 K, the subsequent sample weight gain due
to the amount of gas adsorbed onto the adsorbent was recorded. After
adsorption, desorption tests using He gas ushing through the analyzer
chamber at the same temperature of adsorption and a higher temperature
of 473 K were carried out to verify the occurrence of chemisorption and/or
oxidation of H2S.

3. Results and discussion

H2S breakthrough curves for activated carbons prepared from coconut-shell by steam activation and palmshell by dierent activation methods are shown in Fig. 1.
In a xed bed for adsorption, the part that displays a gra-

Normalized concentration C/C0

1.0

0.8

LMTZ

Ls0:95  s0:05
s0:95 s0:05 =2

Table 2 shows the breakthrough-curve characteristic

parameters for the coconut-shell and palm-shell activated
carbons. Compared to the palm-shell activated carbon by
thermal activation and coconut-shell activated carbon,
the activated carbons prepared by KOH and H2SO4 activation had better dynamic adsorption performances due to
longer breakthrough times, prolonged exhaustion times,
and relatively short MTZs. Therefore, the corresponding
adsorption capacities were also larger [14,15]. This suggests
that the palm-shell activated carbons prepared by chemical
activation are more capable of H2S adsorption.
In the gas-phase adsorption model, the basic assumptions are as follows:

Palm shell: CO2 activation

Coconut shell: H2O activation
Palm shell: KOH activation
Palm shell: H2SO4 activation

0.6

0.4

0.2

0.0
200

dient in adsorbate concentration from zero to equilibrium

is called the mass transfer zone (MTZ). This is the active
part of the bed where adsorption actually takes place. As
the saturated part of the bed increases, the MTZ travels
downstream and eventually exits the bed. The length of
the MTZ (LMTZ) may be estimated as follow [13]:

240

280

320

360

400

Time (min)
Fig. 1. Breakthrough curves for activated carbons prepared from coconut
shell by steam activation and palm shell by dierent activation methods.

1. The activated carbon particles are perfect spheres; diusion taking place along the radial direction (r) on the
adsorption sites that are uniformly distributed within
the particles.
2. External mass convective ux is negligible in comparison to transport by Knudsen diusion. Therefore, the
external adsorbate concentration can be considered to
be uniform (C0).
3. The adsorbent is isothermal (temperature constant) during the adsorption process.
4. Adsorption at the pore mouth follows a Freundlich
equilibrium isotherm.
5. The porosity e and the tortuosity factor n of the particle
are regarded as constant during the adsorption process.
6. No chemical reactions occur at the adsorbent surface.

J. Guo et al. / Carbon 45 (2007) 330336

333

Table 2
Breakthrough-curve characteristic parameters for the coconut shell and palm shell activated carbons
Activated carbon

Breakthrough time s0.05

(min)

Exhaustion time
s0.95(min)

Length of MTZ LMTZ (cm)

Adsorption capacity
(mg/g)

Palm shell: CO2 activation

Coconut shell: H2O
activation
Palm shell KOH activation
Palm shell: H2SO4 activation

245.6
270.7

316.1
359.4

5.0
5.6

46
53

291.5
304.3

323.8
334.0

2.1
1.9

68
76

The rst and second terms represent accumulation of

adsorbate molecules in gaseous and solid phases within
the adsorbent particle respectively, while the term on the
right-hand side represents Knudsen diusion of adsorbate
molecules in the gas phase within the particle. In adsorption of gas pollutant by activated carbon, the adsorbed
phase is strongly favoured and so the rst term in Eq. (2)
can be neglected without loss of accuracy.
The initial condition is
C0

at s 0

for 0 < r < R

The boundary conditions are

oC
0 at r 0 for all s
or
C C 0 at r r0 for s > 0

3a

120

80
Model prediction
Coconut shell: H2O activation

40

Palm shell: CO2 activation

10

20

30

40

50

60

Time (min)

3b
3c

Combining Eqs. (2) and (4), the following equation can be

obtained:
oC
eDke
o2 C

C 1m 2
os 1  eFm
or

160

Fig. 2. Experimental results and model predictions of amount H2S

adsorbed onto coconut shell and palm shell activated carbons.

If the equilibrium isotherm follows Freundlich type, the

relationship between Cl and C can be expressed by the following equation:
C l FC m

200

Amount of H2S adsorbed (mg/g)

Based on these assumptions, the intra-particle mass

transfer can be described by the following equation [16]:


oC
oC l
e o
oC
1  e
Dke r2
2
e
2
os
r or
or
os

eDke
C 1m can be regarded as a concentraThe coecient 1e
Fm
tion-dependent diusion coecient, which links the degree
of asymmetry in the rates of adsorption to the Freundlich
isotherm constant m.
The mass of the adsorbate that has entered the particle,
Ms, can be found by integrating the adsorbate adsorbed
over the entire adsorbent particle, i.e.
Z R
M s 3M 1
r2 C m r; sdr
6
0

However, an analytical solution for Eq. (5) is not available

and a numerical method has to be employed. The non-linear partial dierential Eq. (5) was converted into a set of
time-dependent, non-linear, ordinary dierential equations
using orthogonal collocation [17].
Fig. 2 shows experimental results and model predictions
of amount H2S adsorbed onto the coconut-shell and palm-

shell activated carbons. The Freundlich constants were

obtained from experimental data under dierent adsorption temperatures by curve tting. In this study, the Freundlich constants F of 1.19 103 and m of 0.84 were
used. It could be seen that the predicted results by diusion
model based on Freundlich isotherm agreed with the experimental data very well. One minor disadvantage of this
model is the need for a numerical solution, which is more
time-consuming than the analytical integration procedure
for linear isotherm model.
Experimental results and model predictions of amount
H2S adsorbed on the palm-shell activated carbons prepared
by chemical activation are shown in Fig. 3. For both KOH
and H2SO4 used as activation agent, the diusion model
based on Freundlich isotherm always under-estimated the
amount of H2S adsorbed. The possible reason was that this
model did not take into account chemical reactions (e.g.
chemisorption or H2S oxidation), which are related to the
samples surface chemistry.
The results of desorption at room temperature and
473 K are shown in Table 3. For the activated carbons prepared by physical activation, all (100%) H2S adsorbed
could be desorbed at room temperature, indicating a pure
physisorption process involved. However, besides large
part of H2S that was weakly bonded to the chemically activated carbons and easily desorbed at room temperature,
some H2S required a higher temperature (473 K) for
desorption, suggesting that chemisorption occurred. For

334

J. Guo et al. / Carbon 45 (2007) 330336

200

10

20

30

40

50

60

Time (min)
Fig. 3. Experimental results and model predictions of amount H2S
adsorbed on palm shell activated carbons prepared by chemical activation.

4000

3400

2800

2200

659

754

1251
1204

1507
1502
1504

CO2 activation

2439

Palm shell: KOH activation

1723

Palm shell: H2SO4 activation

50

1627

Model prediction

1613

100

H2SO4 activation

3415

150

1745

KOH activation

Transmittance (arbitrary units)

Amount of H2S adsorbed (mg/g)

250

1600

1000

400

Wave Number (cm-1)

the activated carbon prepared by H2SO4 activation, even

after heated up to 473 K, there were still some residual
weights on the carbon surface, suggesting that some irreversible chemical reactions occurred and indecomposable
products attached to the sample.
In order to further investigate their surface chemistries,
FTIR spectra of activated carbons prepared from palm
shell by dierent activation methods were measured and
the results are shown in Fig. 4. The spectrum of the activated carbon prepared by 30% KOH impregnation displayed the following bands: 1754 cm1, C@O stretch in
ketones; 1507 cm1, C@C stretch in aromatic rings;
1251 cm1, CO stretches; and 754 cm1, CH out-ofplane bending in benzene derivatives. The main surface
functional groups present on the KOH-impregnated adsorbent are presumed to be alkaline groups of pyrones (cyclic
ketone) and other keto-derivatives of pyran. In addition,
the alkaline chromenes groups might also be present as
proposed by Jankowska [18]. Therefore, the surface of
the oil-palm-shell adsorbent with KOH impregnation is
given below.

Fig. 4. FTIR spectra of activated carbons prepared from palm shell by

dierent activation methods.

These surface functional groups account for the chemisorption of H2S gas.
The spectra of the activated carbon prepared by 40%
H2SO4 impregnation in Fig. 4 displayed the following
bands: 3415 cm1: HO stretching in hydroxyl groups;
1723 cm1: C@O stretching in carboxylic acids or isolated
carbonyl groups; 1627 cm1: C@O stretching in quinones
or carboxylic anhydrides; 1502 cm1: C@C stretching in
aromatic rings, and 1204 cm1: COC stretching in ethers
or ether bridges between rings.
The oxygen functional groups are likely to be phenols,
carboxylic acids (or carboxylic anhydrides if they are close
together) and carbonyl groups (either isolated or arranged
in quinone-like fashion), all of which are typical acidic functional groups [19]. The surface structure of the H2SO4impregnated palm-shell activated carbons is given below.
O O

O
O

O
C
H

HO

H
R

O
C

O
C

HO

O
O

O
O

Table 3
Desorption properties of the coconut shell and palm shell activated carbons
Activated carbon

Total amount
adsorbed (mg/g)

Percentage of
desorption at 298 K (%)

Percentage of
desorption at 473 K (%)

Percentage of
residue (%)

Palm shell: CO2

activation
Coconut shell: H2O
activation
Palm shell KOH
activation
Palm shell: H2SO4
activation

131

100

162

100

169

79

21

203

83

10

J. Guo et al. / Carbon 45 (2007) 330336

335

For the activated carbon prepared by CO2 thermal activation, the band at 2439 cm1 is attributed to CH stretching vibrations in aliphatic structures, in addition to phenols
and the aromatic rings. In this case, the surface structure of
the thermally activated carbon is given below:
H
H

HO

This agreed with the results of Boehm titration as shown

in Table 4. For thermally activated carbons, only phenol
and carbonyl groups were detected, whilst lactonic and carbonyl groups were found on the surface of the activated
carbon prepared by KOH impregnation. On the surface
of the activated carbon prepared by H2SO4 impregnation,
carboxyl, phenol, lactonic and carbonyl groups were
detected.
During chemical activation with H2SO4 for palm shells,
the formation of oxygen functional groups can be represented as follows:
Cn Hx Oy  H2 SO4 ! H2 O Selement Cn Hx Oy3 

During H2S adsorption, besides physisorption onto the

pore surface due to van de Waals forces, chemisorption
by forming hydrogen bonding also occurred such that
Cn Hx Oy3  H2 S ! Cn Hx Oy3    H2 S

Hydrogen atoms in H2S could strongly interact with oxygen in form of hydroxyl (HO) and carbonyl (C@O)
groups due to the high electrostatic attraction. H2S can
therefore preferably adsorb onto active adsorption sites
provided by oxygen functional groups via hydrogen bonds
besides on pure carbon sites. Other researchers also conrmed the formation of hydrogen bonds during chemisorption [2022]. In addition, due to the oxygen functional
groups, H2S was easily oxidised as follows:
Cn Hx Oy3  H2 S ! Cn Hx Oy2  Selement H2 O

This may explain why, for the activated carbon prepared

by H2SO4 activation, there were still some residual weights
on the carbon surface when desorption was carried out at
up to 473 K. Some irreversible chemical reactions (H2S oxidization) occurred and indecomposable products (elemental sulphur) attached to the sample. The XPS spectra of
the activated carbon surfaces before and after H2S adsorption processes were shown in Fig. 5. [23,24]

Table 4
Number of surface groups (meq/g) obtained from Boehm titration
Activated carbon

Carboxyl

Lactone

Phenol

Carbonyl

Palm shell: CO2 activation

Palm shell KOH activation
Palm shell: H2SO4 activation

0.089

0.355
0.416

0.120

0.208

0.285
1.167
0.604

Fig. 5. XPS spectra of the activated carbon surfaces before and after H2S
adsorption processes.

4. Conclusions
From the adsorption of H2S onto the activated carbons
prepared from oil-palm shells with and without preimpregnation, the following conclusions can be drawn:
(1) Compared to the palm-shell activated carbon by thermal activation and coconut-shell activated carbon, the
activated carbons prepared by KOH and H2SO4 activation had better dynamic adsorption performances
due to longer breakthrough times, prolonged exhaustion times, and relatively short MTZs. Therefore, the
corresponding adsorption capacities were also larger.
(2) The Freundlich constants were obtained from experimental data under dierent adsorption temperatures
by curve tting. In this study, the Freundlich constants F of 1.19 103 and m of 0.84 were used. It
could be seen that the predicted result by diusion
model based on Freundlich isotherm agreed with
the experimental data very well.
(3) For both KOH and H2SO4 used as activation agent,
the diusion model based on Freundlich isotherm
always under-estimated the amount of H2S adsorbed.
The possible reason was that this model did not take
into account chemical reactions (e.g. chemisorption
or H2S oxidation), which are related to the samples
surface chemistry.
(4) The main surface functional groups present on the
KOH-impregnated adsorbent are presumed to be
alkaline groups of pyrones (cyclic ketone) and other
keto-derivatives of pyran. The oxygen functional
groups on the H2SO4-impregnated sample are likely
to be phenols, carboxylic acids (or carboxylic anhydrides if they are close together) and carbonyl groups
(either isolated or arranged in quinone-like fashion),
all of which are typical acidic functional groups.

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J. Guo et al. / Carbon 45 (2007) 330336

(5) Besides physisorption, some H2S adsorbed by the

H2SO4-impregnated sample required a higher temperature for desorption, suggesting that chemisorption via hydrogen bonding occurred. There were
still some residual weights on the carbon surface
when desorption was carried out at up to 473 K since
H2S oxidization resulted in indecomposable products
of elemental sulphur attached to the sample.
Acknowledgements
The author (Dr. J. Guo) appreciates the nancial support from the Program for New Century Excellent Talents
in University (Contract No. NCET-05-0681) and the Scientic Research Foundation for the Returned Overseas
Chinese Scholars (Contract No. 2005-383), Ministry of
Education, PR China.
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