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Surface modification of a granular

activated carbon by citric acid for
enhancement of copper adsorption

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DOI: 10.1016/S0008-6223(03)00197-0

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 Carbon 41 (2003) 19791986

Surface modification of a granular activated carbon by citric

acid for enhancement of copper adsorption
J. Paul Chen a , *, Shunnian Wu b , Kai-Hau Chong a
a
Department of Chemical and Environmental Engineering National University of Singapore, 10 Kent Ridge Crescent, Singapore
129791, Singapore
b
Institute of High Performance Computing, 1 Science Park Road, [01 -01, The Capricorn, Singapore 117528, Singapore
Received 19 February 2003; accepted 5 May 2003

Abstract

In this study, citric acid was used to modify a commercially available activated carbon to improve copper ion adsorption
from aqueous solutions. The carbon was modified with 1.0 M citric acid, followed by an optional step of reaction with 1.0 M
sodium hydroxide. It was found that the surface modification reduced the specific surface area by 34% and point of zero
charge (pH pzc ) of the carbon by 0.5 units. Equilibrium results showed that citric acid modification increased the adsorption
capacity to 14.92 mg Cu / g, which was 140% higher than the unmodified carbon. Higher initial solution pH resulted in
higher copper adsorption. The chemical surface modification adversely affected the copper adsorption rate. Adsorption
kinetic mechanisms were investigated with an intraparticle diffusion model. It was found that the modification did not
change both external diffusion and intraparticle diffusion.
2003 Elsevier Ltd. All rights reserved.

Keywords: A. Activated carbon; B. Chemical treatment, Surface treatment; C. Adsorption; D. Adsorption properties

1. Introduction carbon had much higher adsorption of cadmium, lead and

Surface modification of activated carbons is recognized
as an attractive approach for enhancement of heavy metal
removal. Different heavy metal ions have different af-
finities for different surface functional groups. It has been
reported that the affinities between heavy metals and
organic functional groups are different [1]. Modification
can be performed by adsorbing foreign organic compounds
on the surfaces of carbons. It is well known that activated
carbons are able to effectively adsorb organic compounds
in aqueous solutions. This chemical behaviour leads to
immobilization of organic compounds on the carbon
surface.
Surface modification has been studied recently. Ravin-
dran et al. [2] impregnated 8-hydroxyquinoline (oxine) on
an activated carbon. It was found that oxine-impregnated
*Corresponding author. Tel.: 165-6874-8092; fax: 165-
6779-1936.
E-mail address: checjp@nus.edu.sg (J.P. Chen).
zinc. Lakov et al. [3] modified activated carbons with
3-methyl-1-phenyl-pyrazolone-5 (HMPP). The copper ad-
sorption capacity was enhanced by 50% even though the
specific surface area of the carbon decreased by 80%.
More recently, Monser and Adhoum [4] reported that,
when tetrabutyl ammonium iodide (TBA) or sodium
diethyl dithiocarbamate (SDDC) were applied onto an
activated carbon, a substantial improvement in Cu, Zn and
Cr removal capacity was achieved.
It has been reported that citric acid has a higher binding
affinity to copper ions [5]. It is biodegradable and widely
used in the food and pharmaceutical industries. As a result,
it was selected for the modification of a commercially
available granular activated carbon in this study. The main
objective of this paper was to compare the adsorption
performance of citric acid-modified activated carbons with
the unmodified activated carbons. The copper adsorption
equilibrium and kinetics were determined. Langmuir and
Freundlich isotherm equations were employed to quantify
the adsorption equilibrium. The effect of solution pH on

0008-6223 / 03 / $ see front matter 2003 Elsevier Ltd. All rights reserved.
doi:10.1016 / S0008-6223(03)00197-0
1980 J.P. Chen et al. / Carbon 41 (2003) 19791986
copper ion adsorption behaviour was examined. An in-
traparticle diffusion model was used to investigate the
adsorption mechanisms.
2. Experimental
2.1. Materials
In this study, Fitrasorb 200 (Calgon, Pittsburgh, PA,
USA) was used. Copper chloride dihydrate from J.T. Baker
(Phillipsburg, USA), and sodium nitrate, lead nitrate,
sodium hydroxide, sodium acetate, acetic acid, hydrochlo-
ric acid, nitric acid and citric acid monohydrate from
Merck (Germany) were used. All chemicals were of
reagent grade. Solution pH was adjusted by 0.1 M HCl or
0.1 M NaOH. The citric acid has a chemical formula of
HOOCCH 2 COH(COOH)CH 2 COOH, indicating that
it is a small organic compound rich in carboxylic groups.
The concentration of metal ions was measured using
inductively coupled plasma emission spectroscopy (ICP-
ES) (Perkin-Elmer Optima 3000, USA). Samples were
acidified with concentrated nitric acid, and filtered with a
0.45-mm Whatman Autovial filter (USA) before analysis.
Solution pH was measured using an Accumet basic pH
meter (Fisher Scientific, USA).
2.2. Preparation of citric acid-modified and base-
extracted activated carbons
The activated carbon was ground and sieved to retain
the 2032 mesh fraction. It was washed with deionised
(DI) water to remove fine powdered activated carbon left
after sieving. It was then left to dry in an oven at 110 8C
for 2 h and denoted by WAC.
The WAC was reacted with a 1 M citric acid solution at
a ratio of 4 g activated carbon to 25 ml citric acid solution.
It was shaken for 30 min before being dried at 50 8C
overnight. The citric acid modified activated carbon was
then washed with DI water until no turbidity could be
observed when a 0.1 M lead nitrate solution was added to
the washed liquid. The modified activated carbon was
dried at 110 8C for 2 h and referred to as CAC.
A fraction of CAC was continuously washed with a 1 M
sodium hydroxide solution for at least 2 h. It was then
washed with DI water to remove the excess sodium
hydroxide until no pH variation in the washed liquid could
be detected. This base-extracted CAC was then dried at
110 8C for 2 h and referred to as SAC.
2.3. Surface properties
The specific surface areas of the activated carbon
samples were determined using a NOVA 300 BET analyzer
(QuantaChrome, USA). Before adsorption isotherms were
obtained, the activated carbon sample was purged with
pure nitrogen gas overnight at a temperature of 150 o C to
remove any contaminants as well as moisture that might be
present on the activated carbon surfaces.
The surface morphology of the activated carbon samples
was visualized by scanning electron microscopy (JEOL,
JSM-5600V, Japan). SEM enables the direct observation of
any surface microstructure changes in the activated car-
bons that would have occurred due to the citric acid
modification.
Potentiometric titration experiments were carried out
with an automatic titrator (Metrohm 716 DMS Titrino,
Switzerland). A 0.25-g amount of activated carbon was
added to a conical flask containing 50 ml of 0.1 M sodium
nitrate as background ionic strength. The solution was
shaken for 48 h on a shaker. The titration was carried out
using 0.1 M NaOH and 0.1 M HNO 3 solutions.
2.4. Adsorption equilibrium
The activated carbons of varying amounts were added to
conical flasks that contained 100 ml buffered or unbuffered
CuCl 2 solutions. Buffered solution with a pH of 4.9 was
comprised of 0.07 M sodium acetate and 0.03 M acetic
acid. The unbuffered solutions pH values ranging from 3
to 11 were adjusted by adding HCl or NaOH. The
solutions were shaken on a shaker with temperature
controlled at 25 8C for 48 h in order to reach equilibrium.
The final samples were analyzed using ICP-ES.
2.5. Adsorption kinetics
A 10-g amount of activated carbon was added to 1000-
ml buffered or unbuffered 1310 24 M CuCl 2 solution. The
solution was then stirred at a constant rate. Samples were
taken at different time intervals and analysed using ICP-
ES. The pH was 4.9 in the buffered solutions; while the
initial and final pH values were 5.0 and 5.2 in the
unbuffered solutions.
3. Results and discussion
3.1. Specific surface areas of activated carbon samples
As represented in Table 1, the surface area is 648 m 2 / g
for the WAC, similar to the value reported by Corapcioglu
and Huang [6], but lower than 1008.8 m 2 / g reported by
Chen and Lin [7]. The difference could be due to the
removal of considerable organic by-products and minerals
present in the activated carbon surface. In this study, the
carbon was washed between 20 and 30 times until the pH
and the conductivity of the water samples became con-
stant; while the carbons were normally washed 35 times
in most of studies (e.g., Chen and Lin [7]).
The citric acid modification of the activated carbon
further reduces the surface areas of CAC and SAC by 34
 J.P. Chen et al. / Carbon 41 (2003) 19791986 1981

Table 1
Summary of specific surface areas of activated carbon samples
Carbon type Description Specific surface area (m 2 / g)
WAC Unmodified activated carbon 648
CAC Citric acid modified activated carbon 431
SAC Sodium hydroxide-extracted CAC 448

and 31%, respectively. This could arise from pore block-
age by adsorbed citric acid molecules. Because of its small
molecular size, citric acid can easily access the pore
structure of the activated carbon. This finding is consistent
with the results reported by Ferro-Garcia et al. [8],
indicating that the surface area of activated carbon de-
creased from 1086 to 643 m 2 / g after adsorption of gallic
acid [(HO) 3 C 6 H 2 CO 2 H]. Some surface area of CAC is
recovered after sodium hydroxide treatment. This may be
partially attributed to the removal of the organic substances
within the pore structure, which are soluble in alkali
solution.
3.2. SEM micrographs
reduction in the surface area of CAC as compared with
that of WAC (Table 1). It implies that the adsorption
kinetics in CAC may be much slower than that in WAC
since clogging of the cracks and cavities can lead to
resistance in the metal transport from the solution to the
adsorption sites.
3.3. Potentiometric titration
The effect of the modification was investigated by
potentiometric titration of the carbon samples before and
after modification. The amphoteric behaviour of activated
carbons can be described by the following ionisation
reactions [6,7]:

SOH 1 H SOH 2
1 1
Fig. 1 shows the SEM micrographs of activated carbon Ka1 (1a)
samples before and after citric acid modification. It dem-
onstrates that there are considerable small cavities, cracks SOH SO 1 H
2 1
Ka2 (1b)
and attached fine particles over the activated carbon
surface, forming a system of complicated pore networks. where SOH represents a generalized surface functional
Comparison of these micrographs shows that the modi- group.
fication does not significantly change the morphology of The potentiometric titration data were used in the
the surface matrix of the carbons. However, the citric acid determination of the above the intrinsic surface acidity
modification reduces the number of cracks and cavities on constants (Ka1 and Ka2 ) and the concentration of surface
the carbon surface, which are clogged by the adsorbed functional group of carbons (SOH). An equilibrium con-
citric acid molecules. This also explains the reasons for the stant searching program, called FITEQL developed by

Fig. 1. SEM micrographs of the surfaces of the carbons: (a) WAC; (b) CAC.
1982 J.P. Chen et al. / Carbon 41 (2003) 19791986
Fig. 2. Experimental and modelled titration curves for WAC and
CAC.
Herbelin and Westall [9] was employed. The experimental
data and modelling fitting curves for the titration of WAC
and CAC are given in Fig. 2. The modelling results for
both WAC and CAC are in good agreement with the
experimental data. The adsorption constants and the con-
centration of surface functional group are given in Table 2.
The surface site density, calculated from the concentration
of surface functional group and specific surface area, is
0.18 sites / nm 2 for WAC and 0.44 sites / nm 2 for CAC.
These values are in good consistence with the reported
values of 0.05|0.3 sites / nm 2 for granular activated car-
bons by Corapcioglu and Huang [6]. Citric acid modi-
fication increases the surface site density by 144%, indicat-
ing that the modified activated carbon would greatly
enhance its metal adsorption capacity.
The intersection points of the titration curves with
solution pH axis are defined as point of zero charge
(pH pzc ). The pH pzc values for WAC and CAC are 7.07 and
6.54, respectively. The pH pzc result of WAC is in good
agreement with that of Chen and Lin [7]. The pKa and
pH pzc values of CAC show that it is more acidic than the
WAC due to the modification.
Table 2
Surface site properties of activated carbon samples*
Carbon type
Concentration of surface functional groups (mmol / g)
Surface acidity constants
pKa1
pKa2
pH pzc
* Units: Ka1 : M 21 ; Ka2 : M.
3.4. Copper ion adsorptive isotherms at controlled pH
Copper ion adsorption capacities of various activated
carbons at pH 4.9 were calculated by best-fitting the
experimental results with least-square regression to the
Langmuir isotherm model, which is expressed by the
following equation:
qmax bCe
qe 5 ]] (2)
1 1 bCe
where qe is the amount of Cu 21 adsorbed at equilibrium
(mg / g), Ce is the equilibrium concentration of copper in
solution (mg / l), qmax is the maximum adsorption capacity,
b is the Langmuir constant related to heat of adsorption.
The Langmuir plots for copper isothermal adsorption
data at controlled pH are shown in Fig. 3a. It demonstrates
that the Langmuir adsorptive isothermal equation fits the
experimental data well. Comparison of the qmax values in
Table 3 shows that the CAC has 143% higher copper
adsorption capacity than WAC, which is very consistent
with the enhancement in the surface site density. This
indicates that the apparent reduction in the surface areas of
the carbons does not adversely affect copper adsorption.
The immobilization of citric acid on the activated carbon
surface introduces more surface adsorptive sites (mainly
carboxylic functional groups from the citric acid), which
provide additional copper ion binding capacity. The im-
mobilization of citric acid may also change the nature of
the carbon surface from hydrophobic to hydrophilic, which
facilitates the access of copper ions to surface adsorption
sites. The copper adsorptive capacity of SAC is 93%
higher than that of the WAC; however, it is lower than that
of the CAC. This might result from removal of organic
substances by the alkali NaOH solution. These substances
can also participate in the metal binding process and
contribute to copper adsorption.
It is noteworthy that the correlation coefficients (r 2 ) in
the linear regression are 0.9940 and 0.9996 for CAC and
SAC, respectively, which are higher than 0.9826 for WAC.
It suggests that the activated carbon surface becomes more
homogenous after the modification. The citric acid con-
tains carboxylic functional groups. They can fully cover
the carbon surfaces when the modification is applied,
which results in homogeneous surfaces of the carbons.
WAC CAC
0.19 0.32
4.52 3.98
8.42 8.77
7.07 6.54
 J.P. Chen et al. / Carbon 41 (2003) 19791986 1983

Higher content of carboxylic functional groups can sig-

nificantly improve the adsorption as the affinity between
metals and the group is very high [1].
To explain the observed adsorption equilibrium more
clearly, the Freundlich isotherm model is also used:

qe 5 Kf C e1 / n (3)

where Kf is Freundlich adsorption constant, 1 /n is a

measure of adsorption intensity.
Freundlich plots for the copper adsorption at pH 4.9 are
shown in Fig. 3b. It illustrates that adsorption of copper
ions onto these activated carbons obeys Freundlich iso-
therm model as well. The calculated constants Kf and 1 /n
are given in Table 3.
1 /n,1 in Table 3 indicates an unfavourable adsorption
reaction. In other words, the increase in the equilibrium
concentration in the solid phase (qe ) is lower than that in
the solution phase (Ce ). This suggests that with progressive
coverage of activated carbon surface, the repulsive forces
among the copper ions (e.g., electronic and Coulombic
repulsion) become more dominant than the attractive forces
(e.g., Van der Waals forces) [10]. Hence, copper ions
manifest a weaker tendency to adsorb onto the activated
carbon surface.
The Freundlich equation is based on an assumption of
adsorption onto heterogeneous surfaces. The correlation
coefficient in the linear regression is 0.9934 for WAC,
much higher than the values for CAC and SAC. Hence, it
confirms that the surface of WAC is more heterogeneous
than that of citric acid modified activated carbons. This
heterogeneity arises from the large number of different
functional groups on activated carbon surface (e.g., car-
boxylic, carbonyl, hydroxyl, ether, phenolic, quinine, and
lactonic groups) and the various adsorbentadsorbate
interactions.

3.5. pH effect on copper adsorption

Adsorption of copper ions onto the carbons at different

Fig. 3. Copper isothermal adsorption at pH 4.9: (a) Langmuir plot,
(b) Freundlich plot.
initial pH is shown in Fig. 4. It demonstrates that the
copper adsorption by the WAC is strongly pH dependent.
The copper adsorption sharply increases when the solution
pH is increased from 3 to 4, which is in consistence with
the observations reported in the literature [6,7]. The copper

Table 3
Adsorption isotherm constants at pH 4.9*
Carbon type Langmuir constants Freundlich constants
qmax b r2 Kf 1 /n r2
WAC 6.14 0.18 0.9826 2.16 0.24 0.9934
CAC 14.92 0.08 0.9940 1.66 0.57 0.9025
SAC 11.85 0.20 0.9996 2.72 0.38 0.9361
* Units: qmax : mg / g; b: (mg / l)21 ; Kf : (mg / g) /(mg / l)1 / n .
1984 J.P. Chen et al. / Carbon 41 (2003) 19791986

Fig. 4. Effect of initial solution pH on copper adsorption.

ion adsorption is mainly due to the strong dependence of

dissociation of surface functional groups on the solution
pH. As pH increases, more surface functional groups
dissociate to provide metal binding sites, which results in
higher metal ion adsorption. The interaction of copper ions
with activated carbon can be described as:

SOH 1 Cu 21 SOCu 1 1 H 1 (4a)

SOH 1 Cu 21 1 H 2 O SOCuOH 1 2H 1 (4b)

The dissociation constant of citric acid is 3.1 [11], which

suggests that citric acid modified activated carbon should
show high copper adsorption at solution pH of above 3.1.
This is confirmed in Fig. 4. CAC adsorbed nearly 85%
copper ions from the aqueous solution even at solution pH
of about 3.5, while SAC adsorbed nearly 100% copper
ions at the same solution pH. It suggests that citric acid
modified activated carbon can be applied efficiently in a
wider pH range.
3.6. Adsorption kinetics
Fig. 5 shows copper ion adsorption kinetics on the
carbons. It illustrates that adsorption follows a first rapid
step and a second slow step. Adsorption kinetics of the
surface modified activated carbons is much slower than
that of WAC. The adsorption equilibrium times are 6, 10,
and 20 h when WAC, CAC and SAC are used, respective-
ly. Immobilization of citric acid on the activated carbon
surfaces impedes the access of copper ion to the adsorption
sites, which are consistent with the findings in the specific
surface area and the SEM micrographs. In the modi-
Fig. 5. Kinetics of copper adsorption: (a) observation, (b) in-
traparticle diffusion.
fication, citric acid is adsorbed to the surfaces of carbons,
which reduces the effective diameter of the mi-
croporosities. This in some cases may actually prevent
further adsorption of other substances. The measurement
of the specific surface area by the BET analyzer is based
on adsorption of nitrogen gas. Our BET measurement
shows that the modification reduces the specific surface
area by 34% (see CAC versus WAC in Table 1). There is
not much difference between WAC and CAC in adsorption
kinetics as shown in Fig. 5a. Comparison of nitrogen
adsorption in the BET measurement and metal adsorption
kinetics indicates that the copper uptake is not so critically
dependent on adsorption potentials within porosities.
 J.P. Chen et al. / Carbon 41 (2003) 19791986
It can be assumed that the adsorption of copper ions
onto the activated carbons follows mainly these three
consecutive steps of external diffusion, intraparticle diffu-
sion, and finally adsorption reactions. One or more of these
steps can control the adsorption kinetics. In most cases, the
adsorption reactions occur rapidly. Therefore, the first two
steps are normally important in the kinetics. There are a
series of theoretical models available to describe the
adsorption kinetics [7,12]. However, the mathematical
solutions are pretty complex and require more input
information, such as adsorption reaction constants.
A simplified intraparticular diffusion model was also
employed to elucidate the adsorption mechanisms. It was
first developed by Weber and Morris [13] and has been
used in adsorption kinetic studies [14]. It is assumed that
the adsorption is controlled by three stages: the first
sharper linear stage being a rapid external diffusion and
surface adsorption; the second linear stage being a gradual
adsorption stage, where the intraparticle diffusion is rate-
limited; and the final stage being final equilibrium stage
where the intraparticle diffusion starts to decrease due to
low concentration in solution phase as well as less
available adsorption sites.
Adsorption capacity (q, mg / g) can be plotted against
t 1 / 2 . As shown in Fig. 5b, the adsorption has three stages.
The first stage in the four adsorption cases is completed in
about 6.25 min. The second stages in the cases demon-
strate a linear relationship. The third stage is a slow
process, due to the low concentration gradient.
The second stage can be described as following:
q | kdt 1 / 2 (5)
where k d is an intrinsic kinetic rate constant for intraparti-
cle diffusion.
In the determination of the above k d values, calculation
only takes into account of the range of 10 to 60 min of the
adsorption region. The k d values are 4.15310 22 , 4.293
10 22 , 4.73310 22 and 6.06310 22 (mg / g) / min 1 / 2 , for
WAS, CAC, SAC and CAC with buffered solution (pH
4.9), respectively. Higher linear regression coefficients
(r 2 .0.99) are obtained, which indicates the importance of
intraparticle diffusion in the second stage.
Comparison of the k d values of WAS, CAC and SAC
indicates that the chemical surface modifications do not
change the kinetic properties in the intraparticle diffusion.
It is observed that the CAC case with buffered solution
(pH 4.9) has a larger value. The buffered solution is
comprised of sodium acetate / acetic acid, which may form
additional copper complexes and possibly facilitate the
metal mass transfer.
4. Conclusions
Activated carbon modification by citric acid significantly
improves its copper ion adsorption capacity. The maxi-
1985
mum adsorption capacity increased from 6.14 mg Cu / g
WAC to 14.92 mg Cu / g CAC and 11.85 mg Cu / g SAC,
respectively. After the modification, the activated carbon
surface became more homogeneous; while its specific
surface area decreased significantly.
The adsorption kinetics of the modified carbons was
slower than that of the unmodified carbon. The modi-
fication does not change both external diffusion and
intraparticle diffusion properties.
Effect of initial solution pH on the copper adsorption
onto the citric acid modified carbons was insignificant;
however, it became important when the unmodified carbon
was used. These modified carbons were able to maintain
high metal adsorption capacity in very wide pH range.
Therefore, they can be useful in treating wastewater with a
wider pH range.
Acknowledgements
The financial support provided to J.P.C. by the National
University of Singapore under RP-3981604 and R-279-
000-104-112 is appreciated.
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