Desalination 242 (2009) 1928

0011-9164/09/$ See front matter 200 Elsevier B.V.

*Corresponding author.
Increasing the phenol adsorption capacity of neutralized
red mud by application of acid activation procedure
Ali Tor
a
*, Yunus Cengeloglu
b
, Mustafa Ersoz
b
a
Selcuk University, Department of Environmental Engineering, Campus, 42031 Konya, Turkey
Tel. +90 (332) 223-1914; Fax +90 (332) 241-0635; email: ali.alitor@gmail.com
b
Selcuk University, Department of Chemistry, Campus, 42031 Konya, Turkey
Received 9 October 2007; accepted revised 19 March 2008
Abstract
The objective of this study was to investigate the removal of phenol from aqueous solution by using acid
activated red mud in batch adsorption experiments. The study was carried out as functions of pH, contact time,
activated red mud dosage and initial phenol concentration. It was found that the maximum removal was obtained at
pH below 8 and the adsorption equilibrium time was 10 h. Adsorption was followed the pseudo second-order
kinetic model. According to the coefficient of determination and non-linear regression analysis carried out by Chi-
square test, the Langmuir isotherm better represented the adsorption data in comparison to the Freundlich isotherm.
The phenol adsorption capacity of the activated red mud (8.156 mg/g) was found to be higher than that of the
neutralized red mud (4.127 mg/g) at pH 6 and 251C. Negative G
0
value (22.692 kJ/mol) indicated that the
adsorption of phenol onto the activated red mud was spontaneous and feasible process.
Keywords: Activated red mud; Adsorption; Phenol removal; Acid activation
1. Introduction
Phenolic compounds are common pollutants
found particularly in the effluents from petroleum
and petrochemical, coal conversion, and phenol
producing industries [1]. Due to their toxicity and
carcinogenity [2], water and wastewater contain-
ing phenolic compounds must be treated before
being used and discharged to receiving water bod-
ies.
Adsorption is a well-known removal technique
for organic compounds from water [3], but the
cost of adsorptive removal process is high when
pure sorbents (i.e. activated carbon, etc.) are used
due to their high price [4,5]. Consequently, the
cost of pure adsorbents may be a limitation for
many treatment applications and there is a strong
motivation to find cost-efficient alternative sor-
bents obtained from industrial and agricultural
waste, such as bagasse fly ash [6], petroleum coke
[7], paper mill sludge [8], red mud [9,10], fertil-
doi:10.1016/j.desal.200 .0 .0 8 3 28
8 All rights reserved.
20 A. Tor et al. / Desalination 242 (2009) 1928
izer and steel industries waste [1114], lignin [15],
wood charcoal [16], etc.
Studies using red mud residues from alumina
production as unconventional adsorbents for wa-
ter and wastewater treatment purposes are moti-
vated by the fact that red mud is a fine-grained
mixture of oxides and hydroxides, capable of re-
moving several contaminants, as well as being
widely available. For instance, several studies
have reported that red mud or activated red mud
can efficiently remove different pollutants from
water, including phosphate [17,18], fluoride [19],
nitrate [20], cadmium, lead, copper [2124], ar-
senic [2527], dye [28], boron [29], etc.
In our previous study [30], it was shown that
neutralized red mud had affinity for phenol due
to the interaction between the metal oxides on the
surface of red mud and polar phenol molecule.
However, considering the handling problems as-
sociated with applying large quantities of adsor-
bent, the necessary amount of red mud required
may be relatively high. It is believed that the ad-
sorption capacity of neutralized red mud is hin-
dered by the presence of surface impurities (i.e.,
salts and basic precipitates). Hence, application
of an activation procedure may improve the ad-
sorption capacity of the red mud [31]. Therefore,
in this study the neutralized red mud was acti-
vated by HCl and adsorption performance of the
obtained activated red mud for the removal of
phenol from aqueous solution was investigated
in batch adsorption experiments as functions of
pH, contact time, adsorbent dosage and initial
phenol concentration.
2. Materials and method
2.1. Red mud and activation procedure
The red mud was obtained from Seydisehir
Aluminum Plant (Konya, Turkey). The raw red
mud has strongly alkaline character (pH 12
13). Therefore, before it was used, the red mud
was neutralized by washing with distilled water
as described in [30] until the equilibrium pH is
8.08.5. Then it was dried at 40C. The grain size
of the neutralized red mud was mostly (>94%)
less than 10 m. Its average composition was de-
termined according to the procedure described in
[32] by using ICP-AES (Varian, vista/AX CCD
Simultaneous ICP-AES, Switzerland) and the re-
sult is given in Table 1.
Later, activation of neutralized red mud was
carried out as follows. 10 g of water-washed and
dried red mud was boiled in 200 mL of 20% wt.
HCl for 20 min. The acid slurry was then filtered
and the residue was washed with distilled water
to remove residual acid and soluble Fe and Al
compounds. Finally, the residue was dried at 40C,
and used for the experiments without further treat-
ment. The BET surface area of the activated red
mud was measured by Apak et al. [21] with nitro-
gen as 20.7 m
2
/g.
2.2. Adsorption experiments
All adsorption experiments were carried out
with the batch method at a constant ionic strength
of 0.01 M maintained with NaCl. The adsorption
equilibrium was attained by stirring a known
amount of activated red mud in 50 mL of aque-
ous phenol solutions which were stirred at 700
rpm with a magnetic stirrer (IKA Labortechnik,
Germany) at 251C for a predetermined period
of time. After the equilibrium time, solution was
centrifuged for 10 min at 3000 rpm.
The supernatant solution was analyzed for re-
sidual concentration of phenol at
max
= 500 nm
Table 1
Average composition of the neutralized red mud (% by
wt), [n = 3]
Fe
2
O
3
39.700.67
Al
2
O
3
18.710.59
SiO
2
14.520.37
Na
2
O 8.820.96
TiO
2
4.900.54
CaO 4.470.56
Loss on ignition 8.150.40
A. Tor et al. / Desalination 242 (2009) 1928 21
using spectrophotometry (Shimadzu UV-160A,
Japan) according to the 4-aminoantipyrene
method [33] as follows: 0.5 mL of 4-amino-
antipyrene was added into supernatant solution.
After mixing the solution, 0.5 mL of K
3
Fe(CN)
6
was added into the solution and mixed again. Af-
ter 15 min, spectrophotometric determination was
carried out. Blank runs, with only the sorbate in
50 mL of distilled water, were conducted simul-
taneously at similar conditions to account for
adsorbed by walls of stoppered conical flask.
Initial pH of the solutions was adjusted to de-
sired pH level by using 0.1 M HCl or 0.1 M
NaOH. The amount of phenol adsorbed was cal-
culated from the change in the phenol concentra-
tion in the aqueous solution before and after equi-
librium and the weight of the dry activated red
mud according to Eq. (1).
( )
0
/
e
q C C V m = (1)
where q is phenol adsorbed (mg/g); C
o
initial
concentration of phenol (mg/L); C
e
concentra-
tion of phenol in the solution at equilibrium time
(mg/L); V solution volume (L); m activated
red mud dosage (g). The experimental parameters
studied are pH (312), adsorbent amount (110
g/L), contact time (116 h), initial phenol con-
centration (5200 mg/L).
Phenol, NaCl, NaOH and HCl were of ana-
lytical grade and obtained from Merck Co.
(Darmstadt, Germany).
3. Results and discussion
3.1. Effect of acid activation procedure
It was reported that acid activation signifi-
cantly enhanced the adsorption capacity of the
neutralized red mud toward some anions (i.e., ar-
senate and nitrate) [20,31]. Therefore, the acid
activation procedure was applied on the neutral-
ized red mud to increase its adsorption efficiency
toward phenol. The results in Table 2 show that
acid activation process increased both the surface
Table 2
Comparison of the neutralized and acid activated red mud
for adsorption of phenol from aqueous sample. (Phenol
concentration: 60 mg/L, contact time: 10 h, pH of the
solution: 6, red mud dose: 8 g/L, agitation speed: 700 rpm
and temperature: 25 1C)
a
data from [21]
b
data from [30]
Surface area,
m
2
/g
q,
mg/g
% removal
Neutralized red
mud
14.2
a
2.501
b
33
b

Acid activated
red mud
20.7
a
5.412 70
area and phenol adsorption capacity of neutral-
ized red mud. Red mud is of sodalite compounds
((Na, Ca)
8
(AlSiO
4
)
6
(SO
4
, OH, S, Cl)
2
) [24] which
are expected to hinder the adsorption by blocking
the available adsorption sites for phenol. There-
fore, the leaching out of the sodalite compounds
during acid treatment increases the adsorption
capacity of the neutralized red mud [31].
3.2. Effect of pH
The amount of phenol adsorbed depends on
the distribution of phenol and phenolate ion which
are controlled by pH of the solution. These two
species in the solution compete for the adsorp-
tion onto the activated red mud. Considering the
pKa of 10 of phenol [8], it is present in molecular
form in aqueous solution when pH is less than 9.
However, it is present in the form of phenolate
ion when pH of the equilibrium solution is higher
than 10. Additionally, the solution pH relative to
the point of zero charge (pHpzc) for the activated
red mud also needs to be considered. pHpzc for
the activated red mud was reported as about 8.5
[23]. When pH of the solution exceeds the pHpzc,
the surface of red mud particles is negatively
charged.
22 A. Tor et al. / Desalination 242 (2009) 1928
It is seen in Fig. 1 that phenol is adsorbed to a
lesser extent at pH above 8 due to the repulsive
forces between phenolate ion and negative
charged of the red mud surface. This result is in
agreement with our previous study [30] which
reported the removal of phenol by neutralized red
mud. The adsorption mechanism of phenol by red
mud was also described in [30].
The change in pH of the solution during the
experiments was observed and it was seen that at
the end of the experiments, final pH of the solu-
tions did not exceed the pKa of phenol and pHpzc
of the activated red mud.
3.3. Effect of contact time and adsorption kinetics
The removal of phenol as a function of con-
tact time is shown in Fig. 2. It was observed that
with a fixed amount of activated red mud, the re-
moval of phenol increases with time and then at-
tains equilibrium after 10 h. Fig. 2 additionally
indicated that the time to reach equilibrium con-
ditions appears to be independent of initial phe-
nol concentrations. The same equilibrium time
was found for phenol adsorption by neutralized
red mud [30]. However, adsorption occurs rap-
Fig. 1. Effect of pH of the solution on the adsorption of
phenol. Phenol concentration: 15 mg/L, activated red mud
dose: 8 g/L, contact time: 10 h, agitation speed: 700 rpm
and temperature: 25 1
o
C.
0
0.5
1
1.5
2
0 2 4 6 8 10 12 14
pH
q
,

m
g
/
g
Fig. 2. Removal of phenol as a function of contact time.
Activated red mud dose: 8 g/L, pH: 6, agitation speed:
700 rpm and temperature: 25 1C; () 5 mg/L with ac-
tivated red mud; () 60 mg/L, () 120 mg/L, solid line
for activated red mud, dashed line for neutralized red
mud from [30].
0
25
50
75
100
0 5 10 15 20
Time (h)
R
e
m
o
v
a
l

(
%
)
idly with acid activated red mud compared to neu-
tralized red mud. For 5 mg/L of phenol concen-
tration, 70% of the initial removal of phenol is
carried out within the first 2 h of contact time us-
ing activated red mud, while 4 h is needed to ob-
tain the 70% removal of phenol using neutralized
red mud.
It is known that adsorption kinetics is con-
trolled by different kinds of mechanisms such as
mass transfer, diffusion control, chemical reac-
tions, and particle diffusion. Lagergrens pseudo-
first order and pseudo-second order kinetic mod-
els were employed in order to clarify the kinetic
characteristics of the adsorption of phenol onto
the activated red mud.
3.3.1. Pseudo-first order kinetic model
The linearized form of pseudo-first order rate
equation is given as Eq. (2) [34].
( )
1
log log / 2.303
e t e
q q q k t = (2)
where q
e
and q
t
are the amounts of phenol adsorbed
(mg/g) at equilibrium and at time t (min), respec-
A. Tor et al. / Desalination 242 (2009) 1928 23
tively, and k
1
(1/min) is the adsorption rate con-
stant of first-order adsorption.
For the studied initial concentrations, the rate
constant (k
1
) and theoretical equilibrium sorption
capacities, q
e
(calculated), calculated from the
slope and intercept of the linear plots of the pseudo
first-order kinetic model are given in Table 3. The
coefficients of determination (R
2
) for the linear
plots are between 0.923 and 0.933. However, q
e
(calculated) and q
e
(experimental) values are not
in agreement with each other. Therefore, it could
be suggested that the adsorption of phenol onto
the activated red mud was not a first-order reac-
tion.
3.3.2. Pseudo-second order kinetic model
The experimental data was also applied to the
pseudo-second order kinetic model given as
Eq. (3).
( )
2
2
d / d
t e t
q t k q q = (3)
where k
2
is the rate constant of pseudo second-
order chemisorption (g/(mg min)). For boundary
conditions (t = 0 to t = t and q
t
= 0 to q
t
= q
t
),
pseudo second-order kinetic model of Ho and
McKay [35,36] is:
( )
2
2
/ 1/ /
t e e
t q k q t q = +
(4)
For different concentrations of phenol, the fit
of this model was controlled by each linear plot
of t/q
t
vs. t, respectively. The constants calculated
from the slope and intercept of the plots are given
Table 3
Values of adsorption rate constant for pseuso first-order and pseudo-second order kinetic models
Pseudo first-order kinetic model Pseudo second- order kinetic model C
(mg/L)
q (exp)
(mg/g)
k
1
(1/min)
q (cal)
(mg/g)
R
2
k
2
[g/(mg.min)]
q (cal)
(mg/g)
R
2

5 0.610 0.005 0.264 0.923 0.027 0.643 0.999
60 5.412 0.004 3.114 0.933 0.002 5.959 0.997
120 7.428 0.003 4.204 0.931 0.001 7.986 0.998
in Table 3. It can be seen from the results in Table 3
that R
2
values are higher than those obtained from
the first-order kinetics. Additionally, theoretical
and experimental q
e
values are in good accordance
with each other. Therefore, it is possible to sug-
gest that the sorption of phenol onto activated red
mud followed second-order type reaction kinet-
ics.
The adsorption would occur via interaction
between the polar phenol molecule and the posi-
tively charged red mud surface as below [30].
( ) ( )
+ +
2
+ +
2 2
MOH + H MOH
MOH phenol MOH --- phenol

+
where M is the metal ion (Si, Fe or Al).
Therefore, second-order chemical reaction ki-
netics would be expected to be followed in the
sorption processes and it is possible to state that
chemisorption is the rate determining step for the
presented study.
3.4. Adsorption isotherm models
The analysis of the sorption isotherms is im-
portant for design purposes. Therefore, experi-
mental data was analyzed with well known sorp-
tion isotherm models including the Langmuir and
Freundlich isotherms.
Langmuir sorption isotherm models the mono-
layer covarage of the sorption surfaces and as-
sumes that sorption take places on a structurally
homogeneous surface of the adsorbent. This iso-
therm is given as Eq. (5) [37].
24 A. Tor et al. / Desalination 242 (2009) 1928
( )
0
/ 1
e e e
q Q b C b C = + (5)
The linear form of the Langmuir isotherm
model can be presented as Eq. (6);
( )
0 0
/ 1/ /
e e e
C q Q b C Q = + (6)
where C
e
is the concentration of phenol (mg/L) at
equilibrium, Q
o
is the monolayer capacity of the
adsorbent (mg/g) and b is the Langmuir adsorp-
tion constant (L/mg). The plot of C
e
/q
e
vs. C
e
gives
a straight line and the values of Q
o
and b can be
calculated from the intercept and slope of the plot,
respectively (Fig. 3).
Freundlich equation models the multilayer
sorption on the heterogeneous surfaces. The
Freundlich model is formulated as Eq. (7) [38].
1/ n
e e
q k C = (7)
Linearised form of the Freundlich equation is
given by the following equation:
log log 1/ log
e e
q k n C = + (8)
where C
e
is equilibrium concentration (mg/L), k
is the sorption capacity (mg/g) and n is an em-
Fig. 3. The Langmuir isotherm plot for phenol adsorp-
tion on activated red mud. Red mud dose: 8 g/L, pH: 6,
agitation speed: 700 rpm and temperature: 25 1C.
y = 0.123 x + 0.938
R
2
= 0.997
0
5
10
15
20
0 50 100 150
C
e
, (mg/L)
C
e
/
q
e
Fig. 4. The Freundlich isotherm plot for phenol adsorp-
tion on activated red mud. Red mud dose: 8 g/L, pH: 6,
agitation speed: 700 rpm and temperature: 25 1C.
y = 0.420x + 0.107
R
2
= 0.962
-0.4
0
0.4
0.8
1.2
-1 0 1 2 3
log C
e
l
o
g

q
pirical parameter. According to Eq. (8), the plot
of the log q
e
vs. log C
e
gives a straight line and k
and n values are calculated from the intercept and
slope of this straight line, respectively (Fig. 4).
The isotherm constants and R
2
values for each
model are given in Table 4. According to the R
2
values, the Langmuir isotherm better represented
the adsorption data. This result is also supported
by non-linear regression analysis carried out by
Chi-square statistic test, which is basically the sum
of the squares of the differences between the ex-
perimental data and data obtained by calculating
from models, with each squared difference divided
by the corresponding data obtained by calculat-
ing from models [39]. The mathematical statement
of Chi-square test can be given as Eq (9):
( )
2
2
/
e m m
q q q
(
_ =

(9)
where q
m
is the equilibrium capacity obtained by
calculating from the model (mg/g), and q
e
is ex-
perimental data of the equilibrium capacity
(mg/g). Small number of
2
indicates that data
from the model is close to the experimental data.
Whereas, large number of
2
indicates that data
A. Tor et al. / Desalination 242 (2009) 1928 25
Table 4
Langmuir and Freundlich isotherm parameters for the adsorption of phenol by activated red mud
Langmuir isotherm Freundlich isotherm
Q
o
(mg/g) b (L/mg) R
2
_
2
k (mg/g) n R
2
_
2

8.156 0.101 0.997 1.138 1.211 2.374 0.962 1.438
from the model is different from experimental data
[40]. It is seen in Table 4 that the Langmuir is a
better-fitting model compared to the Freundlich
one because it has lower
2
value. Fig. 5 shows
the non-linear adsorption isotherms.
It is very well-known that Langmuir type ad-
sorption is resulted with monolayer type adsorp-
tion. Namely, the adsorption is limited by surface
site saturation and the sorption onto red mud is
saturated on sites of the surface layer because of
less heterogeneous mixture of several minerals in
its structure [20]. In other words, less heteroge-
neous mineral assemblage on the surface of acti-
vated red mud results in a homogeneous surface.
The fit of the adsorption data to Langmuir iso-
therm model may indicate the homogeneous sur-
face of the acid activated red mud.
Comparison of the monolayer sorption capac-
ity, Q
o
, and sorption equilibrium constant, b, for
the adsorption of phenol by non-conventional
adsorbents is presented in Table 5. It is seen in
Table 5
Comparison of monolayer sorption capacity, Q
o
, and sorption equilibrium constant, b, for the adsorption of phenol by
non-conventional adsorbents
Adsorbents Q
o
, mg/g b, L/mg References
Petroleum coke treated with KOH 158.0 0.391 [7]
Granular activated carbon 49.720 0.109 [41]
Baggase fly ash 23.832 0.088 [42]
Coal 13.23 0.008 [43]
Acid activated red mud 8.156 0.101 Present study
Rice husk 4.508 0.001 [43]
Neutralized red mud 4.127 0.051 [30]
Coke breeze 0.171 0.001 [43]
Fig. 5. Non-linear adsorption isotherms. Red mud dose:
8 g/L, pH: 6, agitation speed: 700 rpm and temperature:
25 1C.
0
2.5
5
7.5
10
0 50 100 150
C
e
, mg/L
q
,

m
g
/
g
experimental
Langmuir
Freundlich
Table 5 that Q
o
of activated and neutralized red
mud is 8.156 mg/g and 4.127 mg/g, respectively.
In other words, the removal of phenol with acti-
26 A. Tor et al. / Desalination 242 (2009) 1928
vated red mud was two fold higher than the neu-
tralized one and activated red mud gives better
phenol adsorption efficiency than rice husk and
coke breeze [43] (Table 5).
The standard Gibbs free energy (G
0
) for the
adsorption process was calculated by using
Eq. (10) for studied conditions as below [26].
( ) ( )
0
ln 1/ / b G R T = A (10)
where b is a Langmuir constant that is related to
the energy of the adsorption process, R is the gas
constant (8.3145 J/mol.K), and T is temperature
(K). G
0
was determined as 22.692 kJ/mol,
which indicated that the adsorption of phenol onto
the activated red mud was spontaneous and fea-
sible process.
3.5. The effect of activated red mud dosage
The removal of phenol as a function of vary-
ing amounts of activated red mud is presented in
Fig. 6. Because the concentration of surface hy-
droxyl groups is related to the activated red mud
dosage, percent of adsorption increased with red
mud dosage, whereas q decreased (Fig. 6).
Fig. 6. The variation of phenol removal with activated
red mud dose. Phenol concentration: 15 mg/L, pH: 6,
agitation speed: 700 rpm and temperature: 25 1C.
0
25
50
75
100
1 2 4 6 8 10
red mud (g/L)
R
e
m
o
v
a
l

(
%
)
0
2
4
6
8
q
,

m
g
/
g
% removal
q, mg/g
The EPA lifetime health advisory for phenol
is 2 mg/L [1]. The final concentration of 1.95 mg/L
can be achieved by contacting the phenol solu-
tion (15 mg/L) with activated red mud dosage of
10 g/L (phenol removal: 87%). Namely, final con-
centration can be reduced to a value below the
regulatory limit by activated red mud at the fol-
lowing experimental conditions: inital phenol
concentration: 15 mg/L, pH: 6, red mud dose:
10 g/L, pH: 6, contact time: 10 h, agitation speed:
700 rpm and temperature: 25 1C.
3.6. The effect of co-existing anions
As known, drinking water or wastewater con-
tains many substances. In our previous work [30],
it was reported that the influence of co-existing
anions showed that an increase of chloride dos-
age from 10 to 50 mg/L had no effect on removal
of phenol by neutralized red mud, but phenol ad-
sorption decreased from 66 to 32% and 15% in
the presence of 50 mg/L nitrate and sulphate, re-
spectively. Similar effects of these anions on the
adsorption of phenol by activated red mud can be
expected.
4. Summary
This study investigated the possibility of in-
creasing the phenol adsorption capacity of neu-
tralized red mud by application of acid treatment.
It was found that the phenol adsorption from wa-
ter was significantly increased by application of
acid activation (for example, from 33% (for neu-
tralized red mud) to 70% (for activated red mud)
at the following conditions: phenol concentration:
60 mg/L, red mud dose: 8 g/L, pH: 6, contact time:
10 h, agitation speed: 700 rpm and temperature:
25 1C).
This is important when considering the pos-
sible practical application of the adsorption pro-
cess. Hence, we conclude that the acid activated
red mud produced in this study is a promising
unconventional adsorbent for the removal of phe-
nol from water. Additionally, phenol adsorption
A. Tor et al. / Desalination 242 (2009) 1928 27
characteristics of the activated red mud can be
concluded as follows:
1. The phenol adsorption capacity of activated
red mud is 8.156 mg/g. Namely, the removal
of phenol with activated red mud was two fold
higher than the neutralized form (4.127 mg/
g).
2. Maximum removal of phenol was obtained at
pH below 8.
3. The equilibrium time for removal of phenol
by activated red mud was determined as 10 h.
4. Adsorption was followed the pseudo second-
order kinetic model.
5. The Langmuir isotherm showed very good fit
with the adsorption data. This indicates that
the homogeneous adsorption occurs, which is
also supported by Chi-square statistic test.
6. Adsorption of phenol onto the activated red
mud is spontaneous and feasible process.
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