Journal of Colloid and Interface Science 295 (2006) 71–78

www.elsevier.com/locate/jcis

Application of zeolite MCM-22 for basic dye removal from wastewater

Shaobin Wang a,∗ , Huiting Li a , Longya Xu b
a Department of Chemical Engineering, Curtin University of Technology, G.P.O. Box U1987, Perth, WA 6845, Australia
b Dalian Institute of Chemical Physics, Chinese Academy of Science, Dalian, People’s Republic of China

Received 30 June 2005; accepted 3 August 2005

Available online 6 September 2005

Abstract
MCM-22 was employed as an effective adsorbent for removal of basic dyes including methylene blue, crystal violet, and rhodamine B from
aqueous solution. The adsorption kinetics and isotherms were investigated. The adsorption capacity of MCM-22 for three dyes follows an order of
MB > CV ∼ RB. Kinetic studies indicate that the adsorption follows the pseudo second-order kinetics and the adsorption is a two-step diffusion
process with film diffusion dominating the process. The adsorption isotherm can be well fitted by both the Langmuir and the Freundlich models.
Thermodynamic calculations suggest that the adsorption of basic dyes on MCM-22 is an endothermic reaction.
 2005 Elsevier Inc. All rights reserved.

Keywords: MCM-22; Adsorption kinetics; Isotherm; Basic dyes; Wastewater treatment

1. Introduction zeolite composites for methylene blue adsorption and found

Dye effluents, discharged from the dyestuff manufacturing,
dyeing, printing, and textile industries, may contain chemicals
that exhibit toxic effects toward microbial populations and can
be toxic and/or carcinogenic to mammals. Conventional meth-
ods for the removal of dyes in effluents include physical, chem-
ical, and biological processes [1]. Physical adsorption is gener-
ally considered to be an effective method for quickly lowering
the concentration of dissolved dyes in an effluent, and acti-
vated carbon is the most widely used adsorbent for dye removal.
However, activated carbon suffers from high-cost production
and regeneration [2]. Therefore, other adsorbents such as ze-
olite, pillared clays with higher surface areas are alternatives.
Synthetic and natural zeolites have become increasingly im-
portant due to the wide range of their chemical and physical
properties and have been used as adsorbents, molecular sieves,
membranes, ion exchangers, and catalysts in the past decades.
However, the application of zeolites for dye removal from
wastewater has rarely been previously reported [3]. Balkose
et al. [4] reported an investigation using poly(vinyl chloride)-
* Corresponding author.
E-mail address: wangshao@vesta.curtin.edu.au (S. Wang).
0021-9797/$ – see front matter  2005 Elsevier Inc. All rights reserved.
doi:10.1016/j.jcis.2005.08.006
that the adsorption capacity of zeolite decreased when it was
embedded in composites. Meshko et al. [5] studied the adsorp-
tion of basic dyes from aqueous solutions onto granular acti-
vated carbon and natural zeolite. The equilibrium studies have
shown that the granular activated carbon has a higher adsorp-
tion capacity than the natural zeolite. Armagan and co-workers
[6–8] examined the ability of natural and modified zeolites to
remove reactive dyes from aqueous solutions. The adsorption
results indicated that the natural zeolite has a limited adsorp-
tion capacity for reactive dyes but is substantially improved
upon modification of its surfaces with quaternary amines. Qua-
ternary amine surfactant is not only hydrophobic to the surface
of the samples but also neutralizes the negative charge, which
makes the samples receptive to the negative charge of the dye
molecules by means of electrostatic attraction. The modified
zeolites are comparable to activated carbon. Metes et al. [3] in-
vestigated several synthetic zeolites for cleaning printing ink
wastewater and found that adsorption is independent of pore
structure. ZSM-5 and NH4 -Beta are effective while other zeo-
lites studied showed a lower efficiency. We also tested a natural
zeolite for dye removal from aqueous solution [9]. The natural
zeolite exhibits a higher adsorption capacity than fly ash but
still lower than unburned carbon in fly ash.
72 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78
MCM-22 is a novel nanoporous zeolite, synthesized by Mo-
bil researchers in 1990 [10]. It consists of two independent
and noninterconnecting pore systems: one consists of two-
dimensional channels with 10-ring pore openings (0.6 nm in
diameter); the second pore system consists of cavities with 12-
ring openings exposed on the (001) crystals surface with egg-
shaped supercages (1.4 nm in diameter). The unusual frame-
work topology, high thermal stability, large surface area and
good adsorption capacity render this zeolite very interesting for
adsorption and catalysis [11–15]. In the past a few years, MCM-
22 has been used in gas adsorption and catalysis; few applica-
tions have been reported for MCM-22 in aqueous adsorption.
Dahl et al. [16] reported the application of MCM-22 to adsorb
alcohols from water solutions. Enhanced adsorption was ob-
tained for alcohols with longer alkyl chains. To our knowledge,
no other investigations have been conducted for adsorption in
aqueous solution. In this paper, we report an investigation using
MCM-22 as an effective adsorbent to remove some basic dyes,
methylene blue, crystal violet, and rhodamine B, from aqueous
solution. The kinetics and adsorption equilibrium of the basic
dyes on MCM-22 were investigated.
2. Experimental
2.1. Adsorbent and dyes
The MCM-22 zeolite was synthesized by using an organic
mixture solution containing hexamethyleneimine and caprolac-
tam as a template. The detailed synthesis procedure is described
in Ref. [17]. The MCM-22 has a Si/Al ratio of 30 with a surface
area of 490 m2 /g.
Three basic dyes, methylene blue (MB), crystal violet (CV),
and rhodamine B (RB), were selected for adsorption tests. They
were obtained from AJAX Chemical. Their chemical structures
are displayed in Fig. 1. A stock solution with concentration at
10−4 M was prepared and the solutions for adsorption tests
were prepared from the stock solution to the desired concen-
trations (10−6 –10−5 M).
Fig. 1. Chemical structure of basic dyes.
2.2. Sorption test
Adsorption kinetics and isotherm experiments for all sam-
ples were undertaken in a batch reactor. The adsorption of
dye was performed by shaking 0.02 g of solids in a 200 ml
dye solution with varying concentrations at 100 rpm (Certomat
R shaker from B. Braun) at different temperatures. The sam-
ple was collected by separation of solid from solution using a
centrifuge. The determination of dye concentration was done
spectrophotometrically on a Spectronic 20 Genesis Spectropho-
tometer (USA) by measuring absorbance at λmax of 665, 590,
and 556 nm for MB, CV, and RB, respectively. From the dy-
namic adsorption curve, the equilibrium time was determined
for 10 days.
The data obtained from the adsorption tests were then used
to calculate the adsorption capacity, qt (mol/g), of the ad-
sorbent by a mass–balance relationship, which represents the
amount of adsorbed dye per the amount of dry adsorbent,
(C0 − Ct )
qt = V, (1)
W
where C0 and Ct are the concentrations of dye in solution
(mol/dm3 ) at time t = 0 and t = t , respectively, V is the vol-
ume of the solution (dm3 ), and W is the weight of the dry
adsorbent used (g).
3. Results and discussion
3.1. Adsorption of different dyes
Fig. 2 presents the dynamic adsorption of three different
dyes on MCM-22. One can see that adsorption is fast before
20 h and then it approaches equilibrium after 200 h. The time
profile of dye adsorption is a single, smooth, and continuous
curve leading to saturation, suggesting the possible monolayer
coverage of dye on the surface of the adsorbents. For the dif-
ferent dyes, equilibrium adsorption is quite different. MCM-22
exhibits much higher adsorption for MB while it shows simi-
lar adsorption for CV and RB. The equilibrium adsorption for
MB, CV, and RB will be around 1.7 × 10−4 , 1.2 × 10−4 , and
Fig. 2. Adsorption of basic dyes on MCM-22 at 30 ◦ C.
 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78
Fig. 3. Adsorption isotherm of MB on MCM-22 at different temperatures. (a) Freundlich model, (b) Langmuir model.
Fig. 4. Adsorption isotherm of CV on MCM-22 at different temperatures. (a) Freundlich model, (b) Langmuir model.
1.1 × 10−4 mol/g. The difference in adsorption for three dyes is
probably ascribed to the varying molecular size. As seen from
Fig. 1, MB is quite smaller than CV and RB, so that MB easily
enters the inner pores of MCM-22. Vinod and Anirudhan [18]
investigated the adsorption of three basic dyes, MB, CV, and
RB, on the humic acid (HA)-immobilized pillared clay (PILC)
and found the adsorption follows the order of MB > CV > RB.
Graham et al. [19] studied methylene blue and crystal violet ad-
sorption on activated carbon and reported similar results.
3.2. Adsorption isotherms
The equilibrium adsorption isotherm is of importance in the
design of adsorption systems. Several isotherm equations are
available and two important isotherms are selected in this study,
the Langmuir and Freundlich isotherms.
The Langmuir isotherm is based on an assumption that the
adsorption occurs at specific homogeneous sites within the ad-
sorbent. The equation is
Q0 KL Ce
Qe = , (2)
(1 + KL Ce )
where Qe is the adsorbed amount of the dye, Ce is the equilib-
rium concentration of the dye in solution, Q0 is the monolayer
73
adsorption capacity, and KL is the constant related to the free
energy of adsorption.
The Freundlich isotherm is an empirical equation employed
to describe heterogeneous systems. The Freundlich equation is
1/n
Qe = KCe , (3)
where K and n are Freundlich adsorption isotherm constants,
indicative of the extent of the adsorption and the degree of
nonlinearity between solution concentration and adsorption, re-
spectively.
Figs. 3–5 present adsorption isotherms of three dyes on
MCM-22 at different temperatures and the fitted curves for
Langmuir and Freundlich models. The parameters obtained
from the isotherms are given in Table 1. As seen the adsorp-
tion isotherms at different temperatures for the same dye are
very close and can be fitted very well using two isotherm mod-
els (evidenced from the correlation coefficients, >0.990). From
Table 1, it is also seen that the obtained adsorption capacities
from the Langmuir isotherm show slightly higher adsorption
for CV than RB on MCM-22.
The increase in dye adsorption with increasing temperature
might also be due to the enhanced rate of external and intra-
particle diffusion of the adsorbate, as diffusion is a dominant
74 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78

Fig. 5. Adsorption isotherm of RB on MCM-22 at different temperatures. (a) Freundlich model, (b) Langmuir model.

Table 1
Parameters of adsorption isotherms of basic dyes on MCM-22 at different temperatures
Temperature (◦ C) Dye Langmuir model Freundlich model
Q0 (mol/g) KL (dm3 /mol) R2 K [mol/g (L/mol)1/n ] 1/n R2
30 MB 1.73 × 10−4 4.03 × 107 0.999 3.11 × 10−4 0.0486 0.997
40 1.79 × 10−4 2.63 × 107 0.985 4.06 × 10−4 0.0673 0.996
50 1.76 × 10−4 3.53 × 107 0.999 2.86 × 10−4 0.0407 0.998
30 CV 1.20 × 10−4 8.97 × 106 0.994 2.06 × 10−4 0.0473 0.990
40 1.20 × 10−4 6.12 × 106 0.995 2.22 × 10−4 0.0543 0.991
50 1.26 × 10−4 8.70 × 106 0.995 2.27 × 10−4 0.0512 0.992
30 RB 1.05 × 10−4 8.89 × 106 0.989 3.10 × 10−4 0.0891 0.996
40 1.13 × 10−4 4.07 × 106 0.994 3.10 × 10−4 0.0891 0.996
50 1.11 × 10−4 7.87 × 106 0.999 3.35 × 10−4 0.0919 0.997

Table 2 Table 3
Comparison of adsorption capacity of various adsorbents Thermodynamic parameters for the adsorption of basic dyes on MCM-22
Dyes Adsorbent Adsorption capacity Reference Dye G0 (kJ/mol) H 0 (kJ/mol) S 0 (J/mol K)
(mol/g) 30◦ 40◦ 50◦
MB AC from coal 1.38 × 10−3 [21] MB −44.1 −44.5 −46.7 5.40 159.3
MB AC-aluminosilicate 3.66 × 10−4 [22] CV −40.3 −40.7 −43.0 1.24 133.9
MB AC from bamboo 4.48 × 10−4 [23] RB −40.3 −39.6 −42.6 4.96 142.3
MB AC from coconut shell 8.70 × 10−4 [23]
MB AC from coconut shell 5.24 × 10−5 [20]
MB AC from coconut husk 2.68 × 10−4 [19] MB, CV, and RB. MCM-22 shows a higher adsorption capacity
MB Natural zeolite 4.50 × 10−5 [9] than natural zeolite and comparable capacity to activated car-
CV AC from coconut husk 1.67 × 10−4 [19] bon.
CV AC from saw dust 8.37 × 10−4 [24]
Thermodynamic parameters, i.e., free energy (G0 ), en-
CV Humid acid-modified pillared clay 1.19 × 10−3 [18]
RB Humid acid-modified pillared clay 8.62 × 10−4 [18] thalpy (H 0 ), and entropy (S 0 ) changes, were also calculated
RB AC from rice husk (0.7–1.0) × 10−3 [25] based on the adsorption isotherms using Eqs. (4)–(6) [20] and
RB Activated charcoal 2.09 × 10−4 [26] are given in Table 3.
RB AC from fertilizer 1.67 × 10−4 [26]
1.80 × 10−4 G0 = −RT ln K1 , (4)
MB MCM-22 [This work]

CV MCM-22 1.20 × 10−4 [This work] T2 T 1 K2
1.10 × 10−4
H 0 = −R ln , (5)
RB MCM-22 [This work] T 2 − T1 K1
H 0 − G0
S 0 = , (6)
process in the adsorption with an endothermic nature, which T
will be discussed in Section 3.3. where K1 and K2 are the Langmuir constants at T1 = 30 and
Table 2 compares the adsorption capacity of MCM-22 with T2 = 50 ◦ C.
activated carbons and other adsorbents reported before. As seen As seen G0 for all cases is negative, which indicates
activated carbon generally has a high adsorption capacity for the feasibility and spontaneous nature of basic dye adsorption
 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78
Fig. 6. Comparison of kinetic models of MB adsorption on MCM-22.
(a) First-order kinetics, (b) second-order kinetics, (c) diffusion model.
on MCM-22. The change in enthalpy (H 0 ) for MB, CV,
and RB was found to be positive. The positive values con-
firm the endothermic nature of adsorption. The positive values
of the entropy change show the increased randomness at the
solid/solution interface with some structural changes in the ad-
sorbate and adsorbent and an affinity of the adsorbent toward
those basic dyes.
3.3. Adsorption kinetics
A study of adsorption kinetics is desirable as it provides
information about the mechanism of adsorption, which is im-
portant for the efficiency of the process. Successful application
of the adsorption demands innovation of cheap, easily avail-
able, and abundant adsorbents of known kinetic parameters and
sorption characteristics. Adsorption kinetics can be modeled by
several models, the pseudo-first-order Lagergren equation [27]
and pseudo-second-order rate equation [28] given below as (7)
and (8), respectively.
k1
log(qe − qt ) = log qe − t,
2.303
75
Fig. 7. Comparison of kinetic models of CV adsorption on MCM-22.
(a) First-order kinetics, (b) second-order kinetics, (c) diffusion model.
t 1 1
= 2
+ t, (8)
qt k 2 qe qe
where k1 is the rate constant of pseudo-first-order adsorption
(h−1 ), k2 (g mol−1 h) the rate constant of pseudo-second-order
adsorption, and qe and qt are amount of dye adsorbed on adsor-
bent (mol g−1 ) at equilibrium and at time t , respectively.
Equation (7) can be transformed into nonlinear forms, which
can be used to predict the adsorption equilibrium:
qt = qe (1 − e−k1 t ). (9)
In addition, the intraparticle diffusion model is a commonly
used technique for identifying the mechanism involved in the
sorption process, which is expressed as
qt = kd (t 1/2 ), (10)
where kd is the diffusion coefficient.
Figs. 6–8 present the plots for the adsorption of three dyes on
MCM-22 using the pseudo-first-order kinetics, pseudo-second-
order kinetics, and diffusion model. As shown the first-order
(7) model does not seem to be good for modeling the kinetics of
76 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78

Table 4
Parameters of kinetic models of basic dye adsorption on MCM-22
Dye Pseudo-first-order model Pseudo-second-order model Diffusion
k1 (h−1 ) qe (mol/g) R2 k2 (g/mol h) qe (mol/g) R2 kd R2
MB 0.5038 1.52 × 10−4 0.854 1247.7 1.70 × 10−4 0.999 3.55 × 10−6 0.964
CV 0.4910 1.01 × 10−4 0.844 2555.1 1.12 × 10−4 0.999 2.42 × 10−6 0.938
RB 0.4449 1.04 × 10−4 0.858 2717.8 1.10 × 10−4 0.999 2.16 × 10−6 0.919

Fig. 9. Corelationship between Bt and t of various dye adsorptions on

MCM-22.

pattern [29,30]. Allen et al. investigated a basic dye adsorp-

Fig. 8. Comparison of kinetic models of RB adsorption on MCM-22.
(a) First-order kinetics, (b) second-order kinetics, (c) diffusion model.
the whole adsorption process and the regression coefficients are
less than those obtained from the second-order kinetics and dif-
fusion model (Table 4). From the results, it is also seen that the
equilibrium adsorption from the pseudo-second-order model is
close to the experimental data, suggesting the better application
of the second-order kinetics. For the diffusion model plots, one
can see that the process involves two phases. The two-phase
plot suggests that the adsorption process proceeds by surface
sorption and intraparticle diffusion. The initial curved portion
of the plot indicated a boundary-layer effect while the sec-
ond linear portion is due to intraparticle or pore diffusion [29].
Several previous investigations have reported a similar type of
tion on peat and attributed the diffusion in the three regions
to macropore diffusion, transitional pore diffusion, and microp-
ore diffusion, respectively [31]. MCM-22 possess two types of
pores and thus presents a two-phase intraparticle diffusion. The
results from Table 4 also show that MB has the highest diffu-
sion coefficient followed by CV and RB, resulting in the highest
adsorption capacity for MB.
In order to determine the actual rate-controlling step in-
volved in the dye sorption process, the sorption data were fur-
ther analyzed using the kinetic expression given by Boyd et al.
[30,32]
6
F =1− exp(−Bt), (11)
π2
where F is the fraction of solute adsorbed at different times t
and Bt is a mathematical function of F and given by
qt
F= , (12)
qe
where qt and qe represent the amount adsorbed (mol/g) at any
time t and at infinite time. In this work, we take qe from the
second-order kinetic model. Substituting Eq. (12) into Eq. (11),
the kinetic expression becomes


qt
Bt = −0.4977 − ln 1 − . (13)
qe
Thus the value of Bt can be calculated for each value of F us-
ing Eq. (13). The calculated Bt values were plotted against time
as shown in Fig. 9. The linearity of this plot will provide use-
ful information for distinguishing between external-transport-
 S. Wang et al. / Journal of Colloid and Interface Science 295 (2006) 71–78 77

Table 5
Parameters of kinetic models of basic dye adsorption on MCM-22
Temperature (◦ C) Dye Pseudo-second-order model
k2 (g/mol h) qe (mol/g) R2
30 MB 1247.7 1.70 × 10−4 0.999
40 1278.8 1.63 × 10−4 0.999
50 1461.8 1.74 × 10−4 0.999
30 CV 2555.1 1.12 × 10−4 0.999
40 2223.9 1.13 × 10−4 0.998
50 2558.9 1.17 × 10−4 0.998
30 RB 2717.8 1.10 × 10−4 0.999
40 6157.65 1.08 × 10−4 0.999
50 4056.0 1.09 × 10−4 0.999

Fig. 10 shows the dynamic adsorption of MB, CV, and RB

on MCM-22 at varying temperatures. As seen the amount of
adsorption for MCM-22 at different temperatures is very close,
which suggests that temperature does not play a significant role
in adsorption, as for the adsorption isotherm. Table 5 presents
the kinetic parameters obtained from the pseudo-second-order
model and it is seen that the equilibrium adsorption capacity
shows a slight increase with the increasing temperature. The
kinetic constants are similar at three temperatures.

4. Conclusion

MCM-22 is an effective adsorbent for basic dye removal

from aqueous solutions. The adsorption capacities for MB,
CV, and RB can reach 1.8 × 10−4 , 1.2 × 10−4 , and 1.1 ×
10−4 mol/g, respectively. The adsorption kinetics follows the
pseudo-second-order model and the external diffusion is the
controlling process. The adsorption isotherms can be well fitted
with Langmuir and Freundlich models. Thermodynamic calcu-
lations indicate that the adsorption of basic dyes on MCM-22
is spontaneous and an endothermic reaction. The H 0 for MB,
CV, and RB is 5.4, 1.2, and 5.0 kJ/mol, respectively.

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