Desalination 256 (2010) 84–89

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Desalination
j o u r n a l h o m e p a g e : w w w. e l s e v i e r. c o m / l o c a t e / d e s a l

Comparison absorption of new methylene blue dye in zeolite and nanocrystal zeolite
Sh. Sohrabnezhad a,⁎, A. Pourahmad b
a
Department of Chemistry, Faculty of Science, University of Mohaghegh Ardabili, Ardabil, Iran
b
Department of Chemistry, Faculty of Science, Islamic Azad University, Rasht Branch, Rasht, Iran

a r t i c l e i n f o a b s t r a c t

Article history: Mordenite and mordenite nanocrystal, were employed as effective adsorbents for new methylene blue
Received 2 August 2009 (NMB) from an aqueous solution. The adsorption kinetics was investigated. The adsorption capacity of
Received in revised form 6 February 2010 mordenite nanocrystal zeolite for NMB dye is more than that of the mordenite zeolite. Kinetic and adsorption
Accepted 8 February 2010
isotherm studies demonstrate that the adsorption follows the pseudo second-order kinetics. The
Available online 1 March 2010
intraparticle diffusion rate coefficient values at 25 °C obtained by using the Morris–Weber equation showed
Keywords:
that new methylene blue reached equilibrium in mordenite nanocrystal faster than in mordenite adsorbent.
Mordenite nanocrystal The effects of equilibrium time, solution pH and sorption temperature were examined. Solution pH will affect
New methylene blue the adsorption behavior of mordenite and mordenite nanocrystal. Higher solution pH results in higher
Dye removal adsorption capacity. The results show that adsorption capacity dye increases in lower temperature.
Adsorption © 2010 Elsevier B.V. All rights reserved.
X-ray diffraction

1. Introduction connected cages and channels containing mobile water molecules

Dyes are extensively used in the textile industry, photocatalytic
industry, coating industry and photochemical application. Treatment
of colored wastewater from textile or other industries is a serious
problem that has attracted the attention of many researchers during
the last decades. In general, the methods for the treatment of
wastewater containing dyes can be divided into two main groups
[1]: (I) chemical or physical methods of dye removal, which refer to
the process called decoloration and (II) dye removal by means of
biodegradation. Physical methods of decoloration include different
precipitation methods, adsorption, filtration, reverse osmosis, etc.
Among the chemical methods of dye removal, there are processes
such as reduction, oxidation, compleximetric methods, ion exchange
and neutralization. Biological treatment can be conducted in the
presence or absence of oxygen [2]. These processes have their
disadvantages and limitations, such as high cost, generation of
secondary pollutants, and poor removal efficiency. Thus adsorption
has been found to be the most effective economic alternative with
high potential for the removal and recovery of dyes from wastewater
[3,4]. Zeolites have already found many applications because of its
high cation-exchange capacity and surface area, etc. Structurally, it is
mainly composed of aluminosilicates with a three-dimensional
framework structure bearing AlO4 and SiO4 tetrahedral that are
linked to each other by sharing of their oxygens to form inter-
⁎ Corresponding author. Tel.: + 98 451 5517137; fax: +98 451 5514024.
E-mail address: sohrabnezhad@uma.ac.ir (S. Sohrabnezhad).
and alkalis and/or alkaline earth [5,6]. Zeolite is a good adsorbent for
heavy metal ions from wastewater [7] and for organic dyes [8,9]. Of
course, mesoporous materials such as MCM-41 and MCM-22 are
widely used as adsorbents for organic dyes. The larger surface area
and good adsorption capacity render these materials very interesting
for adsorption and catalysis [10,11]. All in all, mesoporous materials
(MCM-41 or MCM-22) have a higher adsorption capacity than
microporous zeolites [10,12]. Synthetic zeolites have become increas-
ingly important due to the wide range of their chemical and physical
properties and have been used as adsorbents, molecular sieves,
membranes, ion exchanger and catalysts in the past decades [10].
Meshko et al. [11] have shown that the granular activated carbon has a
higher adsorption capacity than the natural zeolite. But activated
carbons have higher cost in production and regeneration. Therefore,
other adsorbents such as zeolite with higher surface area can be an
alternative. Armagan et al. [13,14] 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
adsorption capacity for reactive dyes. Metes et al. [15] investigated
several synthetic zeolites for cleaning printing ink wastewater and
found that adsorption is independent of pore structure. They showed
that ZSM-5 and NH4-Beta are effective while other zeolites studied
showed a lower efficiency. On the other hand, nanosized zeolites are
important in catalytic and adsorptive applications. Smaller crystals of
zeolites will have larger surface areas and less diffusion limitations
compared to zeolites with micrometer-sized crystal [16]. That was
why we have chosen mordenite nanocrystal zeolite as adsorbent.
In this paper, we report an investigation using mordenite and
mordenite nanocrystal as an adsorbent to remove new methylene blue

0011-9164/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2010.02.009
 S. Sohrabnezhad, A. Pourahmad / Desalination 256 (2010) 84–89
from an aqueous solution. The kinetics and adsorption equilibrium of
the basic dye on synthetic zeolites were investigated. The results show
that, mordenite nanocrystal is an effective adsorbent to remove dye
with respect to mordenite and other micriporous zeolites.
2. Experimental procedures
2.1. Adsorbent and dye
Mordenite zeolite and mordenite nanocrystal were synthesized
hydrothermally following standard procedures reported in literatures
[17,18]. Tetraethylorthosilicate and sodium silicate were selected as a
silicon source for the preparation of mordenite nanocrystal and
mordenite zeolite respectively. Meanwhile, Al powder and Al2SO4
18 H2O were used as source aluminium. The chemical composi-
tions of the mordenite and mordenite nanocrystals gels were
Al2O3:15SiO2:8.5Na2O:1300H2O and Al2O3:30SiO2:6Na2O:780H2O re-
spectively. Then, the reaction mixtures of mordenite nanocrystal and
mordenite zeolite were introduced into a stainless-steel autoclave,
heated to 170 °C for 24 and 72 h respectively, until crystallisation
were completed. After the autoclave was quenched in cold water, the
crystalline products were filtered, washed with water and dried at
110 °C overnight.
A typical dye, new methylene blue (NMB), was selected for
adsorption tests (Scheme 1). It was obtained from Sigma Chemical. A
stock solution with concentration at 10− 4 M was prepared and the
solution for the adsorption test was prepared from the stock solution
to the desired concentration (10− 5).
2.2. Adsorbent characterization
Powder X-ray diffraction patterns of the samples were recorded
using a X'pert diffractometer with Cu Kα radiation (λ = 1.54°A).
UV–visible absorption spectra were recorded using a Shimadzu
1600 PC in the spectral range of 190–900 nm.
The specific surface area and pore volume of the samples were
measured using a Sibata Surface Area Apparatus 1100. All of the
samples were first degassed at 250 °C for 2 h.
The pH of the samples was measured as follows: 0.1 g of the
samples was mixed with 10 mL of distilled water and shaken for 24 h
at 25 °C. After filtration, the pH of the solution was determined by a
pH meter.
2.3. Sorption tests
Adsorption kinetics and isotherm experiments for all samples
were undertaken using a batch equilibrium technique. The adsorption
of the dye was performed by shaking 0.05 g of adsorbent in 200 mL of
the dye solution with an initial concentration of 1.00 × 10− 5 M at
100 rpm at different temperatures. The determination of dye
concentration was done spectrophotometrically on a Shimadzu
1600 PC in the spectral range of 190–900 nm, by measuring the
absorbance at λmax of 632 nm for NMB.
The data obtained from the adsorption tests were then used to
calculate the adsorption capacity, qt (mol g− 1), of the adsorbent by a
Scheme 1. Structure of new methylene blue (NMB).
85
mass-balance relationship, which represents the amount of adsorbed
dye per amount of dry adsorbent,
ðC0 −Ct Þ
qt = V ð1Þ
W
where C0 and Ct are the concentrations of dye in solution (M) at time
t = 0 and t = t, respectively, V is the volume of the solution (dm3), and
W is the mass of the dry absorbent used (g).
2.4. Regeneration of adsorbents
The regeneration of used zeolites was conducted by high
temperature calcinations (HT). In the high temperature calcinations
process, the used adsorbents were set in a furnace with air and
calcined with a heating rate of 5 °C/min from room temperature to
different temperatures and times for burning off the organics and then
stored in a bottle for testing.
3. Results and discussion
3.1. Material characteristics
The XRD profiles of mordenite and mordenite nanocrystal show
quite well with patterns that are given in literatures [16–19] which
allowed to identify the product as crystalline mordenite zeolite. The
specific surface area and pore volume of the mordenite and mordenite
nanocrystal are presented in Table 1. It is seen that the mordenite
nanocrystal zeolite has a surface area of 379 m2 g− 1 while the
mordenite zeolite only has 240 m2 g− 1 (Table 1). The pore volume of
the two adsorbents also demonstrates that mordenite nanocrystal and
mordenite zeolite are microporous materials. It is seen that mordenite
nanocrystal zeolite has a much higher adsorption than mordenite.
The pH of the solid solution indicates that mordenite and mordenite
nanocrystal zeolite exhibit acidic properties.
3.2. Adsorption isotherms
An adsorption isotherm shows how the adsorbate molecules
partition between the liquid and solid phases when the adsorption
process reaches equilibrium conditions. The adsorption isotherm is
fundamental in describing the interactive behavior between solutes
and adsorbent, and is important in the design of adsorption systems
[20]. Several adsorption isotherms are available and two important
isotherms are used in this study. The Langmuir adsorption is based on
the assumption of monolayer adsorption on a structurally homoge-
neous adsorbent, where all the sorption sites are identical and
energetically equivalent and where, the adsorption occurs at specific
homogeneous sites within the adsorbent and once a dye molecule
occupies a site, no further adsorption can take place at that site. The
equation is as follows:
KL qmax Ce
qe = ð2Þ
1 + KL Ce
where qe is the equilibrium dye concentration on adsorbent (mol/g),
Ce is the equilibrium concentration of the dye in solution (mol/l), qmax
is the monolayer adsorption capacity of adsorbent (mol/g). The
Table 1
Physico-chemical properties of mordenite and mordenite nanocrystal zeolite.
Sample SBET Pore volume Pore volume Si/Al pH
(m2/g) (cm3/g) (micro) (cm3/g) (total) ratio
Mordenite 240 0.14 0.16 6 6.5
Mordenite nanocrystal 379 0.18 0.208 15 6.5
86 S. Sohrabnezhad, A. Pourahmad / Desalination 256 (2010) 84–89

Table 2
Isotherm parameters for adsorption of MB onto mordenite and mordenite nanocrystal.

Zeolites Temperature Langmuir isotherm Freundlich isotherm

(°C)
Qmax (mol/g) Kl (l/mol) R2 Kf (mol/g) 1/n R2
−5 6 −4
Mordenite 25 8.18 × 10 1.15 × 10 0.9984 3.18 × 10 0.072 0.997
35 8.08 × 10− 5 1.11 × 106 0.9883 2.98 × 10− 4 0.067 0.987
45 8.02 × 10− 5 1.01 × 106 0.9894 2.28 × 10− 4 0.064 0.965
Mordenite nanocrystal 25 1.24 × 10− 4 9.83 × 106 0.9987 5.28 × 10− 4 0.085 0.998
35 1.14 × 10− 4 4.06 × 106 0.9876 4.38 × 10− 4 0.082 0.988
45 1.08 × 10− 4 4.06 × 106 0.9889 3.88 × 10− 4 0.078 0.976

Langmuir constant (KL) is a measure of the affinity between adsorbate
and adsorbent and related to the free energy of adsorption [10]. A
linear expression for the Langmuir equation is:
Ce 1 C
= + e
qe qmax KL qmax
A plot of Ce/qe versus Ce gives a straight line of slope 1/qmax and
intercepts 1/qmaxKL.
The Freundlich adsorption isotherm is one of the most widely used
empirical equation, which fits with the experimental data over a wide
range of concentrations. The Freundlich isotherm is applicable to
heterogeneous systems and reversible adsorption [21]. This isotherm
is as follows:
qe = KF Ce
1=n
where KF and n are Freundlich adsorption constants, indicative of the
adsorption extent and the degree of nonlinearity between the
solution concentration and adsorption, respectively. The Freundlich
equation in logarithmic form can be given as:
1
log qe = log KF + log Ce
n where the parameter ki is the diffusion coefficient value, t the time and
If n = 1, the adsorption is homogeneous and there is no interaction
between the adsorded species. If 1/n b 1, the adsorption is favored and
new adsorption sites are generated. If 1/n N 1, the adsorption is
unfavourable, bonds become weak and adsorption capacity decreases.
In our studies, we have found that for mordenite nanocrystal 1/n b 1,
which indicates that adsorption is favourable as compared to
mordenite zeolite. The parameters obtained from the experimental
data using the two isotherms and the related correlation coefficients
are presented in Table 2. As seen the adsorption isotherms at different
temperatures for MB dye onto zeolites are very close and can be fitted
very well using two isotherm models (evidenced from the correction
coefficients, N0.990). The decrease in dye adsorption with increasing
temperature might also be due to the decreased rate of the external
and intra-particle diffusions of the adsorbate, as diffusion is a
dominant process in the adsorption with an exothermic nature.
Based on the adsorption constant in the Langmuir isotherm (KL),
thermodynamic parameters (ΔG°, ΔH° and ΔS°) for adsorption of MB
onto mordenite and mordenite nanocrystal zeolites were calculated
using Eqs. (6)–(8) and are given in Table 3.
ΔG - = −RT ln KL ð6Þ
ð3Þ  
T2 T1 K
ΔH - = −R ln L1 ð7Þ
T2− T1 KL2
ΔH -−ΔG -
ΔS - = ð8Þ
T
As can be seen, the adsorption process is spontaneous with the
negative value of ΔG . The standard enthalpy change (ΔH°) for the
adsorption of the MB dye on mordenite and mordenite nanocrystal
zeolites is negative indicating that the process is exothermic in nature
ð4Þ with ΔH° of − 95 and − 98 kJ/mol, respectively.
Most of the adsorption processes may be described by either the
external mass transfer (boundary layer diffusion) or intraparticle
diffusion model. The latter is given by the Weber–Morris equa-
tion [22].
1=2
qt = ki t ð9Þ
ð5Þ
qt is the amount of dye adsorbed. The diffusion coefficient rate values,
ki, obtained from this equation are tabulated in Table 4 for the two
kinds of zeolites at 25 °C. These values are comparable and one can see
that the diffusion rate coefficient of the mordenite nanocrystal is
higher than that of the mordenite zeolite, thus leading it to reach
equilibrium faster.
Table 5 compares the adsorption capacity of mordenite and
mordenite nanocrystal zeolites with activated carbons and other
adsorbents reported before. As seen activated carbon generally has a
high adsorption capacity for MB. Mordenite nanocystal shows a
higher adsorption capacity than natural and synthesis zeolites and
comparable capacity to activated carbon [23–27].
3.3. Comparison of new methylene blue on adsorbents
Fig. 1 presents the dynamic adsorption of NMB on mordenite and
mordenite nanocrystal at an initial concentration of 1.00 × 10− 5 M
and 25 °C. The equilibrium adsorption for NMB on mordenite and
mordenite nanocrystal zeolite were 8 × 10− 5 and 1.2 × 10− 4 mol g− 1,
respectively. From Table 1, it is seen that mordenite nanocrystal
zeolite has a higher surface area and pore volume, which results in

Table 3
Thermodynamic parameters for the adsorption of MB dye on mordenite nanocrystal
Table 4
ans mordenite zeolite.
Diffussion coefficient values for MB dye on mordenite nanocrystal and mordenite
Zeolites ΔG° (Kg/mol) ΔH° (KJ/mol) ΔSº (J/mol K) zeolite at 25° from Morris–Weber equation.

25° 35° 45° Zeolites Ki (mol/g h1/2) R2 t1/2 (min)

−5
Mordenite −34.71 − 33.5 − 32.4 − 95 − 187 Mordenite 4.0 × 10 0.986 1.00
Mordenite nanocrystal − 41.2 −38.9 − 37.2 − 98 − 197 Mordenite nanocrystal 5.0 × 10− 4 0.999 0.87
 S. Sohrabnezhad, A. Pourahmad / Desalination 256 (2010) 84–89 87

Table 5
Comparision of adsorption capacity of various adsorbents.

Dye Adsorbent Adsorption capacity (mol/g) Reference

MB AC from coal 1.38 × 10− 3 [23]

MB AC from coconut husk 2.68 × 10− 4 [24]
MB AC-aluminosilicate 3.66 × 10− 4 [25]
MB Natural zeolite 4.5 × 10− 5 [26]
MB ZSM-5 zeolite 1.9 × 10− 5 [27]
MB Modified-ZSM-5 zeolite 3.88 × 10− 5 [28]
MB Mordenite zeolite 8.0 × 10− 5 [This work]
MB Mordenite nanocrystal 1.2 × 10− 4 [This work]
MB MCM-22 1.8 × 10− 4 [10]
MB AlMCM-41 2.08 × 10− 4 [12]

Fig. 2. Effect of solution pH on NMB adsorption on mordenite nanocrystal zeolite.

higher adsorption capacity. On the other hand, large pores are larger Adsorption conditions: 0.05 g adsorbent, NMB initial concentration: 1.00 × 10− 5 M,
than the NMB molecular size [28] and are all available for NMB temperature: 25 °C.
adsorption, resulting in higher adsorption capacity. But it is close to
NMB molecular size in mordenite zeolite.

3.4. Effect of solution pH

Fig. 2 shows the dynamic adsorption of NMB on mordenite

nanocrystal at three different initial pH values at an initial dye
concentration of 1.00 × 10− 5 M and 25 °C. It is seen that the amount of
adsorption increases as the pH is increased. The adsorption increase
from 1.2 × 10− 4 M to 2.4 × 10− 4 mol g− 1, when solution pH is
changed from 3 to 9. Several investigations also have shown that
dyes have higher adsorption at higher pH values [10,26,27]. For
cationic dyes, lower adsorption of NMB at acidic pH is probably due
to the presence of excess H+ ions competing with the cation groups
on the dye for adsorption sites. As surface charge density decreases
with an increase in the solution pH, the electrostatic repulsion Fig. 3. Effect of solution temperature on NMB on mordenite nanocrystal zeolite.
between the positively charged dye (NMB) and the surface of the Adsorption conditions: NMB initial concentration: 1.00 × 10− 3 M, pH = 6.5.
adsorbent is lowered, which may result in an increase in the extent
of adsorption. temperature can result in an increase in the mobility of the dye ions
but can decrease the interaction of dye with active sites of zeolites. On
3.5. Influence of temperature on NMB adsorption the other hand, increasing temperature may produce a swelling effect
within the internal structure of the zeolites enabling MB dye to exit
Fig. 3 shows the effect of temperature on the adsorption of NMB further from the pores.
onto mordenite nanocrystal and mordenite zeolite. As seen from the
figures, temperature has an effect on NMB adsorption in zeolites. The
3.6. Influence of adsorbent amount used on NMB adsorption
decrease in dye adsorption capacity with increasing temperature
might be due to the dye desorbed of zeolite. Juang et al. have reported
In order to obtain the optimum zeolite amount required for
similar results [29]. For MB dye onto two zeolites, the adsorption at
adsorption at pH 6.5, a series of experiments were undertaken with
45 °C is lower than that at 25 °C, suggesting the exothermic
different amounts of adsorbents in 200 mL of 1.00 × 10− 5 M NMB
characteristic of the adsorption. For the adsorption, the process is
solutions. The NMB concentration was tested after 2 h of shaking at
usually a diffusion process with exothermic property. A higher
25 °C. The zeolite amounts added against adsorbed NMB (mol g− 1)
are shown in Fig. 4. Examination of this figure revealed that the

Fig. 1. Comparison of dynamic adsorption of NMB on mordenite nanocrystal and

mordenite zeolite. Absorption conditions: 0.05 g adsorbent in 200 mL NMB initial Fig. 4. Influence of mordenite nanocrystal zeolite amount on the adsorption amount
concentration 1.00 × 10− 5 M, temperature: 25 °C, pH = 6.5. of NMB.
88 S. Sohrabnezhad, A. Pourahmad / Desalination 256 (2010) 84–89
Table 6
Parameters of kinetic models of NMB adsorption on zeolites.
Adsorbent T Pseudo-
(°C)
K1 (h− 1)
Mordenite 25 0.255
35 0.122
45 0.06
Mordenitenaocrystal 25 0.442
35 0.235
45 0.198
amount of adsorbed dye per amount of adsorbent (mol g− 1),
decreases with increasing amount of zeolites, while the adsorption
rate (%) increased when the amount of adsorbents increased. The
result is comparable to other studies [27]. Because of the necessity of
additional filtration to lower turbidity to the required levels, the
amount of 0.05 g/200 mL has been found as the optimum.
3.7. Adsorption behavior of regeneration adsorbents
The regenerated zeolites by high temperature were tested for MB
adsorption. The high temperature regeneration was conducted at
550 °C for 5 h. The recovered adsorption efficiency is around 75%.
3.8. Adsorption kinetics
A study of adsorption kinetics is desirable as it provides
information about the mechanism of adsorption, which is important
for optimising the efficiency of the process. Adsorption kinetics can be
modelled by several models, the pseudo-first-order Lagergren
equation [30] and pseudo-second-order rate equation [31] given
below in a non-linear form:
−K
qt = qe ð1−e1t Þ
2 estimating the Thomas model parameters for methylene blue adsorption onto
qe K2 t
qt =
ð1 + qe K2 tÞ
where K1 is the rate constant of pseudo-first-order adsorption (h− 1),
K2 (g mol− 1 h− 1) the rate constant of pseudo-second-order adsorption,
qe and qt are the amount of dye adsorbed on the adsorbent (mol g− 1) at
equilibrium and at time respectively.
We used the above two non-linear equations for curve fitting by
employing a commercially available software Sigma Plot. The
parameters of the kinetic models of NMB adsorption on mordenite
and mordenite nanocrystal zeolites are presented in Table 2. The first-
order model seems to be not good in modelling the kinetics of the
whole adsorption process and the regression coefficients are less than
the ones obtained from the second-order-kinetics (Table 6). From the
results, it is also seen that the equilibrium adsorptions from the
pseudo-second-order model are closer to the experimental data than
the ones from the pseudo-first-order kinetics, suggesting the better
fit of the second-order kinetics.
From Table 5, one can also see that the rate constant for the
mordenite nanocrystal zeolite is more than the mordenite zeolite.
4. Conclusion
Mordenite nanocrystal zeolite is an effective adsorbent for new
methylene blue with respect to mordenite zeolite. The adsorption
capacity for NMB in mordenite nanocrystal and mordenite zeolite was
1.2 × 10− 4 and 8 × 10− 5 mol g− 1 at 25 °C, respectively.
Solution pH affects the adsorption behavior of mordenite and
mordenite nanocrystal zeolite. Adsorption capacity increases with
increasing solution pH. The dye adsorption decreases with increasing
First-order Model Pseudo- Second-order Model
qe (mol g− 1) R2 K1 (h− 1) qe (mol g− 1) R2
6.90 × 10− 5 0.891 1347.7 7.90 × 10− 5 0.992
3.18 × 10− 5 0.953 1228.9 3.65 × 10− 5 0.989
1.40 × 10− 5 0.912 1197.5 1.22 × 10− 5 0.989
1.02 × 10− 5 0.933 2587.2 1.18 × 10− 4 0.991
5.10 × 10− 5 0.892 2223.8 5.70 × 10− 5 0.987
2.00 × 10− 5 0.883 1988.2 2.20 × 10− 5 0.992
temperature and optimum temperature was 25 °C. Kinetic analyses
show that the adsorption of dyes on mordenite nanocrystal and
mordenite zeolite follows pseudo-second-order kinetics. The rate
constant for mordenite nanocrystal zeolite was more than the
mordenite zeolite. Further more, the Morris–Weber equation revealed
that the diffusion coefficient values were comparable, and that MB
dye onto mordenite nanocrystal reaches the equilibrium faster than
mordenite zeolite. The adsorption isotherms can be well fitted with
the Langmuir and Freundlich models.
Acknowledgments
We thank the Research Vice Presidency of Islamic Azad University,
Rasht Branch for their encouragement, permission and financial
support and Miss. Arezoo Pourahmad for her aid.
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