Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

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Journal of Industrial and Engineering Chemistry

journal homepage: www.elsevier.com/locate/jiec

Sorption kinetics of sulphate ions on quaternary ammonium-modied

rice straw
Wei Cao a, Zhi Dang b,c,*, Bao-Ling Yuan a, Chun-Hua Shen a, Jin Kan a, Xiu-Ling Xue d
a

College of Civil Engineering, Huaqiao University, Xiamen 361021, PR China

School of Environment and Energy, South China University of Technology, Guangzhou 510006, PR China
c
Key Lab of Pollution Control and Ecosystem Restoration in Industry Clusters, Ministry of Education, Guangzhou 510006, PR China
d
College of Chemical Engineering, Huaqiao University, Xiamen 361021, PR China
b

A R T I C L E I N F O

Article history:
Received 14 April 2013
Accepted 23 October 2013
Available online 1 November 2013
Keywords:
Sulphate ions
Sorption kinetics
Quaternary ammonium modication
Rice straw
Sorption activated energy

A B S T R A C T

Batch sorption experiments with variable concentration of sulphate and temperature were conducted to
investigate sorption kinetics of sulphate ions on quaternary ammonium-modied rice straw (QMRS).
Kinetic data were discussed with pseudo rst- and second-order rate equations and diffusion models.
The results showed the sorption equilibrium time is about 20 min and the activated energy Ea is 19.3 kJ/
mol. Increase of temperature and initial sulphate concentration favored sorption process. The sorption
kinetics followed pseudo second-order rate equation, and the overall rate was determined by lm
diffusion. Additionally, characterization by 13C NMR and EDS conrmed the presence of quaternary
ammonium groups in QMRS.
2013 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights
reserved.

1. Introduction
Sulphate (SO42), as a common anionic ion, exists widely in
natural water and wastewater, such as acid mine drainage, efuent
from chemical industry and so on. The main source of sulphate in
natural water is chemical weathering of sulphur containing
minerals and oxidation of suldes and elemental sulphur [1].
Sulphate is nontoxic, and sulphur is a necessary nutrient element
for many kinds of living systems. However, improper disposal of
sulphate containing wastewater would cause pollution problems
to surrounding environments. High concentrations of sulphate
could break the balance of natural sulphur cycle [2]. It was
reported that excess ingestion of sulphate would bring many
physiological damages to mammals [3,4]. Under anaerobic
conditions, sulphate can be easily reduced to hydrogen sulde
by microorganism (sulphate-reducing bacteria, SRB). Hydrogen
suldes are more dangerous to environmental ecosystem for its
high reactivity, toxicity and corrosivity. Therefore, there is a need
to remove sulphate from industrial wastewater before discharge.
The main methods for sulphate treatment include chemical
precipitation, sorption, biological treatment and membrane

* Corresponding author at: School of Environment and Energy, South China

University of Technology, Guangzhou 510006, PR China. Tel.: +86 20 39380522;
fax: +86 20 39380508.
E-mail address: chzdang@scut.edu.cn (Z. Dang).

separation, among which sorption techniques may be preferred

because of its high selectivity and short time consumption [5].
Sorbent plays a very important role in sorption treatment process.
Ion exchange resins and zirconium oxides are commonly used as
sorbents to remove sulphate ions from aqueous solution.
Unfortunately, they are too expensive to treat large volumes of
wastewater, resulting limitations for application in developing
countries or rural areas. In the past several years, studies showed
that cellulosic agricultural residues as low cost materials could be
used to prepare low cost sorbent for removal of heavy metals and
dyes from water [6,7]. Crop straw such as rice straw and corn stalk
contains many of cellulose, lignin and hemicelluloses, and a little of
extract and mineral residues. To prepare sorbent for anionic
species, modication of cellulose, especially the grafting of cationic
monomers to the cellulose backbone was considered. Dimethylamine and diethylamine were selected to introduce amino groups
into cellulosic materials in recent reports [810]. In fact, among
nitrogen-containing monomers, quaternary ammonium is a strong
cationic group, which may imply an even better adsorption for
sulphate anions. In our previous work, a quaternary ammoniummodied rice straw (QMRS) was prepared and this new type
sorbent exhibited a good sorption capacity for sulphate anions
from water [11].
Despite many studies of the lignocelluloses-based sorbents
published in this area, only a few have been investigated about the
anionic sorbent from crop straw [810,12,13], and even fewer
about the sorption kinetics of quaternary ammonium modied

1226-086X/$ see front matter 2013 The Korean Society of Industrial and Engineering Chemistry. Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.jiec.2013.10.047

2604

W. Cao et al. / Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

lignocelluloses [9,10]. The sorption rate also plays an important

role in sorption technology. Rapid sorption is signicant to
minimize the consumption of time and cost in wastewater
treatment. It is very necessary to understand the sorption kinetics
of the quaternary ammonium modied lignocelluloses. Therefore,
the present study focuses on the sorption kinetics of sulphate
anions on the QMRS. Sorption experiments were carried out with
variable concentrations of sulphate and temperatures. The data
were analyzed with pseudo rst- and second-order rate equations,
and especially a mathematical model developed by Reichenberg
and Boyd [14,15] was used to determine lm diffusion and particle
diffusion controlled sorption

contained more nitrogen element (2.75%) in contrast with raw

rice straw (0.45%). Further, in this study, the cross polarization/
magic angle spinning (CP/MAS) 13C solid-state NMR were
employed in order to conrm the presence of quaternary
ammonium groups of QMRS. The experiments were performed
on a Bruker AVANCE 400 spectrometer with static eld strength of
2.3 T (100 MHz 1H) at 298 K. The proton 908 pulse time was 5.5 ms.
The acquisition time was 0.0304 s and the delay time after
acquisition of signals was 3Ys. The surface element content of raw
and modied rice straw was analyzed by using energy dispersive
spectroscopy (S3700N, Hitachi Limited, Japan).
2.4. Sorption kinetic experiments

2. Materials and methods

2.1. Materials and chemical reagents
Rice straw was obtained from the countryside around
Guangzhou, China. Raw rice straw was washed with tap water
and with deionized water. Then it was shattered and sieved to
obtain particles in range of 0.20.9 mm (8020 mesh). These straw
particles will be used as raw materials to prepare QMRS.
Trimethylamine water solution and epichlorohydrin used in this
work were bought from Sinopharm Chemical Reagent Co. Ltd
(Shanghai, China). The stock solution of sulphate anion was
prepared by dissolving certain weight dried sodium sulphate
(Na2SO4) in deionized water. Sulphate anion solutions with
required concentrations were diluted from this stock solution.
The pH of solution was adjusted with 0.1 M sodium hydroxide
(NaOH) and 0.1 M hydrochloric acid (HCl) solution. All the
chemicals are analytical grade.
2.2. Preparation of QMRS
Six-gram virginal rice straw particles were rstly treated with
10% (w/v) NaOH solution at room temperature for 2 h to expose
cellulose and to form sodium cellulose. Secondly, the alkali
treated rice straw was reacted with 60 mL epichlorohydrin in a
three-neck ask for 6 h at 65 8C to obtain epoxypropyl-cellulose.
The excess epichlorohydrin was removed from reaction system
by ltration. Thirdly, 60 mL 33% trimethylamine water solution
was added into the ask and reacted for 3 h at 80 8C to introduce
quaternary ammonium groups into rice straw. The product was
washed with 1:1 ethanol, 0.1 M HCl solution, and deionized
water to convert it into chlorine resident form. After being dried
at 60 8C, the dried product as quaternary ammonium modied
rice straw (QMRS) would be used in following sorption
experiments. During modication process, the main chemical
reactions of cellulose from rice straw were simply shown in
formulae (1) and (2).

Sorption kinetic experiments were carried out in a 100 mL

conical ask containing 0.1 g RS-AE and 50 mL sulphate solution.
The asks were put into a thermostat orbital shaker at rotation rate
of 150 rpm and desired temperature (1 K). The pH value of sulphate
solution was 6.8 without any adjustment during experiment process.
The effect of initial concentration on sulphate sorption kinetics was
studied by varying initial sulphate concentration from 50 to 200 mg/L
(50, 100, 150 and 200 mg/L) at temperature of 298 K. While to study the
effect of temperature on sulphate sorption kinetics, experiments were
performed at temperature of 291, 298, 308 and 318 K with 100 mg/L
sulphate initial concentration. The contact time intervals (1, 2, 5, 10, 20,
30, 40, 50, 60, 70, 80 and 90 min) were adopted to obtain sorption
kinetic data. The supernatant liquid in the conical ask was separated
from adsorbent by ltration, and the ltrate was collected for chemical
analysis. Sulphate concentration in this study was measured by ion
chromatography (ICS 900, Dionex Co. Ltd., USA). The samples were at
least duplicated, and the mean values were used.
The sorption amount of sulphate at time t, qt (mg/g), was
calculated from mass balance equation in the following form (3):
C o  C t  V
;
(3)
m
where Co (mg/L) and Ct (mg/L) are in the places of initial sulphate
concentration and sulphate concentration at time t, respectively; V
(0.05YL) is the volume of sorption solution and m (0.1 g) is the mass
of adsorbent.
qt

2.5. Sorption kinetic models

In order to describe sorption process, various overall reaction
rate equations were proposed, such as pseudo rst- and secondorder rate equations. These two models were widely used for
pollutants sorption from wastewater in recent years [1618].
Lagergren proposed the pseudo rst-order equation as follows:
dqt
k p1 qe  qt ;
dt

(4)

(1)

(2)

2.3. Characterization of rice straw and QMRS

To assess the modication efciency and the sorption potential
of QMRS, we have tested the nitrogen content (N%) of the rice straw
before and after being modied. The results showed QMRS

where qe and qt (mg/g) are the sulphate sorption amount at

equilibrium and time t, respectively; kp1 (1/min) is the pseudo
rst-order rate constant [19,20]. After being integrated at the
boundary conditions of qt = 0 at t = 0 and qt = qt at t = t, the pseudo

W. Cao et al. / Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

2605

rst-order equation yields

logqe  qt logqe 

k p1
 t:
2:303

(5)

The pseudo second-order equation was presented as

dqt
k p2 qe  qt 2 ;
dt

(6)

where kp2 (g/(mg min)) is the pseudo second-order rate constant

of sorption process [21,22]. Integrating Eq. (6) with boundary
conditions t = 0 to t = t and qt = 0 to qt = qt, gives
1
1
k p2  t:
qe  qt qe

(7)

Separating the variables qt and t, Eq. (7) was rearranged into a

linear form
1
1
1
1

 :
qt qe k p2  q2E t

(8)

The plot of 1/qt to 1/t should be a straight line if the sorption

kinetics follows pseudo second-order rate equation. In this study,
the linear form of pseudo rst- and second-order models (Eqs. (5)
and (8)) will be used to t the sorption kinetic data of sulphate on
QMRS.
3. Results and discussion
3.1. Characterization of sorbents
Fig. 1 shows the CP/MAS 13C NMR spectra of raw rice straw and
QMRS. The main signals in both raw rice straw and QMRS are
consistent with that of native cellulose. The signals at 105 ppm
arise from C-1 of cellulose. The signals at 84 and 89 ppm are
attributed to C-4 of amorphous cellulose and crystalline cellulose,
respectively; and the signal from 72 to 75 ppm is related to C-2, C-3
and C-5 [2325]. These results suggest the structural skeleton of
QMRS is native cellulose. Compared to the 13C NMR spectra of raw
rice straw and QMRS, the largest difference is a new sharp peak at
55.6 ppm observed in the spectrum of QMRS. This signal is
attributed to the carbon atom combined to quaternary ammonium
(CN(CH3)3) [26,27]. The presence of this signal at 55.6 ppm
provides evidence to the existence of quaternary ammonium
groups in QMRS. In addition, the results of EDS analysis (Fig. 2)
also showed nitrogen content (%) of rice straw highly increased
after quaternary ammonium modication. The main elemental
composition of raw rice straw and QMRS were 25.78% C, 66.21% O,
6.49% Si, and 31.29% C, 3.67% N, 60.61% O, 1.64% Si, 2.78% Cl,

Fig. 1. The

13

C NMR spectra of raw rice straw and QMRS.

Fig. 2. The EDS analysis of rice straw before and after modication.

respectively. Quaternary ammonium, as a strong basic group, is

positively charged in aqueous solution and it could bind negatively
charged species through electrostatic attraction [10,28,29]. Therefore, the formation of quaternary ammonium groups could highly
improve the sorption of anionic sulphate by QMRS.
3.2. Sorption kinetics with different initial sulphate concentration
The variations of sulphate sorption amount with contact time
under different initial sulphate concentrations were shown in
Fig. 3a. The sorption amount qt increases fast within initial 20 min,
and then its growth slows down. Accordingly, the sorption process
can be divided into two stages, the rapid increase stage and the
slow increase stage, which was also called near equilibrium stage
[30]. The rapid increase stage is possibly derived by electrostatic
force between SO42 and active sorption sites (quaternary
ammonium groups) on the surface of QMRS [11]. The slow near
equilibrium stage may be resulted from the decrease of electrostatic
attraction after the adsorbent being saturated by SO42 anions. It
also can be seen that the equilibrium sorption capacity (qe) of
sulphate on QMRS is enhanced as initial sulphate concentration
increases from 50 to 200 mg/L.
The experimental data are analyzed with pseudo rst- and
second-order sorption kinetic models, and the results are plotted in
Fig. 3b and c, respectively. The calculated parameters of the two
kinetic models are presented in Table 1. The correlation
coefcients of pseudo second-order equation are greater than
that of pseudo rst-order. The experimental equilibrium sorption
amounts (qe,Exp) agree perfectly with the theoretical values (qe, Cal)
calculated from pseudo second-order equation. Nevertheless, qe,Exp

W. Cao et al. / Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

2606

Table 1
The parameters of pseudo rst- and second-order kinetic models for sulphate sorption on QMRS under different initial sulphate concentration.
C0 (mg/L)

50
100
150
200

qe,Exp (mg/g)

24.2
46.8
72.4
74.8

Pseudo rst-order equation

Pseudo second-order equation

qe,Cal (mg/g)

kp1 (1/min)

qe,Cal (mg/g)

kp2 (g/(mg min))

R2

12.1
26.6
44.8
46.9

0.0610
0.0829
0.0949
0.117

0.927
0.943
0.986
0.960

26.9
44.4
73.6
74.6

0.0111
0.0113
0.016
0.0124

0.998
0.996
0.995
0.996

deviates considerably from that of pseudo rst-order rate

equation. These results suggest that sulphate sorption on QMRS
follows pseudo second-order kinetic models, and the sorption rate
is proportional to the square of sorption driving force (qe qt).
From the variation of the pseudo second-order rate constant kp2, it
can be seen that the pseudo second order rate constant kp2 is
enhanced as the initial sulphate concentration increase from 50 to
200 mg/L. This result indicates that increase of initial sulphate
concentration accelerates the sorption of sulphate on QMRS. To
understand this phenomenon, collision theory of chemical reaction
perhaps should be considered. According to reaction collision
theory, the reaction rate is proportional to activated collision
fraction [31]. Increase of initial sulphate concentration improves
the possibility of activated collision between sorbate (SO42) and
sorption site. Therefore, the sorption rate of sulphate is enhanced
with initial sulphate concentration.
3.3. Sorption kinetics at different temperature
The sorption kinetics of sulphate on QMRS at 291 K, 298 K,
308 K and 318 K are plotted in Fig. 4. From Fig. 4a, it nds that the
sorption amount of sulphate increases with contact time, and a
large fraction of sulphate is removed in the rst 20 min, which
was called rapid increase stage in above. Then the sorption amount
of sulphate reached a limit value in the left time called near
equilibrium stage. From Fig. 4a, we also can see that the
equilibrium sorption amount of sulphate is slightly improved
with increase of sorption temperature. It preliminarily shows that
increase of temperature facilitates the sorption of sulphate on
QMRS.
The sorption kinetic curves at different temperature are
also analyzed with pseudo rst- and second-order sorption
rate equations. The related parameters of kinetic models are
presented in Table 2. From Fig. 4b, it can be seen that pseudo rstorder equation is not applicable with the entire contact time of
sulphate sorption on QMRS. Fig. 4c shows that the experimental
plots agree well with pseudo second-order kinetic equation, of
which the correlation coefcient is much greater than that of
pseudo rst-order kinetic equation. These results conrm the
sorption kinetics of sulphate anions on QMRS follows pseudosecond order kinetic model. From Table 2, it can also be seen that
the pseudo second-order rate constant kp2 increases with the
enhancement of sorption temperature from 291 K to 318 K. It
suggests the increase of temperature can accelerate the sorption
of sulphate on QMRS.

3.4. Sorption activation energy Ea

It is known that the temperature dependence of the rate of most
chemical reactions can be t successfully with Arrhenius equation
[32]. So the activation energy Ea of the sorption of sulphate anion is
evaluated by using the linearized Arrhenius equation in the
following form [33]:
lnk lnA 

Ea
RT

(9)

where Ea is the sorption activation energy (kJ/mol); k is the

sorption rate constant A is the Arrhenius constant; R (8.314 J/
(K mol)) and T (K) were the ideal gas constant and Kelvin
temperature, respectively. The sorption of sulphate anion on
QMRS follows pseudo second-order kinetic model, so here the
sorption rate constant k is replaced by pseudo second-order rate
constant kp2. The magnitude of activation energy was often used
to distinguish physical sorption and chemical sorption. The
energy requirement for physical sorption usually is no more than
4.2 kJ/mol since the forces involved in physical sorption are weak
[34,35]. Chemical sorption involves chemical bond force, which is
much stronger than that of physical sorption. The rate for activated
chemical sorption varies with temperature according to a nite
activation energy from 8.4 to 83.7 kJ/mol [36].
The activation energy Ea for sorption of sulphate anion on QMRS
is 19.3 kJ/mol, which is calculated from the slope of corresponding
ln kp2 versus 1/T (shown in Fig. 5). This result suggests that the
sorption of sulphate anion mainly involves chemical sorption
mechanism. The positive value of Ea indicates that the sorption is
an endothermal process and the rise of temperature can accelerate
its occurrence. Furthermore, the magnitude of activation energy
also gives information about whether the sorption rate is governed
by the sorption reaction or the by the diffusion process. The Ea of
diffusion controlled sorption process is usually less than 25 kJ/mol,
while reaction kinetics controlled sorption process is greater than
30 kJ/mol [33,35,37]. Therefore, the rate of sulphate sorption by
QMRS is possibly controlled by diffusion process of SO42. Whether
the sorption rate is controlled by lm diffusion or by particle
diffusion needs deeper analysis.
3.5. Film diffusion and particle diffusion
The sorption process in liquid system usually includes three
consecutive steps according to previous studies [38,39]: (1)
transport of the adsorbate to penetrate the boundary lm

Table 2
Parameters of pseudo rst- and second-order kinetic models for sulphate sorption on QMRS at different temperature.
T (K)

291
298
308
318

qe,Exp (mg/g)

41.2
46.8
48.1
48.8

Pseudo rst-order equation

Pseudo second-order equation

2

qe,Cal (mg/g)

kp1 (1/min)

qe,Cal (mg/g)

kp2 (g/(mg min))

R2

28.8
26.6
27.4
25.4

0.0759
0.0829
0.0997
0.108

0.986
0.943
0.978
0.959

42.4
44.4
47.8
48.5

0.00856
0.0113
0.0142
0.0169

0.979
0.996
0.999
0.995

W. Cao et al. / Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

Fig. 3. Sorption kinetics of sulphate on QMRS under different initial sulphate

concentration: (a) experimental plots; (b) pseudo rst-order kinetic plots; (c)
pseudo second-order plots (conditions: pH 6.8; temperature = 298YK; sorbent
dose = 2Yg/L).

surrounding the sorbent and to reach the external surface of the

sorbent (lm diffusion); (2) transport of the adsorbate from the
external surface to the active sorption sites existing on the internal
surface of the sorbent (particle diffusion); (3) sorption reaction
between the adsorbate and the active sorption site. For an ion
exchange process, the transport of ions being exchanged should be

2607

Fig. 4. Sorption kinetics of sulphate on QMRS at different temperature: (a)

experimental plots; (b) pseudo rst-order kinetic plots; (c) pseudo second-order
plots (conditions: pH 6.8; initial sulphate concentration = 100Ymg/L; sorbent
dose = 2Yg/L).

considered because they also affect the rate of the sorption process.
Generally, sorption or ion exchange reaction (step (3)) is so rapid
that it does not represent the limiting step of overall sorption rate.
Therefore, the overall sorption rate is determined by lm diffusion

2608

W. Cao et al. / Journal of Industrial and Engineering Chemistry 20 (2014) 26032609

(step (1)), otherwise by particle diffusion (step (2)). A mathematical model of Eqs. (10)(12) has been developed and used to
distinguish between the lm diffusion and particle diffusion
controlled sorption [14,18,38,40,41].
F 1

Fig. 5. Arrhenius plots for the sorption of sulphate on QMRS.

1
6 X
expn2 Bt
;
n2
p2 n1

qt
;
qe

p2 Di
r2

(10)

(11)

(12)

where F is the fractional attainment of equilibrium at time t and it

is calculated as the ratio of the sorption amount at time t and at
equilibrium. B is a time constant determined by the effective
diffusion coefcient Di and the radius r of the sorbent particle. The
n means an integer, which denes the innite series solution.
The linearity test of Bt versus t can be used to distinguish
whether the lm diffusion or the particle diffusion controls the
sorption rate. If the plot of Bt vs. t is a straight line passing through
the origin, then the sorption rate is controlled by particle diffusion
mechanism otherwise by lm diffusion mechanism. Bt values at
each observed F can be obtained from Reichenbergs table [14].
Fig. 6 shows the Bt plots vs. time for sulphate sorption on QMRS at
different temperature and concentration. It can be seen, under all
experimental conditions, the Bt vs. time plots do not pass through
the origin. The results indicate that sorption rate of sulphate by
QMRS is controlled by the lm diffusion of sulphate ions. It also
should be noticed that, under lower initial sulphate concentration
and lower temperature, the plot is linear and nearly passes though
the origin. Perhaps, we can infer that particle diffusion of SO42 will
turn to be the rate limiting process when the initial sulphate
concentration and the sorption temperature are decreased to some
extent.
4. Conclusion
The sorption of sulphate anions by QMRS is fast and the
equilibrium time is about 20 min, which is an advantage for
continuous treatment of wastewater containing sulphate. The
sorption kinetics of sulphate on QMRS follows pseudo secondorder rate equation, and an increase of initial sulphate concentration and sorption temperature facilitates the sorption. The sorption
activated energy Ea is 19.3 kJ/mol indicating that sulphate sorption
is an endothermic and chemical sorption process. Under experimental conditions, the over sorption rate is controlled by lm
diffusion of sulphate anions. In addition, the 13C NMR spectrum of
QMRS conrms the presence of quaternary ammonium groups as
functional groups in QMRS.
Acknowledgements
This work was nancially supported by the National Natural
Science Foundation of China (Nos. 41073088 and 21207043), and
the Starting Scientic Research Fund for Imported Talents of
Huaqiao University (No. 12BS211), and the Key Lab of Pollution
Control and Ecosystem Restoration in Industry Clusters, Ministry
of Education, China.
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Fig. 6. Bt vs. time plots for sorption of sulphate anion on QMRS under different initial
sulphate concentration (a) and different temperature (b).

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