Removal of Toxic Heavy Metal Ions from Aqueous Solutions

Using Jute Fibers Grafted With Acrylic acid by Gamma

Irradiation

Mahmoud S. Hassan , Maged H. Zohdy

Department of Radiation Chemistry, National Center for Radiation Research and Technology, Atomic Energy
Authority, Cairo, Egypt

Jute fibers were grafted with acrylic acid by using the
direct gamma irradiation technique, which used as an
adsorbent substrate for the toxic heavy metal ions
such as Hg21 and Pb21 from their aqueous solutions.
The structure and crystallinity of the grafted jute fibers
were characterized by using Fourier-transform infrared
spectroscopy and X-ray diffraction, respectively. The
effect of pH range of the metal ion solutions, contact
time, and the adsorption kinetics of the adsorption
process were investigated. The effect of the initial con-
centration of dissolved metal ions and the adsorption
isotherm for both Langmuir and Freundlich adsorption
models were also investigated. From the results, it can
be concluded that the adsorption process obeys the
second-order kinetic reaction and follows the Lang-
muir adsorption isotherm model, while, about 86 and
80% of Pb21 and Hg21, respectively, were adsorbed at
pH 5 and 6 after a contact time of 60 min. J. VINYL
ADDIT. TECHNOL., 00:000–000, 2017. V
C 2017 Society of Plas-
tics Engineers
INTRODUCTION
Heavy metal pollution can cause serious environmental
problems as a result of their toxicity and carcinogenic
effects on the natural environment and its accumulation
in living organisms [1]. The toxicity of heavy metals
might be caused by blocking essential functional groups
of biomolecules and by disrupting the integrity of bio-
membranes [2]. Mercury and lead are from the most
famous toxic heavy metals, which are responsible for the
water pollution from industrial effluents.
Mercury pollution usually comes from different indus-
tries such as chloroalkali, paint, pharmaceutical, pulp, and
paper. Lead pollution comes as a result of the batteries’
storage and plating industries [3]. The increase in lead
concentrations in the drinking water can affect the mental
development of children and can increase the blood pres-
sure in adults. On the other hand, the presence of mercury
Correspondence to: M. S. Hassan; e-mail: mah5moud@hotmail.com
DOI 10.1002/vnl.21603
Published online in Wiley Online Library (wileyonlinelibrary.com).
C 2017 Society of Plastics Engineers
V of cellulose, hemicellulose (82–85%), and lignin [20]. It
in water with higher quantities can damage of the central
nervous system and chromosomes and can cause the chest
pain [4]. Because of increased environmental awareness,
the development of cost-effective methods for the
removal of lead and mercury from aqueous solutions has
gained great importance. Different techniques were used
to remove the undesirable dissolved heavy metal ions
from aqueous solutions. The conventional techniques such
as chemical precipitation, ion exchange, reverse osmosis,
membrane separation, and electrochemical treatment pro-
cesses [5–7], although, these techniques are often costly
or ineffective, especially in removing heavy metal ions at
low Concentrations [8], whereas the adsorption methods
are more effective for removing the undesirable heavy
metals without producing unwanted by-products. Different
materials such as activated carbon [9], carboxylated cellu-
lose nanocrystals [10], fly ash [11], soy protein hollow
microspheres [12], sawdust [13], polyrhodanine-
encapsulated magnetic nanoparticles [14], and chitosan
entrapped CM-cellulose hydrogels [7], were used as
adsorbents. Moreover, the grafted substrates with poly(a-
crylic acid) have a characteristic chelating ability toward
different divalent metal ions [15, 16].
The irradiation technique is known to be an effective
technique for changing the properties of matters. The
graft copolymerization by using the direct irradiation
technique was used over the past decades for polymer
treatments, in which, new side chains could be introduced
to the polymer backbone by covalent bonding [17–19]. In
this regard, the radiation was used to induce the graft
copolymerization process to produce high performance
chemically active polymer materials for adsorption and
separation processes. For example, the grafting process
with poly (acrylic acid), which acts as a chelating poly-
mer, has a considerable attention in the separation of
heavy metals due to its ability to form chelates [15].
Jute is one of the most affordable natural fibers and is
the second to cotton in amount produced and variety of
its raw material extracted from vegetable fibers. Jute
fibers are lignocelluloses natural fibers, composed mainly

JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017

is also cheap, contains huge interspaces, and can be used
easily as a wastewater effluent filtration. On the other
hand, jute fibers are known for its durability, and eco-
friendly properties, so that they are ideal for the different
adsorption applications.
The present work deals with the preparation and char-
acterization of jute fibers grafted with acrylic acid (AAc)
monomer by using the mutual gamma radiation technique,
which used as an adsorbent substrate for some toxic
heavy metal ions such as Pb21 and Hg21. The grafted
jute fibers were characterized by using Fourier-transform
infrared spectroscopy (FTIR) and X-ray diffraction
(XRD). The effect of different parameters on the adsorp-
tion capacity (mg/g) of grafted jute fibers toward Pb21
and Hg21 such as contact time, pH range, and the initial
concentrations of the metal ions solutions was investi-
gated. The kinetic parameters and the adsorption isotherm
of the adsorption process were also investigated.
EXPERIMENTAL AND TECHNIQUES
Materials
AAc was used as received, and it was supplied by
Fluka. Jute fibers were supplied by the Egyptian Com-
pany for Jute Production, Egypt. Ammonium hydroxide,
ammonium chloride, sodium hydroxide, EDTA, and gla-
cial acetic acid were supplied by El-Nasr Pharmaceutical
Chemicals Co., Egypt. Lead nitrate [Pb(NO3)2] (Mwt;
331.2) and mercuric chloride [HgCl2] (Mwt; 271.52) were
supplied by Alpha Chemika Co., India.
Grafting of Jute Fibers with AAc
Jute fibers were swelled for 24 h in NaOH solution
(20%), washed, neutralized with diluted acetic acid, dried,
and then they were weighted (Wo). For the grafting pro-
cess, the swelled jute fibers were immersed in glass tubes
containing AAc monomer with different concentrations
(under investigation), solvent and ferrous ammonium sul-
fate as an inhibitor for the homopolymer formation, then
gamma irradiated at different doses using 60Co gamma
cell of dose rate 2.5 kGy/h (made in India) installed at
the National Center for Radiation Research and Technol-
ogy, Cairo, Egypt. The grafted fibers were then washed
to extract the residual monomer and homopolymer. The
homogenous grafted samples were dried and weighed
(Wg). The graft yield (%) was calculated according to
 
Graft yield ð%Þ5 ðWg – Wo Þ=Wo 3100 (1)
Characterization of Grafted Jute Fibers with PAAc
The prepared jute fibers grafted with PAAc (Jute-g-
PAAc) were analyzed using FTIR, in a wide range
wavenumbers (400–4000 cm21), and in solid state using
Mattson 5000 FTIR spectrometer (Mattson Instruments,
2 JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017
Madison, WI). XRD studies were performed using Philips
(PW 1390) equipment and Nickel-filtered Cu-Ka radia-
tion. A scanning electron microscopy (SEM) study of the
prepared jute fibers was carried out by JSM-640, JEOL at
15 kV, in which the dried sample was sputter-coated with
gold using a microscope sputter coater and viewed
through the microscope.
Determination of Metal Ions Adsorption Capacity by
Jute-g-PAAc
The adsorption capacities of jute fibers towards the dif-
ferent metal ions were determined. A constant weight of
dry treated jute fibers (0.2 g) was immersed in a 50 ml
metal salt solution from HgCl2 or Pb(NO3)2 at the initial
concentration of 27.15 and 33.12 (g/L), respectively, which
equivalent of (0.1 M) for both of them, under shaking. The
remaining metal ion concentrations were determined by
using standard solution of EDTA [21]. The adsorption
capacity, the amount of ions adsorbed per mass unit of
treated jute fibers q (mg/g), was calculated using
q 5 ðCo – Ce Þ V=W; (2)
where Co and Ce are the initial and equilibrium metal ion
solution concentrations (mg/L), respectively, W is the
weight of treated Jute fibers (g), and V is the volume of
metal salt solution (L).
RESULTS AND DISCUSSION
Graft Copolymerization of Jute-g-PAAc
Jute fiber is known to be stiff fiber with rough textured
surface, with high crystalline proportion as a result of the
high lignin percent and hemicellulose ratios. To overcome
this drawback, the alkali impregnation of the fibers was
used as a pretreatment, to decrease the crystalline fraction
related to the amorphous portion. This consequently leads
to the increase in the chemical reaction possibilities of
the jute fibers [22, 23]. In the grafting of individual
monomers by radiation, it is easy to control the grafting
process by controlling the factors affecting the graft yield
(%). From the previous works, it was found that the graft-
ing solution, which have an effective role in the grafting
process as a swelling medium for jute fibers and as a dil-
uent for AAc monomer [24], was preferred to be included
H2O/MeOH (90:10) in the presence of 0.1% of ammo-
nium ferrous sulphate as inhibitor for homopolymer for-
mation. The effect of irradiation dose and monomer
concentration on the obtained graft yield (%) was investi-
gated as shown in Fig. 1. The results showed that the
grafting yield (%) increases with increasing of the irradia-
tion dose, as a result of the free radicals formation, which
leads to the increase in the grafting yield (%) [25]. It was
found also that the grafting yield (%) increases with
increasing of the AAc monomer concentration up to 30%,
then by increasing AAc monomer concentration more
than 30%, the grafting yield (%) slightly increased, or
DOI 10.1002/vnl
FIG. 1. Effect of (a) AAc concentration and (b) irradiation dose on the graft yield (%) of PAAc onto jute fibers at constant solvent composition
(H2O/MeOH; 90/10) and am. ferr. sulfate (0.1%).
tends to level off as a result of homopolymer formation
of PAAc [26].
Characterization of Jute-g-PAAc
Fourier-Transform Infrared. FTIR spectroscopic anal-
ysis was used to confirm the formation of graft copoly-
merization of PAAc onto Jute fibers. Figure 2 shows the
IR spectra of ungrafted and grafted jute fibers with PAAc
(28% grafting yield). The FTIR spectrum of jute fibers
before grafting, as an example of cellulosic materials,
showed a characteristic absorption band at 3448 cm21
assigned to the stretching vibration of –OH, the vibration
band at 2923 cm21 confirms the presence of C–H stretch-
ing, the vibration band at 1650–1640 cm21 due to the
water associated with cellulose. In addition, absorption
bands at 1375–1320 and at 1047–1004 cm21 confirm the
presence of C–H bending of cellulose and the stretching
vibration of C–O, respectively. On the other hand, the
FTIR spectrum of Jute-g-PAAc showed that the same
characteristic vibration bands of jute fibers were found
beside new characteristic absorbed bands for –CO of car-
boxylic acid at 1320–1210 cm21, –C5O of carboxylic
acid at 1720–1700 cm21, accompanied with an increase
in –OH broad band of carboxylic acid at 3448 cm21.
FIG. 2. FTIR spectra of ungrafted jute and Jute-g-PAAc fibers.
DOI 10.1002/vnl
These findings prove the introduction of PAAc grafted
chains onto the backbone of jute fibers [27].
X-ray Diffraction. The XRD patterns of ungrafted jute
and Jute-g-PAAc are shown in Fig. 3. The jute fibers
showed a definite characteristic peak at 2h 5 22.458 with
high intensity (908 kcps), which reflects the high crys-
tallinity nature of the jute fibers, due to the presence of
the crystalline lignin with high portion (80%) in the
Jute fiber composition [22]. On the other hand, the Jute-
g-PAAc fibers showed the same characteristic peak of the
jute fibers with lower intensity (620 kcps), which indi-
cates that the crystallinity of the jute fibers was decreased
after the incorporation of the PAAc, which characterized
with its amorphous nature [28] into the jute matrix, result-
ing in the lowering in the overall crystallinity of the
grafted jute fibers.
Scanning Electron Microscopy. The SEM was used to
compare the differences in the surface morphology and
the physical appearance of ungrafted jute fibers and Jute-
g-PAAc as shown in Fig. 4. The SEM micrographs of
ungrafted jute fibers showed the smooth crystalline
FIG. 3. XRD patterns of ungrafted jute and Jute-g-PAAc fibers.
JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017 3
 FIG. 4. SEM micrographs of (a) ungrafted jute and (b) Jute-g-PAAc fibers.
appearance as shown in Fig. 4a. After the grafting process
with PAAc, thick spongy layers of the graft copolymer
were noticed on the jute surface resulting in the increase
in the diameter of fibers with uniform shape as shown in
Fig. 4b, which can enhance the effluent diffusion through
the fiber interspaces leading to the increasing of the
adsorption efficiency.
Adsorption Mechanism of Metal Ions by Jute-g-
PAAc. The mechanism of the metal ion adsorption pro-
cesses is not fully understood, but several mechanisms
were suggested for metal ion binding to the grafted poly-
mer chains including ion exchange, complexation, co-
ordination/chelation, electrostatic interactions, acid–base
interactions, hydrogen bonding, hydrophobic interactions,
physisorption, and possibly precipitation. In the case of
Jute-g-PAAc, the hydrogen atom in the carboxylic group
of AAc can be exchanged by metal ion and then the car-
boxyl groups have two lone pair of electrons on the oxy-
gen which can form a chelate with metal ion [29]. Two
carboxyl groups are required to form a chelate with diva-
lent metal ions. The Jute-g-PAAc was used as an adsor-
bent matrix for some toxic divalent heavy metal ions
such as Pb21 and Hg21. Previous reports [30] proved that
the carboxylic groups of AAc act as a strong complexing
agent for the metal ions as shown in Eqs. 3 and 4. This
complex shows a tetrahedral structure (square planar com-
plex) as shown in the following scheme.
2Jute-g-COO2 1Pb21 ! ½Jute-g-COO2 Pb ðcomplexÞ
4 JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017
2Jute-g-COO2 1Hg21 ! ½Jute-g-COO2 Hg ðcomplexÞ (4)
Effect of pH. The removal (%) of metal ions by the
adsorbent as a function of pH, using of (0.1 M) as an ini-
tial concentration for both metal salts, at a temperature of
308C, after 60 min of soaking under shaking is repre-
sented in Fig. 5. It is clear that the removal (%) of metal
ions is strongly pH dependent and maximum removal (%)
occurs at pH 5 for lead and pH 6 for mercury. The
increase of metal ion removal (%) with an increase in the
pH is due to a decrease in competition between proton
and metal ions for the surface sites and by the decrease in
positive surface charge. Meanwhile, the metal ion
removal (%) was decreased at low pH values as a result
of the protonation effect and the increasing competition
of protons for the same binding sites that metal ions can
bind. A slight decrease in removal (%) observed above
pH 5 for lead, which may be due to the precipitation of
Pb21 as Pb(OH)2. Hence pH experiments at alkaline
ranges were avoided. The maximum removal (%) of
Hg21 observed at higher pH (6) than that of Pb21 may be
attributed to the electrostatic attraction between Hg(OH)1
ions and the negatively charged adsorbent surface [31].
Effect of Contact Time. The effect of contact time on
the removal (%) of Pb21 and Hg21 by Jute-g-PAAc fibers
using the initial concentration of (0.1 M) at pH 5 and a
temperature of 308C was studied, and the results are rep-
resented in Fig. 6. It can be seen that the removal (%) of
FIG. 5. Effect of pH on the removal (%) of Pb21 and Hg21 by Jute-g-
(3) PAAc after 60 min, using the initial concentration of (0.1 M) of both
metal ion solutions.
DOI 10.1002/vnl
 TABLE 1. Adsorption kinetic parameters.

Pseudo-first-order Pseudo-second-order
kinetic model kinetic model
Metal ions k1 (min21) qe (mg/g) r2 k2 [g/(mg/min)] qe (mg/g) r2

Pb21 0.07 1.19 0.79 0.03 22 1.00

Hg21 0.07 1.16 0.79 0.02 20.75 1.00

log ðqe 2qt Þ5log qe –k1 =2:303t (5)

FIG. 6. Effect of contact time on the removal (%) of Pb21 and Hg21
by Jute-g-PAAc at pH 5, using initial concentration of (0.1 M) of both
metal ion solutions.
Jute-g-PAAc toward Pb21 and Hg21 increased signifi-
cantly after 10 min, and it tended to increase with lower
rate with increasing the time up to 60 min. Above 60
min, the removal (%) tended to level off. The rapid
removal (%) in the initial stage was due to the abundant
available chelating PAAc sites on the surface of grafted
Jute fibers and the high concentration of metal ions [32].
Meanwhile by increasing the contact time, the removal
(%) slow down and finally reached equilibrium, due to
limited vacant adsorption sites available on the Jute-g-
PAAc fibers. It was also found that, at the same condi-
tions, the removal (%) was grater in the case of Pb21
than that in the case of Hg21. This could be attributed
the change in their binding capacity, where it was 7.18
and 6.75 for Pb21 and Hg21, respectively [33]. Also, the
metal ion atomic number plays an important role
[34–36], in which the Pb21 metal ions possess the higher
atomic number and the smaller hydrated ionic radii,
which increase its adsorption possibility by using Jute-g-
PAAc.
Adsorption Kinetics. Various adsorption kinetic models
have been used to describe the adsorption kinetics of the
metal ions. The pseudo-first-order model [37, 38] was
used according to
where qe represents the adsorbed amount of metal ions
(mg/g) at equilibrium, qt is the adsorbed amount of metal
ions (mg/g) at time t, while k1 represents the pseudo-first-
order rate constant (min21). The slopes and intercepts of
the plots of log(qe–qt) versus time (t) were used to deter-
mine k1 and qe [13, 32] as illustrated in Fig. 7. The values
of k1, qe, and correlation coefficient (r2) are listed in
Table 1. As a comparison, the pseudo-second-order model
[39] was used according to
t=qt 51=k2 qe 2 1t=qe (6)
where qe is the adsorbed amount of metal ions (mg/g) at
equilibrium, qt represents the adsorbed amount of metal
ions (mg/g) at time t, while k2 represents the pseudo-
second-order rate constant (g/mg/min), The slopes of the
plot of (t/qt) versus time (t) were used to determine the
adsorbed amount of metal ions qe (mg/g), while the inter-
cepts were used to determine the rate constant of pseudo-
second-order model k2 (g/mg/min) [32, 40], as illustrated
in Fig. 7. The values of qe, k2, and correlation coefficient
(r2) are also listed in Table 1.
As shown in Table 1, the obtained data for both
adsorption kinetic models, the correlation coefficients
were found to be 0.7882 for both Pb21 and Hg21 accord-
ing to the pseudo-first-order model. Meanwhile, the corre-
lation coefficients by using of the pseudo-second-order
model were found to be 0.9991, which have good linear
relationship (r2 > 0.99) than the first-order kinetic model,
for both Pb21 and Hg21.

FIG. 7. The pseudo-first- and second-order plots for the adsorption of Pb21 and Hg21 by Jute-g-PAAc.

DOI 10.1002/vnl JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017 5

 TABLE 2. Adsorption isotherm parameters.

Langmuir model Freundlich model

2
Metal ions qm (mg/g) B (L/mg) r Kf [mg/g(L/mg)1/n] n r2

Pb21 16.67 0.01 0.99 0.75 0.78 0.97

Hg21 15.63 0.01 0.99 0.74 0.75 0.97

adsorbent molecules with the adsorbent surface [42, 43].

FIG. 8. Effect of initial ion concentrations on the adsorption capacity
of Pb21 and Hg21 by Jute-g-PAAc after 60 min at pH 5.
The common adsorption isotherm models that can be
used to describe the adsorption data are Langmuir and
Freundlich models. The Langmuir adsorption isotherm
assumes that the adsorption process occurs at specific
homogeneous sites on the Jute-g-PAAc and is the most
commonly used for the monolayer adsorption process,
according to:

On the other hand, the results of qe obtained by using
of the pseudo-first-order model were much lower than that
in the case of the pseudo-second-order model, which could
be attributed to the inapplicable of the pseudo-first-order
equation throughout the contact time more than 20–30 min
of the adsorption process [13, 32]. This indicates sharply
that the adsorption processes for both Pb21 and Hg21 by
Jute-g-PAAc obey the pseudo-second-order model.
Effect of Initial Concentration. The influence of the
initial metal ions concentrations Co (M) on the amount of
adsorbed Hg21 and Pb21 at equilibrium (qe) by Jute-g-
PAAc is shown in Fig. 8. It can be seen that the adsorp-
tion capacity (mg/g) at equilibrium (qe) increases with
increasing of the initial concentration of both Pb21 and
Hg21. This could be attributed to the acceleration of the
metal ions diffusion into the polymeric network, where,
at high concentration, the driving force increases, which
overcome the mass transfer resistance between solid–liq-
uid phases [41].
Adsorption Isotherms. The adsorption isotherms are
important for the discussion of the interaction of the
Ce =qe 51=b qm 1Ce =qm ; (7)
where qe represents the adsorption capacity (mg/g) at
equilibrium of metal ions on Jute-g-PAAc, Ce is the metal
ion concentration at equilibrium (M), qm is the monolayer
adsorption capacity (mg/g), and b is the Langmuir adsorp-
tion constant (L/mg). Figure 9 shows the Langmuir plot
of the adsorption of Pb21 and Hg21 by Jute-g-PAAc. The
slope and intercept of the plot of Ce/qe versus Ce were
used to determine qm and b as illustrated in Fig. 9. The
values of qm, b, and correlation coefficient (r2) are listed
in Table 2.
The Freundlich adsorption isotherm assumes that the
adsorption process occurs at specific heterogeneous sys-
tems and is most commonly used for adsorption process,
using
ln qe 5ln Kf 11=nln Ce (8)
where qe represents the adsorption capacity (mg/g) at
equilibrium of metal ions on Jute-g-PAAc, Ce (M) is the
metal ion concentration at equilibrium, Kf is Freundlich
constant, and 1/n is the heterogeneity factor. The slopes
and intercepts of the plot of ln qe versus ln Ce were used

FIG. 9. The Langmuir and Freundlich plots for the adsorption of Pb21 and Hg21 by Jute-g-PAAc.

6 JOURNAL OF VINYL & ADDITIVE TECHNOLOGY—2017 DOI 10.1002/vnl

to determine Kf and n as shown in Fig. 9 [44]. The values
of Kf, n, and correlation coefficient (r2) are also listed in
Table 2.
As shown in Table 2, the obtained data for both iso-
therm models indicate that the values of r2 for both
Pb21 and Hg21, according to the Langmuir equation,
were found to be 0.9954, while the maximum amount of
adsorption (qm) was 16.67 and 15.63 (mg/g) for Pb21
and Hg21, respectively. Meanwhile, r2 for both metal
ions, according to the Freundlich equation, were found
to be 0.9765. According to the values of the determined
correlation coefficients (r2), it can be seen that the Lang-
muir equation has a nearest fit to the experimental data
and have good linear relationship (r2 > 0.99) than the
Freundlich equation. Therefore, it can be concluded that
the adsorption of the metal ions by Jute-g-PAAc follows
the Langmuir model more than that of the Freundlich
model.
CONCLUSIONS
This work deals with the grafting of jute fibers with
PAAc. The prepared Jute-g-PAAc was used as an adsor-
bent for Pb21 and Hg21 from their solutions. From the
results, it can be concluded that the grafting yield found
to increase by increasing the concentration of AAc and
irradiation dose. The FTIR results prove the introduction
of PAAc onto the jute fibers. The XRD measurements
indicate the decrease of the crystallinity of jute fibers
after grafting by the amorphous PAAc. The adsorption
capacity (mg/g) of Jute-g-PAAc was enhanced at moder-
ate pH range up to 5 and 6 for Pb21 and Hg21, respec-
tively. It can be concluded also that the adsorption
kinetics of the adsorption process of Pb21 and Hg21 by
Jute-g-PAAc follow the pseudo-second-order rate and the
Langmuir adsorption isotherm model. For all cases, the
adsorption selectivity for Pb21 was greater than that in
the case of Hg21, according to the change in their binding
capacity.
ACKNOWLEDGMENTS
The authors thank the National Center for Radiation
Research and Technology (NCRRT), Egyptian Atomic
Energy Authority, for providing the facilities and financial
support throughout this work.
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