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International Journal of Nanomaterials and Biostructures


Universal Research Publications. All rights reserved

ISSN 2277-3851
Original Article
Chitosan-Activated Carbon Nanocomposites as Potential Biosorbent for Removal
of Nitrophenol from Aqueous Solutions
Usha Soni, Jaya Bajpai and A.K.Bajpai
Bose Memorial Research Laboratory
Department of Chemistry, Government Autonomous Science College, Jabalpur (MP), Inida
Received 22 November 2015; accepted 15 December 2015
Abstract
The adsorption of nitro phenol by chitosan based nano composites, prepared from activated carbon and chitosan was
investigated to assess its possible use as adsorbent. The resulting particles were characterized by techniques like Fourier
transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) spectroscopy,
particle size and charge analysis. The effect of pH, initial adsorbate concentration, adsorbent dosage and contact time were
studied to identify adsorption capacity of the nano composites. Adsorption data were modelled with the Freundlich,
Langmuir, Tempkin and Dubinin-Radushkevich classical adsorption isotherms. The data fitted the Freundlich isotherm
model better than Langmuir and Dubinin-Radushkevich. Adsorption kinetic studies, showed that the adsorption process
followed a pseudo second -order kinetic model. The maximum adsorption capacity of nitro phenol, on to the chitosan-
based nano composites was found to be, 1257 mg g-1, respectively.
2015 Universal Research Publications. All rights reserved
Key words: Adsorption, nitro phenol, composites, chitosan.

1. Introduction 21) deserve particular attention.These biopolymers


Now-a-days, one of the major represent an interesting and attractive alternative as
environmental problems facing by humanity is the adsorbents because of their particular structure, physico-
increasing worldwide contamination of fresh water systems chemical characteristics, chemical stability, high reactivity
from various industrial chemical compounds. Out of all and excellent selectivity towards phenolic compounds,
contaminants contained in industrial waste water, phenolic resulting from the presence of chemical reactive groups
compounds are the most un-desired ones. The major (hydroxyl, acetamido or amino functions) in polymer
industries that contribute to chemical compound and waste chains. Moreover, it is well known that polysaccharides
production are petrochemical, chemicals, agrochemical, which are abundant, renewable and biodegradable
textile and pharmaceutical. Since these chemicals could biodegradable resources, have a capacity to associate by
cause adverse effect on digestive system, nervous system physical and chemical interactions with a wide variety of
and respiratory system (1) particularly, nitrophenols are molecules (22,23) Hence adsorption polysaccharide
listed as a priority toxic pollutant and used to produce derivatives can be a low-cost procedure of choice in water
pharmaceutical drugs and pesticides such as nitrofan and decontamination for have been used as adsorbents to adsorb
parathion (2) phenolic compounds .Among them, chitosan have been
Various techniques have been employed considered as one of the best choice because Chitosan is a
for the removal of phenolic compounds from waste water very promising adsorbent, which can be modified in many
such as electrochemical treatment (3) membrance (4), ways (grafting, cross-linking, functionalization for forming
adsorption (5,6) and biological treatment (1). Despite the composites, etc.). The potential of chitosan is strong due to
availability of above mentioned processes for the removal its origin product being chitin which can be found in
of phenolic compounds, adsorption is efficient,effective abundance
and extensively adopted(7). Recently, many low cost 2. Materials and methods
adsorbents such as baggasse fly ash (8), zeolite (9) , Chitosan, activated carbon, acetic acid, toluene,
activated carbon (10) and natural polymer among these, tripoly phosphate (TPP) and nitro phenol used were of
polysaccharides such as chitin (1113) and starch (1416), analytical reagent grade and supplied by Merck India.
and their derivatives (chitosan (17,18), cyclodextrin (19 Water used for preparation of solutions was generated in
International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61
53
the laboratory by double distilling the deionized water in a biosorbent were recorded on a FTIR-8400, Shimadzu
distillation unit. The stock solution of nitro phenol was spectrophotometer. Samples for the spectral analysis were
prepared by dissolving 100 mg nitro phenol in one litre prepared by mixing adsorbent and KBr in1:10 proportion
water. All other required reagents were of analytical grade and the spectra were obtained in the range of 4000400
quality. cm1with a resolution of 2 cm.1
The concentration of nitro phenol in aqueous SEM analysis
solution was determined by measuring absorbance at A scanning electron microscope inter-phased
wavelength of 317 nm, using a UV spectrometer (model with an electron dispersive X-ray spectrometer (SEM, JEO,
Shimadzu UV-1500). In order to reduce measurement JSM-5800LV) was used to study the surface morphologies
errors in all the experiments, the UV adsorption intensity of and elemental analysis of chitosan based nanocomposite
each solution sample was measured in triplicate and the and activated charcoal.
average value was used to calculate the equilibrium X- Ray diffraction (XRD) analysis
concentration based on standard calibration curve, whose In order to ascertain crystalline nature of the
correlation coefficient (R2) was found to be 0.9967 chitosan based nanocomposite. XRD analysis were per-
Adsorption experiments were carried out using formed on a rotating X-ray diffractometer in the 2 range
the batch contact method. In brief, 50 mg of chitosan based of 1070C
nanocomposite was added into a 10 mL of nitro phenol Particle size and particle charge analysis
solution at constant pH and temperature. The suspension The sample was prepared by dispersing a definite
was shaken on a thermostat shaker (Rivotech India) for 1 h amount of nanoparticles in ethylene glycol, having a
to attain equilibrium at the room temperature (30 0C). After viscosity 0.0100 cP as the dispersant. The dispersant was
shaking was over the mixture was filtered through the placed in the disposable zeta cell and the surface charge of
Whatman filter paper (2.5 size particle retention). The the nanocomposite was determined using Zetasizer Nano
adsorption capacity of the adsorbent was determined by (Backman Coulter Delso Nano C.)Dynamic light scattering
material balance of the initial and equilibrium technique was used to determine particle size. The zeta
concentrations of the solution. potential distribution was determined from the zeta
The adsorbed amount and the percentage removal of nitro potential (Mv) versus intensity (kcps) curve and the
phenol were calculated by using the following equations, measurements were performed at 25 0 C with the count rate
respectively. of 2272.3kcps
Adsorbed amount (mg/g) =
Ci Cf
v (1) 3. Results and Discussion
m Fourier Transform Infrared (FTIR) Studies
Ci Cf
% removal = 100 (2) FTIR spectra of chitosan, chitosan based
Ci
Where Ci is the initial and the Cf is the final concentrations nanocomposite particles, before and after adsorption are
of the nitro phenol solutions (mg/L), shown in Figures (1a-c), respectively. The FTIR spectrum
V is the volume of the adsorbate solution, and m being is of chitosan(1-a) shows a broad and strong band at
the weight of adsorbent (chitosan composite). The pH of 3431.1 is due to overlapping of the OH and N-H
the solution was adjusted using required volumes of 0.1 M stretching vibration of functional groups engaged in
HCL and /or 0.1 N NaOH before adding the adsorbent. hydrogen bond (24). The band at 2910.1 and
2.1 Preparation and characterisation of adsorbent 2874.1 is due to symmetric and asymmetric -
Chitosan based biosorbent was prepared by emulsion 2 vibration attributed to pyranose ring. A peak at
crosslinking method. In brief, for preparation of adsorbent 1653.1 is C=O stretching in amide group
a known amount of chitosan was dissolved in 10 mL of 1% band,1572.1 is N-H bending in non acetylated 2-
acetic acid solution and after its homogenous mixing a aminoglucose primary amine, The sharp peak at 1381.1
requisite amount of activated carbon was added in to it. The is C-N stretching ,The peaks at 1068.1 ,1035.1 ,are
whole mixture was stirred on a magnetic stirrer for about skeletal vibration involving the CO stretching which are
1 h at room temperature while for preparing w/o emulsion, characteristic of chitosan saccharide structure and
10mL paraffin-oil was added in to homogenous mixture of 663.1 is due to -2 wagging vibration peak.
chitosan-charcoal suspension. The above solutions were The following changes were observed in the FTIR spectra
mixed on a magnetic stirrer for 2 h to form a stable of chitosan based nanoparticles before adsorption ( Fig-1b),
emulsion. Now to this stable emulsion 10 mL of TPP the absorption peak 3431cm-1 has a shift to 3504 cm-1and
solution of 0.1 M concentration was dropwise added and the peak for asymmetric deformation of NH vibration in
stirred for 4 h at room temperature. The nanocomposite NH3+ ion is 1696 cm-1 (25, 26 ). Some new bands
particles so prepared were cleaned by washing frequently appears, a band at 1149 cm-1 that corresponds to P=O
with toluene and acetone. The final particles were dried at stretching vibration in phosphate ion (27) and peak at 3745
room temperature and stored in an air tight polyethylene cm-1 is due to surface functional group OH stretching
bag. vibration that present on activated charcoal(28). A
Prior to using the prepared adsorbent for significant difference can be seen in the FTIR spectra of
adsorption experiments, the adsorbent was characterized by composite nanoparticles before and after adsorption, peaks
the following techniques. are shifted and/or broadened indicating that the functional
Fourier transforms infrared (FTIR) spectroscopy groups present on the composite nanoparticles is involved
The FTIR spectra of prepared chitosan based in interaction with the nitro phenol.

International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61


54
Fig. 1 FTIR spectra of (a) chitosan (b) chitosan based nanocomposite (c) nitro phenol adsorbed chitosan based nano
particles.
For the pure chitosan, there were two peaks around 2
X-Ray diffraction (XRD) analysis value 10 and 200 (29) Chitosan retained semi crystalline
XRD analysis is based on constructive interference of
monochromatic X-rays. It is a non-destructive technique characteristic in the nano composites. The peak of chitosan
widely used to investigate the interlayer changes and the at 2 = 100 is disappearing in the nanocomposite and the
crystalline properties of the synthesized material. The inter- peak at 20.60 which corresponds to a d (110) spacing of
planer distances may be calculated by the following 0.45nm X-ray diffraction (b) become weakened and the
Braggsequation. intensity of the peak became low. These evidences
n = 2d(hkl)Sin (3) suggested that strong interaction occurred between
where is the wavelength of the X-ray, is the scattering activated carbon and chitosan molecule in the formation of
angle, n is an integer representing the order of the nanocomposite. Many new sharp peaks were observed in
diffraction peak, d is the inter planer distance of the lattices, XRD spectra of the nanocomposite which illustrated the
and (hkl) are the Miller indices.The XRD spectra of presence of different alumino-silicate minerals in activated
chitosan based carbon composite particles were recorded carbon. Major peaks were observed at 2 = 28, 29.2, 34,
and results are depicted in Fig. 2 which clearly indicates a 36.9 and 40.1.The peak at 29.2 is for zeolites, and at 2 =
crystalline nature of particles due to sharpness of peaks in 26 peaks corresponds to graphite. Spectra also depicts so
the spectra. many small and medium diffraction peaks at various 2
values which suggest for the presence of a number of other
aluminosilicates such as quartz, sodium silicates etc .The
mean grain size of composite particles was calculated using
Debye-Scherrer formula as shown in equation

= (4)

Where is mean size, k is the shape factor (0.94),
is broadening of the diffaction angle and is diffaction
wavelenth (1.54A0).The estimated average crystal size of
particles was calculated to be 28.1nm with lattice strain
0.0074.

The amorphous and crystalline nature of


particles can also be quantified in terms of degree of
crystallinity. The numerical formula to calculate the percent
crystallinity of biocomposite is given in the following
Fig.2. XRD pattern of chitosan based nanocomposites. equation

International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61


55
found to be 7.32m. The zeta potential of composite
xc % = (5)
+
particles is commonly used to characterize the surface
Where Ac and Aa are the area of crystalline
charge properties of surface active materials. High electric
and amorphous phases respectively (30). The percent
surface charge shows high value of zeta potential of the
crystallinity of nanocomposite was found to be more than
composite particles due to repulsive forces between
80%.Chitosan is semi crystalline in nature, Impregnation of
particles which leads to stop it from aggregation (30, 31).
activated charcoal in the matrix increases its overall
The zeta potential of composite particles was measured
crystallinity and many sharp peaks with different intensities
before and after adsorption. Before adsorption it was found
were observed in XRD spectra of chitosan based
to be 54.75mV, which indicates cationic nature of particles.
nanocomposites.
After adsorption of nitro phenol it decreases up to 2.15 mV
Particle Size and Charge Analysis
which clearly indicates that nitro phenol were adsorbed in
Particles size distribution of chitosan-based
the form of nitro phenolate ions.
nanoparticles are shown in Figure 3. It was observed that
aggregate size of chitosan based composite particles were

Fig.3. Image shows particle size distribution


Scanning electron microscope (SEM) then it decreases as the pH further increases. Fig .reveals
Emission electron microscopy is that, pH primarily affects the degree of ionization of nitro
the most widely used technique for the investigation of phenol and the surface properties of nanocomposites. Here
shape, size morphology and porosity of the chitosan based we have observed highest uptake of nitro phenol by at
nanoparticles matrices. Figure 4 (a and b) show SEM pH=2, at low pH values, the surface of the nanocomposites
microphotographs of the activated charcoal and chitosan would be protonated and resulted in a stronger attraction
based composite nanoparticles. Sem photograph of for negatively charge phenolate ions.nitro Phenol, being
activated carbon shows that wide variety of pores is present weakly acidic (pKa =7.15), partially ionizes in solution.
along with fibrous structure while the composite These ions are negatively charged and are directly attracted
nanoparticles showed rod like structure. to the cationic surface of nanocomposites by electro-static
force. Unionized nitro phenol molecules would also be
attracted, possibly, by physical force. After that the uptake
capacity goes down at pH of 7.

Fig.4. SEM image of (a) activated carbon (b) chitosan


based nanocomposites.
Effect of pH
The initial pH of adsorption medium is one of the
most important parameters affecting the adsorption process.
The effect of initial pH on the adsorption of nitro phenol
was also evaluated at 30oC at different initial pH values in
the range of 28 for initial concentrations of 100 mg/L for
nitro phenol solution adjusted by adding either 0.1M HCl
or 0.1M NaOH. The variation of adsorption with different Fig. 5. Effect of pH on % removal of nitro phenol [Temp]
values of pH are shown in Figure 5 which clearly reveal =2820C.[nano-composites] =0.05g ,0.01mL-1 nitro phenol
that the nitro phenol adsorption is maximum at 2 pH and solution,[Time] =60 min.
International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61
56
Effect of adsorbent dose Effect of contact time
The effect of adsorbent doses on the removal of The rate of nitro phenol removal is found
nitro phenol was studied in the range 10- 100 mg//10mL of to be very rapid during the initial 30 min, but it declines
nitro phenol solutions .From the Figure 6 it is clearly gradually and reaches equilibrium at around 45min. No
visible that % removal increases with the adsorbent dose significant change in nitro phenol removal is observed after
and then it becomes constant. The increase in % removal about 45min. The initial rapid phase may be due to the
could be explained by the fact that an increase in number of availability of more adsorption/vacant sites at the initial
active sites results with increase in adsorbent dose. stage. Results are shown in Fig.8, there exists an increased
However, above a certain dose removal percentage assumes concentration gradient between adsorbate in solution and
as asymptotic value. It can be explained by assuming that adsorbate on the adsorbent. This can be explained by strong
there is an overlapping of active sites at high doses which attractive forces between nitro phenol molecules and the
decreases the surface area as was observed by others (32). adsorbents, and also by the fast diffusion into the
interparticle matrix to attain rapid equilibrium,.nitro phenol
removal versus time curves are single, smooth and
continuous leading to saturation, thus suggesting coverage
of nitro phenol on the outer surface of the adsorbent. This
result is consistent with the results obtained by others (35,
36, 37).

Fig.6. Effect of adsorbent doses on % removal of nitro


phenol [Temp] =282oC, 0.01mL-1 nitro phenol solution
[Time]=60 min
Effect of temperature
The effect of temperature on the percent removal
of nitro phenol has been studied by increasing the
temperature of adsorption system from 20 0C to 500C. The
results are shown in Fig. 7 which shows the effect of
increasing temperature on the % removal of nitro phenol. Fig.8. Effect of contact time on % removal of nitro phenol
The behaviour of the graph shows that the maximum [Temp]=282OC [nanocomposites]=0.05g,0.01mL-1 phenol
removal of 91% nitro phenol is obtained at 20 0C and then it solution
decreases gradually with increasing temperature. The
decrease in percentage removal of nitro phenol with Adsorption Kinetics
increasing temperature may be due to damage of active Kinetic study is helpful in prediction of adsorption rate
binding sites and weakening of binding forces between the constants, adsorption capacity and adsorption mechanism.
nitro phenol molecules and adsorbent. Similar type of The capability of pseudo-first order and pseudo second
results has also been reported elsewhere by others (33, 34). order kinetic model were examined in this study at
constant temperature of 300C.
The linear form of pseudo- first order model
of Lagergreen (38) is generally expressed as follows: Log
( )= log ( ) K*t (4)
Where the adsorption
capacities of the nitro phenol per unit are weight of
nanocomposite particles at equilibrium and at time t (min)
respectively (mg/g) and 1 is the pseudo first order rate
constant (min-1), 1 and values are determined from the
slope and the intercepts of the graph which is plotted
between Log ( ) vs t
From results it can be seen that experimental values
do not agree with the calculated ones that shows
applicability of the pseudo first order model to the
Fig.7. Effect of temperature on % removal of nitro phenol
adsorption process of the nitro phenol onto chitosan based
[nanocomposites]=0.05g,0.01mL-1 nitro phenol solution,[
nano particles is unfeasible.
Time]=60 min

International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61


57
The linearized form of pseudo-second order kinetics log qe =log Kf +log Ce (7)
is given by the following equation: According to the above equation, a plot of (log qe) against
1 (logCe) yields a straight line which indicates the
= 2 2+ (5)


confirmation of the Freundlich isotherm for adsorption. The
From the equation, the plot of against t should give a constants can be obtained from the slope and the intercept

linear relationship. The and 2 can be determined from of the linear plot of the experimental data and summarized
the slope and intercept of the plot. The pseudo second-order in the Table 2. The value of n indicates a favourable
kinetic parameters are presented in Table-1. physical adsorption .Vander-Waals forces involved in
From the above data we see that the values adsorption.
(experimented) values are quite closer to those of . Langmuir isotherm
(calculated) values for pseudo second order kinetics. The Langmuir adsorption isotherm is often used
Hence, it can be concluded that the adsorption of nitro to describe adsorption of solutes from a liquid solution. A
phenol on chitosan based nano particles is described by basic assumption of the Langmuir theory is that sorption
pseudo second order kinetic mode. takes place at specific homogeneous sites within the
adsorbent. It is then assumed that once a nitro phenol
Table- 1. kinetics constant for the adsorption of nitro occupies a site, no further sorption can take place at that
phenol on the chitosan based nano composite site. The rate of sorption to the surface should be
Kinetic models parameters
proportional to a driving force multiplied by area. The
Pseudo first order
qe (mg/g) driving force for adsorption is the concentration in the
68.75 solution, and the area is the amount of bare surface
k1 (min1)
5.310-2
R2 available on the adsorbent. The Langmuir adsorption
.91079
Pseudo second order isotherm is perhaps the best known of
qe (mg/g)
360 all the isotherms and is often expressed as,
k2 (g/mg/min)
3.910-2 0
R2 . a= (8)
9992 1+
where a = is the amount of nitro phenol adsorbed per unit
Adsorption Isotherms mass of adsorbent (mg/g), Ce= is the equilibrium
Several two or three-parameter models havebeen concentration of nitro phenol (mg/L), Q0= is a measure of
published in the literature to describe the adsorption capacity of adsorbent (mg/g), b = is the
equilibriumadsorption isotherms (39, 40, 41, 42, 43). In this Langmuir constant which is measure of energy of
study, the adsorption mechanisms and characteristic adsorption (L/mg).The above equation can be rearranged to
parameters for the present processes were analyzed by four give the following linear
1
two-parameter (Freundlich, Langmuir, Temkin and = + (9)
0 0
Dubinin-Radushkevich) isotherms,these are commonly The above equation can be used for the linearization of
used to describe the adsorption characteristics of adsorbent experimental data by plotting Ce/qe against Ce, and a good
utilized in water and wastewater treatment. Therefore, fit of this equation reflects monolayer adsorption.
adsorption data of nitro phenol on chitosan based nano Moreover, the Langmuir constants b and Q0 can be
composite were employed to test Langmuir, Freundlich, evaluated from the slope and intercept of linear equation,
Temkin and Dubinin-Radushkevich in this study. Which respectively. The values of Q0 and b obtained in this work
have been tested to describe the relationship between the and presented in Table -2 respectively.
amounts of nitro phenol adsorbed (qe) and its equilibrium
concentration (Ce) in the solution. Table 2: Data showing the values of adsorption isotherms
Freundlich isotherm obtained for adsorption of nitro phenol on chitosan based
Freundlich isotherm assumes that the uptake of nanocomposites
nitro phenol occurs on a heterogeneous surface by Isotherms parameters
multilayer adsorption and that the amount of nitro phenol Freundlich
adsorbed increases infinitely with an increase in R2
.9557
concentration. It is a most popular model for a single solute n
.133
kf (mg/g)
system, based on the distribution of solute between the 2.19710-4
Langmuir.
solid phase and aqueous phase at equilibrium. Freundlich R2
isotherm is an empirical equation and expressed as, Q0(mg/g) .8569
qe =Kf Ce 1/n (6) b (L/g) - 89.76
where qe =is the amount of nitro phenol adsorbed Tempkin -1.007
per unit mass of adsorbent (mg/g), Ce is the equilibrium R2
concentration of nitro phenol (mg/L), Kf= is the measure of B
.9841
adsorption capacity(empirical constants depending on AT (L/g)
10155
several environmental factors),1/n = adsorption intensity D-R model
.1478
R2
(an empirical parameter representing the energetic
qm ( mol/g)
heterogeneity of the adsorption sites). The equation is (mol2/j2 ) .9573
conveniently used in the linear form by taking the .004 1.66 106
logarithmic of both sides as shown below:
International Journal of Nanomaterials and Biostructures 2015; 5(4): 53-61
58
Temkin isotherm adsorbent dose, and temperature and solution pH were
Temkins isotherm model was also applied to the optimized. The adsorption was found to be highly
experimental data. The Temkin isotherm equation assumes influenced by initial nitro phenol concentration and nitro
that the heat of adsorption of all the molecules in layer phenol speciation which is directly related to solution pH.
decreases linearly with coverage due to adsorbent Equilibrium study show that the data fit very well in the
adsorbate interactions, and that the adsorption is Freundlich equation of multilayer adsorption, this result
characterized by a uniform distribution of the bonding indicate the heterogeneity of the adsorbent surface. The
energies, up to some maximum binding energy was carried values of R2 obtained from pseudo second-order model
out by plotting the quantity sorbed qe against lnCe and the were higher than 0.9992, indicating that the adsorption
constants were determined from the slope and intercept. process obeyed the pseudo second-order model. Finally the
The model is represented by the following equation adsorption experiments indicated that chitosan based nano
composite was efficient adsorbent for the removal of nitro
qe = RT ln(ATCe) quation (10) phenol from water.

5. Acknowledgements
qe = lnAT+ lnCeB = (11) Authors wish to acknowledge the, Indian

Institute of Technology of Bombay, Model science college
Eq. (11) can be expressed in its linear form as:
Jabalpur, and Indian Institute of Science Education and
qe = BlnAT + BlnCe (12) Research (IISER) Bhopal, analytical facilities for
characterization of the pre-pared materials
Where AT= Temkin isotherm equilibrium binding constant
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Source of support: Nil; Conflict of interest: None declared

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