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Materials Today: Proceedings 5 (2018) 3334–3345 www.materialstoday.com/proceedings

ICMPC 2017

Synthesis of activated carbon from agricultural waste using a simple

method: Characterization, parametric and isotherms study
Jatinder Kumar Ratana, Manjeet Kaura, Bharadwaj Adirajua*
a
Department of Chemical Engineering, Dr B R Ambedkar National Institute of Technology, Jalandhar-144011, Punjab, India

Abstract

A low- cost activated carbon has been produced from agricultural waste using a simple method. Rice husk, corncob and wheat
straw have been used as precursor for synthesis of activated carbon. A simple method involving chemical activation using NaCl
has been tried for production of activated carbon. The synthesized activated carbon has been characterized using SEM (Scanning
electron microscopy), FTIR (Fourier transform infrared spectroscopy), EDS (Energy-dispersive-X-ray spectroscopy), BET
surface area analyzer, proximate and ultimate analysis. The adsorption experiments were also performed to evaluate the
adsorption capacity of the prepared activated carbon. The effects of contact time, adsorbent dose and solution pH on the
adsorption process were studied. The applicability of the Langmuir and Frendulich isotherms to the experimental data has also
been investigated.

© 2017 Elsevier Ltd. All rights reserved.

Selection and/or Peer-review under responsibility of 7th International Conference of Materials Processing and Characterization.

Keywords: Activated carbon, adsorption, isotherms, water purification.

1. Introduction

Purified drinking water is essential for living a healthy lifestyle. Contaminated drinking water may cause
serious diseases [1]. These diseases result in plenty of deaths of children under five years in developing countries
[2]. The purification of drinking water is one of the biggest issues all over the world especially in rural and remote
areas where availability of safe drinking water is limited.

* Corresponding author. Tel.: +91-9876850908

E-mail address: kumarj@nitj.ac.in

2214-7853 © 2017 Elsevier Ltd. All rights reserved.

Selection and/or Peer-review under responsibility of 7th International Conference of Materials Processing and Characterization.
 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345 3335

Nomenclature

C0 initial methylene blue concentration

Ce equilibrium methylene blue concentration
V volume of the methylene blue solution in contact with the adsorbent
m mass of adsorbent
KL Langmuir adsorption constant
KF Freundlich constant
n heterogeneity factor
qe adsorption capacity at equilibrium
qm maximum adsorption capacity

There are many techniques used for purification of water such as chemical oxidation [3], foam flotation [4],
ozonation [5, 6, 7, 8, 9], biological treatment [10], photocatalytic treatment [11], membrane filtration [12], Fenton
and photo-Fenton processes [13, 14, 15, 16, 17]. These processes are too complex and costly to be adopted by the
rural community for purification of drinking water for their day to day life. One of the simple and economical
technique for purification of water is adsorption [18]. Adsorption using activated carbon has a great potential for
removal of pollutants from water [19, 18]. Activated carbon (AC) is a microcrystalline material with a complex
heterogeneous surface functionality and high surface area [20].
Activated carbon adsorption is an attractive technique for removal of contaminants from water. Research is
being carried out all over the world for development of low-cost activated carbon [21]. The use of agricultural
waste as precursor for synthesis of activated carbon would reduce the cost of production. Agricultural waste
contains high carbon content. Being a renewable resource, agricultural waste is also available in large quantities
[22]. The use of simple process to produce activated carbon can also significantly decrease the cost of production. A
simple method of production of low-cost activated carbon from agricultural waste would greatly improve the quality
of living in rural and remote areas [23].
The objective of the present study is to prepare a low-cost activated carbon from agricultural waste using a
simple technique. Agricultural waste such as rice husk, wheat straw and corncob have been used as precursor for
production of activated carbon. A simple method involving chemical activation using NaCl has been tried for
production of activated carbon. The proposed method does not require any costly equipment and chemicals. It can
also be used in remote areas for production of activated carbon for purification of drinking water. The chemical
agent NaCl used for activation is generally available in the houses for routine use.
The prepared activated carbon has been characterized using SEM (Scanning electron microscopy), FTIR
(Fourier transform infrared spectroscopy), EDS (Energy-dispersive-X-ray spectroscopy), BET surface area analyzer,
proximate and ultimate analysis. The adsorption experiments were also performed to evaluate the adsroption
capacity of the prepared activated carbon. The cationic dye methylene blue was chosen as a model pollutant for
adsorption studies. The effects of contact time, adsorbent dose and solution pH on the adsorption were studied. The
application of the Langmuir and Frendulich isotherms to the experimental data has also been investigated.

2. Experimental methods

2.1. Preparation of activated carbon from agricultural waste

Three types of agricultural waste such as rice husk, wheat straw and corncob were used as precursor for
preparation of three kinds of activated carbon. The precursors were collected from a village Harchowal in Gurdaspur
district of Punjab, India. The precursors were washed for 2-3 times with distilled water. The washed raw material
was dried in hot air oven at 110 ᵒC for 12 h. The dried precursors were then cut into small pieces for chemical
activation. The chemical activation of the treated precursors was done with NaCl in 4:1 ratio using a magnetic
stirrer. The precursor material was then placed in a sealed aluminium box (50 mm diameter and 150 mm length)
3336 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345

having five holes of 2 mm diameter at the top side for gas outlet. The box containing the precursor was placed on an
open air wood fire for 30 min for carbonization. The carbonized material, which is the activated carbon, was again
washed with distilled water for 2-3 times and then dried in an oven for 24 h. The dried activated carbon was crushed
into small particles using mortar and pestle. The resulting activated carbon was stored in a desiccator for further
analysis and characterization. The % yield of the activated carbon, an indication of the efficiency of the production
process, was calculated as follows:

W
% yield = × 100 (1)
W

2.2. Characterization of samples

Proximate analyses was performed as per procedure of [24] to determine the volatile matter, ash, moisture
and fixed carbon content of the raw materials and respective activated carbons. Ultimate analyses of the activated
carbons was performed using an elemental analyzer (LECO CHNS 932) to determine the carbon, hydrogen, nitrogen
and sulphur content of the activated carbons. The surface area and pore volume of the activated carbons were
determined by Brunauer-Emmett-Teller (BET) method using a surface area analyzer (Gemini VII 2390,
Micromeritics ).The FT-IR spectra of the prepared activated carbons were recorded using Fourier transforms
infrared spectrometer (Perkin-Elmer Spectrum One). Oven-dried samples were mixed with potassium bromide in an
agate mortar, and the resulting mixtures were pressed into pellets for analyses. The spectra were recorded in the
wavelength range of 4000 cm-1 - 500 cm-1. The surface characteristics and structure of pores were determined using
a scanning electron microscope (JOEL JSM-6610LV). Energy-dispersive-X-ray spectroscopy (EDX) analyses of the
prepared activated carbons was done for chemical characterization of the activated carbons. The pHpzc of the
prepared activated carbons were determined according to the procedure mentioned in [25].

2.3. Adsorption Experiments

Batch adsorption experiments were carried out to evaluate the methylene blue adsorption capacity of the
obtained activated carbons. All the experiments were performed using 50 ml aqueous solution of methylene blue
with concentration of 50 mg/l. The solution was shaken at 50 rpm and 25 ᵒC in an incubator shaker (GYROMAX
727.) during the experiments. The concentration of methylene blue was determined at regular intervals using a UV-
visible spectrophotometer (UV-2600) at the maximum absorbance wavelength of 660 nm. All batch experiments
were carried out in triplicates, and mean values were used in the data analysis. The amount of methylene blue
adsorbed at equilibrium qe (mg/g) was calculated from the initial and final equilibrium concentrations according to
the following equation:

×
= (2)

Where, C0 (mg/l) is the initial methylene blue concentration; Ce (mg/l) is the equilibrium methylene blue
concentration; V (l) is the volume of the methylene blue solution in contact with the adsorbent; and m (mg) is the
mass of adsorbent.
The removal efficiency of methylene blue was calculated using the following equation:

% = × 100 (3)

The effect of adsorbent dosage, pH and contact time on the adsorption capacity was also evaluated during
the experiments. Langmuir [26] and Freundlich [27] isotherms were fitted to the experimental data of the adsorption
process.
 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345 3337

2.4. Adsorption Isotherms

The study of adsorption isotherms is very useful to describe the interaction between the adsorbate and the
adsorbent of any system. The adsorption isotherms give an indication about the distribution of adsorbate between
the liquid and solid phase at equilibrium. The analysis of the equilibrium data using Langmuir [28] and Freundlich
[27] isotherms provides information about the mechanism of the adsorption [29].
The Langmuir isotherm in its linear form is given by the following equation:

= + (4)

Where, qe (mg/g) is the adsorption capacity at equilibrium, Ce (mg/l) is the equilibrium concentration of the
adsorbate, qm (mg/g) is the maximum adsorption capacity, and KL (l/mg) is the Langmuir adsorption constant related
to the affinity of binding sites. The KL and qm can be obtained by fitting the experimental data to the Langmuir
model.
Freundlich model presents an empirical model which describes a non-ideal and multilayer adsorption on
the heterogeneous surface of the adsorbent. Freundlich isotherm is represented by the following equation:

= + (5)

Where, KF (l/g) is the Freundlich constant related to the relative adsorption capacity of the adsorbent, n
(dimensionless) is the heterogeneity factor. The values of KF and n can be obtained by fitting the experimental data
to the Freundlich model. If the value of n <1, the adsorption is a chemical process; if n>1, then it is a physical
process [30, 29].

3. Results and discussion

3.1. Characterization

The result of proximate analyses of raw materials and the prepared activated carbons is shown in Table 1. It
is obvious that the percentage of the fixed carbon content is more in the activated carbons as compared to the
respective raw materials. The obtained activated carbons have lesser percentage of the moisture, ash and volatile
content, which is due to effective carbonization of the raw materials. Among the activated carbons, activated carbon
prepared from corncob has the highest fixed carbon content (69.7 %) followed by activated carbon obtained from
wheat straw (55.4 %) and rice husk (41.0 %). The moisture, ash and volatile content of the activated carbon
(corncob) is lesser as compared to activated carbon (wheat straw) and activated carbon (rice husk). The ultimate
analyses of the activated carbons is shown in Table 2. There is no nitrogen and sulphur available in the activated
carbons indicating that most of their surface functionality is attributed to oxygen groups. Table 2 also shows the %
yield of the activated carbons obtained using different raw materials. Yield is maximum in case of rice husk
followed by corncob and wheat straw.
Specific surface area and pore volume of three activated carbons has been summarized in Table 2. The
specific surface areas of all three activated carbons were higher than 250 m2/g, and the highest corresponds to the
corncob (290 m2/g). The results indicated that there is subtle difference in the surface area and pore volume of the
three activated carbons. Therefore, it is likely that any difference in adsorption performance can be attributed to their
surface chemistry rather than their pore properties [25].
The FT-IR spectra of the activated carbons were recorded to find out the structural groups available on the
surface. FT-IR plots of the activated carbons and their respective raw materials are shown in Fig. 1a &1b. It can be
observed from Fig.1 that there is a large difference in the surface chemistry of the prepared activated carbons and
their respective raw materials. This difference may be attributed to disappearing of many of the functional groups
3338 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345

Table 1. Proximate analyses of the raw material and activated carbon.

Raw Material (% w/w) Activated Carbon (% w/w)
Proximate Analysis
Rice husk Wheat straw Corn cob Rice husk Wheat straw Corn cob
Moisture Content 1.7 0.7 2.9 3.8 5.7 6.7
Ash Content 7.4 8.0 8.5 2.3 1.0 1.0
Volatile Matter 75.2 68.2 58.0 53.0 38.0 77.4
Fixed Carbon 15.7 23.2 30.6 41.0 55.4 69.7

Table 2. Ultimate and surface area analyses.

Activated carbon Ultimate analysis Surface area Pore volume (cc/g) Yield (%)
(m2/g)
C (%) H (%) N (%) S (%)
Rice husk 45.5 1.5 0 0 281.7 0.14 34.1
Wheat straw 72.2 1.3 0 0 282.1 0.08 31.2
Corncob 73.7 2.2 0 0 290.2 0.19 33.9

during carbonization and activation process. Thermal degradation during carbonization leads to the destruction and
formation of some of the functional group. The FT-IR spectra (Fig. 1a) of the activated carbon of rice husk indicated
the presence of following functional groups: O-H group (600 - 800 cm-1); ester (1750-1800 cm-1); C-O and C-O-C
(1060-1115 cm-1); alkyl halide C-Cl (1620-1680 cm-1) [31, 32, 33]. Fig.1b shows the FT-IR spectrum of wheat straw
and activated carbon (wheat straw). The peak at 3399 cm-1 corresponds to O-H stretching bond. The peaks around
2950-2900 cm-1 were due to stretching of C-H [34, 35, 36, 37]. The hydrophilic tendency (–OH groups) of wheat
straw and activated carbon (wheat straw) was reflected in the region 3700 – 3100 cm-1. The peak at 1652 cm-1
represents carboxylate groups. The peaks at 1373 cm-1 represented C-H asymmetric deformation. The peaks in the
region of 1200 – 1059 cm-1 represent all C-O stretch bands [35]. The FTIR spectra of activated carbon (corncob)
also showed the similar results, and hence, not shown here for brevity.

SEM analysis was done for both raw materials and activated carbons. Fig. 2 (a)(b) and (c) shows the SEM
images of rice husk, wheat straw, corncob and respective activated carbons. Fig. 2 (d), (e) shows that the surfaces of
rice husk, wheat straw and corncob are smooth, and have no pores on them before activation. However, the surfaces
of the corresponding activated carbons are rough. This can be attributed to the activation with NaCl. Porosity is also
visible on the surfaces of the obtained activated carbons which may be attributed to effective activation and
carbonization. The activated carbon (corncob) clearly showed the more porous structure (Fig. 2f) as compared to
other activated carbons. Porosity is an excellent texture of an adsorbent as it provides large surface area for the
adsorption process [38].

Energy dispersive X-ray (EDX) analysis of the raw materials and obtained activated carbons was
performed to estimate the composition of various elements present in the adsorbents. Table 3 shows the EDX
analysis of the raw materials and activated carbons. It can be observed that the carbon weight percentage has
increased in all of the three activated carbons as a result of activation and carbonization. The surface is composed of
higher weight percentage of carbon and oxygen. The EDX analysis proves the presence of sodium and chlorine on
activated carbons. As sodium chloride is strong dehydrating agent, it adsorbs water from surrounding, thus
increasing the porosity of raw material. The pHpzc is an important characteristic for any activated carbon as it
indicates the acidity/basicity of the adsorbent and the net charge on the surface of the activated carbon [39]. If pH of
the working solution is less than pHpzc, the net surface charge on the activated carbon is positive, while it is negative
whenever the pH of the solution is more than pHpzc. The pHpzc value is important to determine the working pH
conditions at the time of adsorption studies. The pHpzc of activated carbons obtained from rice husk, wheat straw and
corncob was determined to be 4.23, 5.23, and 5.43, respectively
 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345 3339

(a)

(b)
Fig. 1 FTIR spectra of (a) rice husk and activated carbon (rice husk) (b) wheat straw and activated carbon (wheat straw).
3340 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345

3.2. Effect of contact time

To find out the effect of contact time on the adsorption of methylene blue, 0.1g of activated carbon was
added to 50 ml of the solution, and stirred at 25 °C. The initial concentration of the methylene in the solution was 50
mg/l. The adsorption studies were carried out for 240 min (4h). It was observed that percentage removal of
methylene blue increases with increase in contact time as shown in Fig. 3. Initially, the pores of the adsorbents are
unoccupied, which leads to rapid removal of the methylene blue. Gradually, the pores gets occupied resulting into
slower adsorption of methylene blue. Eventually, the surface of the adsorbent becomes saturated, and no net
adsorption takes place [18]. As clear from Fig.3, 94, 91.5 and 79.6 % of the methylene blue was removed by
activated carbon (wheat straw), activated carbon (corncob) and activated carbon (rice husk), respectively after 60
min. The difference in methylene blue removal may be attributed to the different physical as well as chemical nature
of the pores of the activated carbons. At 120 min, almost 96 % of the methylene blue was removed by all the
activated carbons. After this time, the rate of adsorption decreased gradually and reached equilibrium at 240 min.
The percentage removal of the methylene blue was obtained as 99.5, 99.2 and 88.7 % for activated carbons
produced from wheat straw, corncob and rice husk, respectively.

3.3. Effect of dose

The effect of adsorbent dose on percentage removal of methylene blue is shown in Fig 4. The dose was
varied from 0.05 to 0.10 g, while pH and time was fixed at 7.4 and 240 min, respectively. As the dose increased
from 0.05 to 0.07 g, the percentage removal of methylene blue increased from 61.2, 91.2 & 85.8 % to 87.0, 95.4 &
90.9% for activated carbons obtained from rice husk, corncob and wheat straw, respectively. The increase in
removal percentage is due to increase in availability of number of active sites for adsorption due to increase in dose
of adsorbent. As the activated carbon dose is further increased from 0.07 g to 0.10 g, the removal of methylene blue
increases by 11.7, 3.8 and 8.6% for activated carbons obtained from rice husk, corncob and wheat straw,
respectively. This slower increase in percentage removal may be attributed to the equilibrium between the active
sites on the adsorbents and methylene blue [40].

3.4. Effect of pH

Fig. 5 shows the effect of pH on adsorption of methylene blue onto the activated carbons. The activated
carbon dose and time were fixed at 0.05g and 240 min, respectively. It is observed from Fig. 5 that the removal
efficiency remarkably increased with increase in the pH values. The percentage removal of methylene blue
increased from 47.8, 39.2 and 31.4 % at pH of 2 to 98.7, 98.4 and 98.5% at pH of 12 for activated carbon (rice
husk), activated carbon (corncob) and activated carbon (wheat straw), respectively. The evident dependence of
adsorption capacity on solution pH gives an indication that the electrostatic interaction and repulsion forces are
dominant in the adsorption process. At pH lesser than pHPZC, the carbon surface has a net positive charge,
while at pH greater than pHPZC the carbon surface has net negative charge. Methylene blue is a cationic dye
having positive charge. Therefore, a higher percentage removal at higher pH may be attributed to electrostatic
attraction between the negatively charged carbon surface and positively charged methylene blue. At lower pH, the
carbon surface is positively charged, which gives smaller percentage removal of methylene blue due to electrostatic
repulsion between adsorbent and adsorbate [41, 42]. The results are in agreement with the findings of [43].

3.5. Analysis of isotherms

Adsorption isotherm data was obtained using 0.05 g activated per 50 ml of methylene blue solution at
different initial concentrations ranging from 10 to 50 mg/l. The obtained values of different parameters of Langmuir
and Freundlich isotherms are shown in Table 4. The applicability of the both the isotherms were evaluated by
comparing the values of correlation coefficient, R2. It can be observed from Table 4 that the values of regression
 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345 3341

coefficients are better for Langmuir isotherm as compared to Frendulich isotherm for all the activated carbons. This
proves that the Langmuir model fits to the adsorption data better than the Frendulich model. The applicability of the
Langmuir model suggests that the adsorption of methylene blue on activated carbon is a homogeneous and
monolayer adsorption. There is no intermolecular interaction among the adsorbed molecules of methylene blue. As
obvious from Table 4, the activated carbon (wheat straw) has the highest adsorption capacity (90.9 mg/g), while
activated carbon (rice husk) and activated carbon (corncob) have almost similar adsorption capacities of 72.4 and
72.5 mg/g, respectively.

Fig. 2 SEM images of raw materials and activated carbons.

3342 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345

.
Table 3 EDX analysis of the raw material and activated carbon.
Raw Material (% w/w) Activated Carbon (% w/w)
Element
Rice husk Wheat straw Corn cob Rice husk Wheat straw Corn cob

C 30.13 60.04 39.36 46.11 67.94 46.69

O 58.35 34.75 59.07 36.50 29.52 52.60

Na 0.16 1.57 0.19 2.25 0.93 0.12

Mg 0.36 0.03 0.28 0.09 0.02 0.17

Si 9.72 2.00 0.15 11.32 0.97 0.07

Cl 0.13 1.62 0.16 3.72 0.62 0.06

Ca 0.72 0 0.27 0.11 0 0.09

Fig. 3 Effect of time on removal efficiency.

Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345 3343

Fig. 4 Effect of adsorbent dose on removal efficiency.

Fig. 5 Effect of solution pH on removal efficiency.

3344 Jatinder Kumar Ratan et al. / Materials Today: Proceedings 5 (2018) 3334–3345

Table 4 Langmuir and Frendulich isotherm parameters.

Adsorbent Langmuir Freundlich
qm(mg/g) 72.4 n 2.77
Activated carbon (rice
KL(l/mg) 5.5 KF(l/g) 26.4
husk)
R2 0.997 R2 0.956
qm(mg/g) 90.9 n 1.66
Activated carbon (wheat
KL(l/mg) 2.0 KF(l/g) 2.91
straw)
R2 0.995 R2 0.778
qm(mg/g) 72.5 n 1.04
Activated carbon
KL(l/mg) 3.4 KF(l/g) 1.68
(corncob)
2 2
R 0.997 R 0.979

4. Conclusions

Agricultural waste such as rice husk, corncob and wheat straw was used as precursor for the production of
activated carbon by chemical activation with NaCl. The characterization provided an idea about the surface, textural
and functional properties of the produced activated carbons. The adsorption experiments showed good capacity of
the prepared activated carbons for adsorption of methylene blue. The equilibrium data for adsorption of methylene
blue fitted well into Langmuir isotherm. The results showed that agricultural wastes can be used to produce low-cost
adsorbents using a simple method. These adsorbents have potential for purification of drinking water in remote
areas.

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