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<div class="articledetails article-header clearfix">
<p class="art-type">Research Article</p>
<p class="art-title">Adsorption of Chemically Prepared Cocoa Nibs Based
Activated Carbon Onto Methylene Blue: Equilibrium
and Kinetic Studies</p>
<p class="art-author"><?php $authors="KhairulAdli Nikman<sup>1,2</sup>, Fisal Ahmad<sup>3</sup>, MohdSukri Hassan<sup>1</sup>, Khairunisa Nikman<sup>4</sup> and Mohd Azmier Ahmad<sup>5,6*</sup>"; echo (stristr($authors,$coauthor))?str_replace($coauthor,"<a href='".$extpath."authors/".$courl."' target='_blank'>".$coauthor."</a>",$authors):$authors; ?></p>
<p class="art-affl">
<sup>1</sup>Faculty of Science and Technology, Universiti Sains Islam Malaysia, 71800 Nilai, Negeri Sembilan, Malaysia<br>
<sup>2</sup>Jabatan Perubatan Forensik, Hospital Kuala Lumpur, 50586 Kuala Lumpur, Malaysia<br>
<sup>3</sup>Cocoa Innovative and Technology Centre, Malaysian Cocoa Board, Lot 12621, 71800 Nilai, Negeri Sembilan, Malaysia<br>
<sup>4</sup>Academy of Language Studies, Universiti Teknologi MARA Pahang, Bandar Tun Abdul Razak, Jengka, Pahang, Malaysia<br>
<sup>5</sup>School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 NibongTebal, Penang, Malaysia<br>
<sup>6</sup>Solid Waste Management Cluster, Science & Engineering Research Centre, Engineering Campus, Universiti Sains Malaysia, Nibong Tebal, Penang, Malaysia
</p>
<p class="art-aff"><b>*Corresponding author: <?php $corresponding_author="Mohd Azmier Ahmad"; echo ($coauthor!="" && $coauthor==$corresponding_author)?"<a href='".$extpath."authors/".$courl."' target='_blank'>".$coauthor."</a>":$corresponding_author;?></b>, Associate Professor, School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia, Tel: +604 5996459, Fax: +604 5996908, E-mail: <a href="mailto:chazmier@usm.my">chazmier@usm.my</a>
</p>
<p class="art-aff"><b>Received:</b> March 23, 2017 <b>Accepted:</b> April 4, 2017 <b>Published:</b> April 10, 2017</p>
<p class="art-aff"><b>Citation: </b> Nikman KA, Ahmad F, Hassan
MS, Nikman K, Ahmad MA. Adsorption of
Chemically Prepared Cocoa Nibs Based
Activated Carbon Onto Methylene Blue: Equilibrium and Kinetic Studies. <i>Int J Petrochem Res.</i> 2017; 1(1): 15-18. doi: <a href="https://doi.org/10.18689/ijpr-1000104">10.18689/ijpr-1000104</a></p>
<p class="art-aff"><b>Copyright:</b> &copy; 2017 The Author(s). This
work is licensed under a Creative Commons
Attribution 4.0 International License, which
permits unrestricted use, distribution, and
reproduction in any medium, provided the
original work is properly cited.</p>
<p><a href="<?php echo $extpath;?><?php echo $jres['journal_link'];?>/ijpr-1000104.pdf" class="btn btn-danger pull-right" target="_blank">Download PDF</a></p>
</div>
<div class="articlecontent">
<p class="art-subhead">Abstract</p>
<p class="art-para">This study was aimed to prepare cocoa nibs based activated carbon (CNAC) via
chemical activation for methylene blue (MB) dye adsorption from aqueous solution. The
activation process was performed at 500&#176;C under inert condition using K<sub>2</sub>CO<sub>3</sub> as
activation agent. The effect of contact time and initial concentration of adsorbate on the
adsorption process were examined. Langmuir isotherm model fitted well the adsorption
equilibrium data with monolayer adsorption capacity of 64.98 mg/g at 30&#176;C. The
adsorption kinetic was found to follow the pseudo-second-order kinetic model.<br>
<br>
<b>Keywords:</b> Activated carbon, Chemical activation, Cocoa nibs, Methylene blue.</p>
<p class="art-subhead">Introduction</p>
 
<p class="art-para">Water pollution has become a highlighted issue as some of the industrial effluent is
directly discharged into the river and water bodies without proper treatment <a href="#1">[1]</a>. Dyes
effluent treatments from textile industries are divided into biological, physical and
chemical treatment processes. All these processes have different color removal
capabilities, capital costs and operating rates <a href="#2">[2]</a>. Physical treatment via adsorption
process using Agrowaste based activated carbon as adsorbent is among the most
efficient and cheap method for dyes removal. Several studies on agrowastes have been
employed to remove the contaminants such as methylene blue (MB) dye from the water
bodies <a href="#3">[3]</a> <a href="#4">[4]</a>. Agrowaste is appreciated as economical, sustainable and ecologically
friendly materials. In this study, an attempt was made to utilize cocoa nibs waste into
activated carbon using chemical activation process. The performance of CNAC was
studied in removing MB dye from aqueous solution.<br>
<br>
<b>Experimental</b><br>
<b>Chemicals</b><br>
All reagents and chemicals used in the research were analytical grade chemicals. For
impregnation process, potassium carbonate (K<sub>2</sub>CO<sub>3</sub>) was used. Commercial methylene
blue (C<sub>16</sub>H<sub>18</sub>ClN<sub>3</sub>S&#183;3H<sub>2</sub>O) (MB) textile dye was obtained from Sigma-Aldrich (M) 
Sdn Bhd<br>
<br>
<b>Preparation of Stock and Test Solutions</b><br>
Stock solution of MB with concentration of 500 mg/L was
prepared by dissolving approximately 0.50 g of MB in 1000 mL
distilled water. Test solution of MB ranging from 10 mg/L to
100 mg/L were prepared by subsequent dilution from stock
solution.<br>
<br>
<b>Production of Pellet</b><br>
The cocoa nibs waste was ground and sifted to a uniform
size of 0.5 mm or smaller. The samples were shaped into
pellets by compressing the mixture with a hydraulic press, in
which the cocoa nibs were compacted into pellets with a
specific density of 1.8 g/cm.<br>
<br>
<b>Preparation of Activated Carbon</b><br>
The carbonization was performed by placing approximately
60 g of cocoa nibs pellet in a vertical furnace, which contained
in a tubular stainless steel reactor. This step was carried outat
700&#176;C for 1 hour under purified nitrogen (99.99%) with flowrate
of 120 mL/min. Then, the furnace was allowed to cold to ambient
temperature. Char yield was determined using following
equation:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f001.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">where is the mass of char after carbonization process and
w<sub>i</sub> is the initial mass of cocoa nibs pellet. An amount of dried
char was added with K<sub>2</sub>CO<sub>3</sub> at various impregnation ratio (IR) in a 250 ml beaker. Both were mixed with deionized water to
dissolve the salt. The IR was calculated as follows:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f002.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">where wK<sub>2</sub>CO<sub>3</sub>
is the dry weight of potassium carbonate
pellets and w<sub>char</sub> is the dry weight of cocoa nibs char. The mixture
was then dehydrated in an oven at 105&#176;C for 24 hours. The
activation step was done using similar reactor as in carbonization
step but at final temperature of 500&#176;C under nitrogen flowrate of
120 mL/min for 2 hours. The sample was then cooled to room
temperature and washed with hot deionized water until the pH
of the washed solution reached 6.5-7.<br>
<br>
<b>Removal of MB by Batch Adsorption Study</b><br>
The batch equilibrium experiments of the adsorption
capacity studies were conducted at 30 &#176;C in a 250 mL conical
flask in a water bath shaker. The stock solution (1000 mg/L) of
MB was prepared by dissolving approximately weighed 1.0 gram
of the MB in 1000 mL of distilled water in a 1500 mL volumetric
flask. The stock solutions were stored in dark place to prevent
direct sunlight. The sample solutions were withdrawn at equilibrium
to determine the residual concentration. The concentrations of
the filtrates were measured using UV-Visible Spectrophotometer (Model Agilent Cary 60, USA).<br>
<br>
<b>Effect of Initial Concentration</b><br>
In order to study the effects of initial adsorbate concentration, 100 mL of adsorbate solutions with known initial concentration (10, 25, 50, 80, 100 mg/L of MB) were prepared in a series of
250 mL Erlenmeyer flasks. The amount of adsorbent that was
added into each flask was fixed at 0.1 g. The flasks were placed in an isothermal water bath shaker at temperature and
rotation speed of 30&#176;C and 120 rpm, respectively until
equilibrium point was reached.<br>
<br>
<b>Effect of Contact Time</b><br>
In order to study the effects of contact time on the
adsorption uptake, 100 mL of adsorbate solutions with known
initial concentration (10-100 mg/L) were prepared in a series
of 250 mL Erlenmeyer flasks. The amount of CNAC that was
added into each flask containing MB solution was fixed at 0.1
g. The flasks were then placed in an isothermal water bath
shaker of 30 &#176;C with rotation speed of 120 rpm for 360
minutes. The percent removal of adsorbate was calculated as
follows:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f003.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">Where C<sub>e</sub> is the concentration of adsorbate at equilibrium
and C<sub>i</sub> is the initial concentration of adsorbate. The MB uptake
at equilibrium is calculated as follows:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f004.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">where <em>m</em> is the mass of the adsorbent and V is the volume
of the adsorbate.<br>
<br>
<b>Adsorption Isotherm</b><br>
Adsorption isotherm study was carried out by fitting the
equilibrium data to three isotherm model which are the
Langmuir and Freundlich isotherm models, respectively
represented by Equations (5),(6) and (7). The applicability and
suitability of the isotherm equation to the equilibrium data
was compared by judging the values of the correlation
coefficients, R2. The Langmuir model is atypical model used to
measure the amount of adsorbate on an adsorbent at
equilibrium. The relation is expressed by following equation
<a href="#5">[5]</a>:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f005.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">where, qe is the amount adsorbed (mg/g), C<sub>e</sub> is the
equilibrium concentration of the metal ion (mg/L), q<sub>e</sub> is the
maximum amount of adsorbed metal ion per unit mass of
sorbent corresponding to complete coverage of the adsorptive
sites(mg/g), KL is the Langmuir constant related to the energy
of adsorption(L/mg)<br>
<br>
The Freundlich adsorption isotherm or Freundlich
equations are a relation between the concentrations of a
solute on the surface of an adsorbent, to the concentration of
the solute in the liquid with which it is in contact. The
relationship is stated as follows <a href="#6">[6]</a>:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f006.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">In this equation, q<sub>e</sub> (mg/g) is amount of adsorbed material
in adsorbent surface k in arrangement are adsorption capacity
and adsorption intensification.<br>
<br>
<b>Kinetic Model</b><br>
The kinetics of adsorption describes the rate of adsorbate
uptake on activated carbon prepared and it controls the
equilibrium time. The kinetics of adsorbate uptake is required for
selecting optimum operating conditions for the full-scale batch
process. Therefore, models for liquid-phase adsorption such as
pseudo-first-order and pseudo-second-order were used to
analyze the adsorption kinetic data. The pseudo-first-order kinetic
model equation of Largergren <a href="#7">[7]</a> is generally expressed as:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f008.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-para">Where q<sub>e</sub> is the amount of adsorbate adsorbed at
equilibrium (mg/g), qt is the amount of solute adsorb per unit
weight of adsorbent at time (mg/g), k<sub>1</sub> is the rate constant of
pseudo-first order sorption (1/h). The pseudo-second-order
equation is expressed as <a href="#8">[8]</a>:</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-f009.gif" class="img-responsive center-block"/></div>
<!-- Table -->
<p class="art-subhead">Results and Discussion</p>
 <p class="art-para"><b>Effect of contact time and MB initial concentration on
adsorption equilibrium</b><br>
Figure 2 and Table 1 show the effect of various initial
concentrations on adsorption of MB by CNAC. An equilibrium
time of 100 min was needed for MB dye solution with initial
concentrations of 10-25 mg/l to reach equilibrium. However, for initial concentrations of 50-100 mg/l, longer equilibrium
times of 22-24 hours were required for the system to reach
equilibrium. Initially, adsorbate molecules have to first
encounter the boundary layer effect. Then it has to diffuse
from boundary layer film onto adsorbent surface and finally, it
has to diffuse into the porous structure of the adsorbent <a href="#10">[10]</a>. The ratio of the initial number of dye molecules to the
available surface area was low at lower initial concentration
compared to higher initial concentration. Therefore, MB
solution with higher initial concentration would take relatively
longer contact time to attain equilibrium due to the higher
amount of MB molecules.</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-g002.gif" class="img-responsive center-block"/></div>
<p class="text-center">Figure 2: Effects of contact time of MB onto CNAC</p>
<!-- Table -->
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-t001.gif" class="img-responsive center-block"/></div>
<p class="text-center">Table 1: MB percent removal by CNAC with IR 3:1</p>
<!-- Table -->
<p class="art-para"><b>Effect of IR on adsorption equilibrium</b><br>
Fig. 1 shows the influence of IR on CNAC in removing MB. Sample impregnated with 2:1 ratio has the lowest capability
to adsorb the adsorbate where the value is 27.8 mg/g.</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-g001.gif" class="img-responsive center-block"/></div>
<p class="text-center">Figure 1: Effect of IR on MB uptake</p>
<!-- Table -->
<p class="art-para">The adsorption capacity of CNAC was decreased with
increased in IR from 1:1 to 2:1 before increased at IR of 3:1. CNAC with 3:1 ratio managed to adsorb 30.9 mg/g of MB at
equilibrium. Higher IR was favorable for enhancing the MB
adsorption as more pores are developed on the sample
surface <a href="#9">[9]</a>.<br>
<br>
<b>Adsorption Isotherm</b><br>
The most appropriate correlation for the equilibrium
curve needs to be established in order to understand the
adsorption system. Therefore, the equilibrium adsorption
data were analyzed using the Langmuir and Freundlich
isotherms as shown in Figure 3 whereas Table 2 summarizes
all the constants from both isoterm models.</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-g003.gif" class="img-responsive center-block"/></div>
<p class="text-center">Figure 3: Linear plots of (a) Langmuir and (b) Freundlich adsorption
models</p>
<!-- Table -->
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-t002.gif" class="img-responsive center-block"/></div>
<p class="text-center">Table 2: Parameters of Langmuir and Freundlich adsorption
isotherm for MB.</p>
<!-- Table -->
<p class="art-para">Langmuir model gave the highest R<sup>2</sup> values which were
greater than 0.96. Conformation of the experimental data into
the Langmuir isotherm equation proved that the surface of
CNAC for MB adsorption was made up of homogeneous
adsorption patches with monolayer coverage of MB onto
CNAC <a href="#9">[9]</a>. The monolayer saturation capacity of CNAC was
found to 64.98 mg/g at 30 &#176;C.<br>
<br>
<b>Adsorption Kinetics</b><br>
All the experimental and calculated qe values obtained
from the pseudo-first-order and pseudo-second-order kinetic
model for adsorption of MB at 30 &#176;C are tabulated in Table 3. Comparing the R<sup>2</sup> values, pseudo-second-order model
showed a significant agreement with adsorption mechanisms, which indicated the chemisorption with the heterogeneous
active sites occurred on the surface of CNAC <a href="#11">[11]</a>.</p>
<!-- Table -->
<div class="art-img">
<img src="<?php echo $imgpath;?>images/IJPR-2017-104-t003.gif" class="img-responsive center-block"/></div>
<p class="text-center">Table 3: Parameter values of the kinetic studies of the adsorption of
MB onto CNAC.</p>
<!-- Table -->
<p class="art-subhead">Conclusion</p>
<p class="art-para">CNAC was found to be suitable for the removal of MB
from aqueous solution. Adsorption of MB was found to
increase with increase in contact time and initial dye
concentration. The Langmuir isotherm model was well
described by the equilibrium data with maximum adsorption
capacity of 64.98 mg/g. The pseudo-second-order kinetic
model fits well with the kinetic data.</p>
<p class="art-subhead">Acknowledgment</p>
 <p class="art-para">The authors are grateful for the funding from Solid Waste
Management Cluster, USM (1001/CKT/870023) and research
grant from Ministry of Science, Technology and Innovation (MOSTI), Malaysia.</p>
<div style="clear:both"></div>
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</ol>   
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