Preparation and Characterization of Chitosan with Activated Carbon

as Adsorbent to Reduce Level Metal Cadmium (Cd) and Nickel (Ni)

Fitri Purnama Sari1, Harry Agusnar2* and Muhammad Taufik2

1Postgraduate Chemistry Study Program, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara,
Jl. Bioteknologi No. 1 Kampus USU, Medan, Indonesia
2
Department of Chemistry, Faculty of Mathematics and Natural Sciences, Universitas Sumatera Utara,
Jl. Bioteknologi No. 1, Medan 20155, Indonesia

Keywords: Activated Carbon, Cadmium, Chitosan, Coffee Ground, Nickel.

Abstract: Preparation and characterization of chitosan with activated carbon have been made with the aim of reducing
the metal content of Cadmium (Cd) and Nickel (Ni) in standard solutions. Characterization chitosan with
activated carbon by FT-IR, SEM, and test adsorption by using AAS. Characterization of chitosan and
chitosan - activated carbon by FT-IR shows that there is no difference in wavelength: as for the emerging
groups, NH groups (3448.72 cm-1), CH groups (2924.09 cm-1), C = C groups (1635.64 cm-1), C-N group
(1381 cm-1), and NH group (3441.01 cm-1). SEM characterization on chitosan - activated carbon shows a
rude surface. Absorptions of Cd and Ni in chitosan that best with addition carbon of 0.6 g that is 74.54%
and 73.43%.

1 INTRODUCTION According to the International Board for cancer

study, cadmium is known as carcinogenic (Jeon,
Industrial activities which are rapidly developing 2017) . It is accumulated in human kidneys and
have made the contamination of heavy metal ion in liver, and it can cause various diseases such as
water increase. This condition has caused serious kidney dysfunction, hypertension, diarrhea,
environmental problem throughout the world (Li et stomach-ache, and bone disorder (Pal and Pal,
al., 2016). Heavy metal from industrial waste such 2017). Waste which contains cadmium metal comes
as lead, copper, and cadmium can pollute water, sea from electroplating industry, the making of batteries,
level, and soil. The International institution has pesticides, and mining which bring about water, air,
confirmed that cadmium is latent metabolic poison and soil pollution (Al-Malack and Dauda, 2017).
since it is very dangerous for the life of organism There are several methods used to remove heavy
and can affect human health. metals from wastewater is precipitation, membrane
Electroplating industry has significant risk for filtration, ion exchange (Hegazi, 2013). The
environment and human beings because wastewater adsorption method is the most commonly used
contains heavy metal ion which is not biodegradable because it is more efficient, more economical and
and tends to be accumulated in living organism uses cheap natural adsorbents (Li et al., 2016).
which causes toxic effect or carcinogenic. One of the Chitosan is poly-(2-amino-2-deoxy-β-(1-4)-D-
contents found in electroplating waste is nickel glucopyranose) with the molecule formula of
metal; this metal is usually used in electroplating (C6H11NO4)n which can be obtained from chitin
industry due to its anti-corrosion (Raja Sulaiman et deacetylation (Rahate, 2013).
al., 2018). Nickel is a silver white, hard and ductile Its molecular weight between 300 – 1000 kDa.
metal. Ni normally forms cubic crystal lattice Chitosan produced from crustacean shell such as
(Coman et al., 2013). Nickel is used for production crab and shrimp. These shells contain 30 – 40
of stainless steel, nonferrous alloys and anticorrosion proteins, 30 – 50% calcium carbonate and 20-30%
and temperatures resistance properties.(Reck et al., chitin. Chitosan is natural chelating make chitosan
2008) useful in wastewater treatment by allowing for the
binding and removal of metal ions such as copper,

280
Purnama Sari, F., Agusnar, H. and Taufik, M.
Preparation and Characterization of Chitosan with Activated Carbon as Adsorbent to Reduce Level Metal Cadmium (Cd) and Nickel (Ni).
DOI: 10.5220/0008921802800286
In Proceedings of the 1st International Conference on Chemical Science and Technology Innovation (ICOCSTI 2019), pages 280-286
ISBN: 978-989-758-415-2
Copyright c 2020 by SCITEPRESS – Science and Technology Publications, Lda. All rights reserved
 Preparation and Characterization of Chitosan with Activated Carbon as Adsorbent to Reduce Level Metal Cadmium (Cd) and Nickel (Ni)

lead, mercury, and uranium from wastewater. polysaccharide, and chlorogenic acid (Pujol et al.,
Chitosan (Figure 1) has advantages such as 2013).
biodegradability, natural origin, abundance, The ingredients which can be used for carbon are
reactivity. It has many application include medical, tea, coffee grounds, and rice husk. Carbon from active
agricultural, food processing, nutritional charcoal can absorb inorganic contaminants (Djati
enhancement, cosmetics and waste and water Utomo, 2015). Carbon from active charcoal is usually
treatment. (Paridah et al., 2016). used for absorbent since it is flexible and more
effective; besides that, it has wider surface and good
capacity to decrease metal and the other poisonous
compounds (Salehi et al., 2016) (Zhang et al., 2016).
(Hernández Rodiguez et al., 2018) reported that
adsorption of Nickel from aqueous solutions of
activated carbon from spent coffee. Activated carbon
is effective adsorbent for decrease concentrations of
metal ions in aqueous solutions. These adsorbents
Figure 1: Chemical structure chitosan. have high amount of micropores and mesopores,
large surface area.
Chitosan is absorbent which is very effective to
remove heavy metal ion because chitosan structure
has abundant hydrophilic hydroxyl group and 2 MATERIALS AND METHODS
polycationic amine group which can bind metal
(Ahmad et al., 2017). Among various natural 2.1 Material
polymers, chitosan is the second largest biopolymer
in nature after cellulose (Choi et al., 2016). It is a All materials used in this research were of chitosan,
very effective natural polymer which can be used as acetate, aquadest, NaOH, activated carbon, standard
absorbent because it is biodegradable (Ahmad et al., solution of Cd2+ 1000 mg/L, and standard solution of
2017) and not poisonous (Choi et al., 2016); it also Ni2+ 1000 mg/L.
has bio-compatibility (Liu and Bai, 2014) and
bioactivity (Vakili et al., 2014). 2.2 Methods
Chitosan has several weakness is mechanical
properties and low thermal stability, porosity and 2.2.1 The Making of Chitosan
small surface area. Vakili et al., 2014 modified the
structure of chitosan into chitosan beads, membranes Chitosan 1.2 grams of, dissolved with 3% of acetate,
and films, to improve adsorption ability, physical about 60 mL, and stirred until it became
and mechanical properties. Liu and Bai, 2014 homogenous. It was then poured into acrylic glass
explained that modifying chitosan into semi-IPN and dried up in a oven at the temperature of 600C
(Interpenetrating Network) hydrogel, nano-magnetic within 24 hours. The result was immersed with
particles, chitosan grafting polymers, and chitosan NaOH 1M within 24 hours. It was then removed
composites can improve chitosan adsorption ability. from the acrylic glass and washed with aquadest
Coffee is the most common drink which is until it was neutral. Finally, it was dried up in room
consumed throughout the world. It reaches 400 temperature and stored in desiccators. yielded
billion glasses per year and produces around 8,000 absorbent was analyzed by FT IR, SEM, and tensile
tons of coffee grounds per year. Coffee ground is strength testing.
still considered as waste since it takes a very long
time to be decomposed, compared with the other 2.2.2 The Making of Chitosan – Activated
types of waste (Zein et al., 2017). Carbon
One of the advantages of coffee grounds is that
they can be used as absorbent, tannin compounds Chitosan 1,2 g, dissolved with 3% of acetate about
which contain polyhydroxy and polyphenol groups 60 mL, added by 0.3 gram of activated carbon,
which can be bound with metal cation which forms stirred until it was homogenous, poured into acrylic
chelate (Utomo and Hunter, 2006). Besides that, glass, dried up in an oven at the temperature of 600C
coffee grounds also contain carbon, nitrogen, within 24 hours. The result was immersed with
lipophilic compound, ethanol, lignin, alkaloid, NaOH 1M within 24 hours. It was then removed
from acrylic glass and washed with aquadest until it

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was neutral. Finally, it was dried up in room In the wavelength of 1381.03 cm-1 there was C-N
temperature and stored in desiccators. The yielded functional group (Omidi and Kakanejadifard, 2019) .
absorbent was analyzed by FT IR, SEM and tensile There was C-H bound in –CH2 in the wavelength of
strength testing. The same treatment was done with 2924.09 cm-1. In the wavelength of 1635.64 cm-1
the variation of weight of additional carbon of 0.4, there was vibration peaks of C=O of secondary
0.5, and 0.6 g. amide group. In the wavelength of 1084.14, 1033.85
cm-1 there was asymmetrical vibration from C-O
2.2.3 The Use of Chitosan and Chitosan – functional group (Paluszkiewicz et al., 2011).
Activated Carbon as Adsorbent to The result of the analysis on FI-IR spectrum in
Decrease the Concentration of chitosan and chitosan-active carbon of coffee
Cadmium (Cd) and Nickel (Ni) grounds showed that there was the peaks of
absorption in the wavelength of 3749.62 cm-1 which
Chitosan adsorbent and chitosan-activated carbon indicated the existence of OH strain vibration, in the
were used to decrease the content of Cd and Ni wavelength of 3448.72 cm-1 which indicated the
metal in standard solution. Chitosan and chitosan- existence of N-H strain vibration, in the wavelength
activated carbon were put into column. About 50 mL of 2924.09 cm-1 which indicated that there was C-H
of Cd and Ni standard solution was sucked by a group of aliphatic chain, in the wavelength of
straw, and it was then skipped from the column with 1635.64 cm-1 which indicated that there was C=O
vacuum pump, and the solution was collected to be group from secondary amide, and in the wavelength
analyzed by using AAS (Atom Absorption of 1381.03, 1084.14, 1033.85 cm-1 which indicated
Spectrophotometer). The same treatment was done that there were C-N and C-O groups.
for chitosan-activated carbon of coffee grounds with
the variation of weight 0.4, 0.5, and 0.6 g. Table 1: Functional group of chitosan and chitosan –
activated carbon.
Functional
Sample Wavenumber (cm-1)
3 RESULTS AND DISCUSSIONS Groups
Chitosan 3749.62 OH
3.1 Characterization of Chitosan and 3448.72 N-H
2924.09 C-H
Chitosan – Activated Carbon 1635.64 C=O
1381.03 C-N
The peaks which appeared in the FT-IR spectrum 1084.14
was showed in the Figure 2 and Table 1. C-O
1033.85
50

45
Chit Chit-Activated
Chit-Activated Carbon 386.35 OH
Carbon
40
3448.72 N-H
35
2924.09 C-H
30 1635.64 C=O
25
1381.03 C-N
%T

10722.42
20 C-O
1033.85
15

10 In the spectrum of chitosan and chitosan added

5
by active carbon adsorbent of coffee grounds, there
was no difference in wavelength which indicated
0
4000 3500 3000 2500 2000 1500 1000 500 that physical interaction occurred between carbon
Wavelengths (cm )
-1
and chitosan.
Figure 2: FT-IR Spectrum of Chitosan and Chitosan-
Activated Carbon. 3.2 Characterization of Chitosan and
Chitosan – Activated Carbon with
Based on FT-IR spectrum in chitosan, there was SEM
OH functional group in the wavelength of 3749.62
cm-1 and strain vibration of N-H primary amine in Chitosan adsorbent (Figure 3) characterized by SEM
wavelength of 3448.72 cm-1 (Boggione et al., 2017). was aimed to find out its morphology.

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 Preparation and Characterization of Chitosan with Activated Carbon as Adsorbent to Reduce Level Metal Cadmium (Cd) and Nickel (Ni)

3.2.1 Morphological Analysis of Chitosan Table 2: Tensile strength of chitosan and chitosan –
with SEM activated carbon.
Sample Tensile Strength (MPa)
Chitosan 2.266
Chit – C 0.3 g 3.392
Chit – C 0.4 g 3.924
Chit – C 0.5 g 2.123
Chit – C 0.6 g 1.927

Figure 3: Image of SEM on Chitosan adsorbent surface

with enlargement (A) 64x, (B) 200x and (C) 500x.

Chitosan morphological adsorbent was not fine

enough and homogenous because chitosan was not
distributed equally with acetate solvent. This
condition caused the establishment of clump, but it
could also be caused by air bubble which was
trapped during the mould of adsorbent.

3.2.2 Morphological Analysis of Chitosan

with SEM Figure 5: Tensile Strength.

As in Table 2 and Figure 5, chitosan without the

addition of carbon have tensile test strength of 2.266
MPa, and chitosan with the addition of variations in
the weight of activated carbon have different tensile
strength tests. Chitosan with 0.3 g of carbon addition
has a tensile strength of 3.392 MPa, addition 0.4
Figure 4: Image of SEM on Chitosan – activated carbon carbon is 3.924 MPa, addition 0.5 g carbon is 2.123
Surface with Enlargement (A) 5.000 times, (B) 10.000 MPa, addition carbon 0.6 is 1.927 MPa.
times and (C) 15.000 times. Optimum tensile strength results in chitosan with
the addition 0.4 g carbon. Tensile strength test
The result of chitosan morphology with the results have increased with the addition of activated
addition of active carbon could be seen in Figure 4. carbon. activated carbon from coffee ground acts as
Rough surface and some undistributed carbon an reinforcing agent due to the non-electrostatic
particles were caused by the process of making interactions that are bound between activated carbon
adsorbent was not homogenous. The addition of and chitosan (Lessa et al., 2018). Addition activated
active carbon to chitosan adsorbent influenced the carbon more than 0.4 g, the tensile strength has
smoothness of the surface and the compatibility of decreases. that with increasing carbon concentration
the arranging materials (Lessa et al., 2018). in chitosan composites it will reduce the value of
tensile strength.
3.3 Characterization of Chitosan and
Chitosan – Activated Carbon 3.4 Analysis Samples with Atomic
Absorption Spectrophotometer
Tensile strength testing in this research aims to (AAS)
determine the tensile strength of chitosan and
chitosan - activated carbon. The result of the tensile In this research, before the sample analysis was
test from the processing of chitosan and chitosan - carried out, we examined the sensitivity and linearity
activated carbon samples with a variation of the of atomic absorption spectrophotometer (AAS)
weight of carbon addition of 0.3, 0.4, 0.5 and 0.6 g. instruments with equipment operating conditions
such as Table 3 and Table 4 below:

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Table 3: Conditions for AAS instruments Shimadzu type

AA-7000 on measurement of concentration Cadmium
(Cd).
Parameter Cadmium (Cd)
Wavelength (nm) 228,8
Flame Air – C2H2
Burning gas flow rate 1,8
(L / min)
Air flow rate (L / min) 15,0
Gap Width (nm) 0,7
Furnace Heigth (nm) 7
Figure 6: Calibration Curve of Standard solution
Cadmium.
Table 4: Conditions for AAS instruments Shimadzu type
AA-7000 on measurement of concentration Nickel (Ni).
Based on the calibration curve above (Figure 6),
Parameter Nickel (Ni) the correlation coefficient (r) is 0.999, indicating that
Wavelength (nm) 232 the instrument used has a good response.
Flame Air – C2H2
Table 6: Absorbance Linearity Test of Nickel (Ni).
Burning gas flow rate 1,8
(L / min) Concentration (ppm) Absorbance
Air flow rate (L / min) 15,0 0 0,056
Gap Width (nm) 0,7 0,2 0,0234
Furnace Heigth (nm) 7 0,4 0,0441
0,6 0,0672
Based on Tables 3 and 4 above the wavelength 0,8 0,0857
for the measurement of nickel and cadmium is 1 0.1044
different, the use of cathode lamps that are suitable
for the metal to be analyzed. The cathode lamp will
emit radiation energy that corresponds to the energy
needed for the transition of atomic electrons. With
giving a voltage to a certain current the metal begins
to glow and the cathode metal atom will be
evaporated by sprinkling. The atom will be excited
then emit radiation at a certain wavelength.

3.4.1 Linearity Test

Linearity test aims to determine the correlation
Figure 7: Calibration Curve of Standard solution Nickel.
between the concentration of standard solutions with
the response/signal from the absorbance instrument.
In this research evaluation is done by making a Based on the calibration curve above (Figure 7),
calibration curve (concentration of standard solution the correlation coefficient (r) is 0.999, indicating that
versus absorbance solution) can be seen in the Table the instrument used has a good response.
5:
3.5 Analysis on Measuring Cadmium
Table 5: Absorbance Linearity Test of Cadmium (Cd). Metal
Concentration (ppm) Absorbance The result of measuring Cd concentration in the
0 0,0100
samples with AAS could be seen in the following
0,2 0,1203
Table.
0,4 0,2366
0,6 0,3509
0,8 0,4587
1 0,6773

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 Preparation and Characterization of Chitosan with Activated Carbon as Adsorbent to Reduce Level Metal Cadmium (Cd) and Nickel (Ni)

Table 7: Result of Measuring Cd Concentration in the result of their research, it was reported that chitosan
Samples with AAS. which has been coated with active carbon increased
Sample Abs Concentration % its percentage (%) of absorptive power on cadmium
(ppm) Adsorption metal (Hydari et al., 2012).
Chit 0,5571 0,9764 51,17 % Activated carbon is commonly used as adsorbent
Chit – C 0,3 g 0,4414 0,7769 61,52 % to absorb metal because it has high capacity to
Chit – C 0,4 g 0,3734 0,6480 67,59 % absorb and has good endurance against abrasion.
Chit – C 0,5 g 0,3089 0,5327 73,36 % Active carbon has porous structure and wide surface.
Chit – C 0,6 g 0,2957 0,5091 74,54 % (Obregón-Valencia and Sun-Kou, 2014) reported
that active carbon was able to absorb cadmium metal
Based on the data in Table 7, it was found that because it had high chemical reactivity. The use of
the largest amount of Cd metal absorption was in the commercial active carbon is limited since its price is
chitosan with the addition of 0.6 gram carbon relatively high. Active carbon is very effective
(74.54%), while the least amount of Cd metal adsorbent in absorbing metal in waste water because
absorption was in the chitosan without the addition of its large number of micropores and mesopores, its
of carbon (51.1%). wide surface, and its big pores, and the functional
The result of measuring Ni concentration in the group on its surface interacts with heavy metal ion
samples with AAS could be seen in the following (Hernández Rodiguez et al., 2018). Carbon has the
Table. capacity to absorb metal because it has large pores.
The more the in its pores so that metal content in
Table 8: Result of Measuring Ni Concentration in the chitosan decrease by adding more carbon.
Samples with AAS.
Sample Abs Concentration %
(ppm) Adsorption
Chit 0,0897 0,8450 57,71 %
4 CONCLUSIONS
Chit – C 0,3 g 0,0721 0,6706 66,46 %
Chit – C 0,4 g 0,0682 0,6318 68,40 % Chitosan and chitosan-active carbon can be used as
Chit – C 0,5 g 0,0609 0,5590 72,03 % adsorbent to decrease Cd and Ni metal content. The
Chit – C 0,6 g 0,0581 0,5313 73,43 % best decrease in Cd metal content is found in
chitosan by adding 0.6 g carbon (75.45%) and the
Based on the data in Table 8, it was found that best decrease in Ni metal content is found in
the largest amount of absorption of Ni metal was in chitosan by adding 0.6 g carbon (73.43%).
the chitosan adsorbent with the addition of 0.6 gram
of active carbon (57.71%). The amount of active
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