Preparation of Activated Carbon from
The surface area of activated carbon is
coconut shells for simplified water
purification system
-Nishanth CB, Siddhesh Borkar, Rohit Dash, Naman
Jain, Deepak Kumar
Department of Chemical Engineering, NIT Rourkela,
Odisha, India
Abstract
In this work, an attempt was made to prepare activated
carbon from sun-dried coconut shells as the precursor
using laboratory apparatus and experimentation scale
heating equipment as a product development project.
Considering the time, equipment available and product
scale, the chemical activation method was chosen to
prepare the activated carbon. A sample of
commercially available activated carbon was obtained
and used as a standard against which we compared our
prepared sample for certain key characteristics and
performed tests to determine the relative performance
of our product. The physical parameters measured for
our sample were bulk density, ash content, and fixed
carbon content among others. The adsorption
performance was checked by testing on methylene
blue dye solutions and determining Iodine number.
The prepared carbon sample would then be used as the
purifying agent in a mechanically operated portable
water purifier.
Introduction
Activated carbon, sometimes also called activated
charcoal, is a form of carbon processed to have small,
low-volume pores that increase the surface area
available for adsorption or chemical reactions.
Activated carbons are manufactured from coconut
shell, peat, hard and soft wood, lignite coal, bituminous
coal, olive pits and various carbonaceous specialty
materials. Chemical activation or High Temperature
Steam Activation mechanisms are used in the
production of activated carbons from these raw
materials.
The intrinsic pore network in the lattice structure of
activated carbons allows the removal of impurities
from gaseous and liquid media through a mechanism
referred to as adsorption.
Key Properties
 Surface Area - Generally, higher the internal
surface area, higher the effectiveness of the
carbon.
impressive, 500 to 1500 m2/g or even more
 Total Pore Volume - Refers to all pore spaces
inside a particle of activated carbon. It is
expressed in millilitres per gram (ml/g). Total
pore volume (T.P.V.) differs by raw material
source and type of activation method
 Pore Volume Distribution - Each type of carbon
has its own unique distribution of pore sizes.
They're referred to as micropores, mesopores
and macropores. Carbons for adsorbing many
types of gas molecules are microporous. The
best carbons for decolorization have a higher
distribution of mesopores.
Micropores r < 1nm
Mesopores r 1-25nm
Macropores r > 25nm
Methods of Activation
Steam activation is the most widely used process
because it is generally used to activate both coconut
shell and coal based carbons. Firstly, the raw material,
is carbonized by heating in an inert atmosphere such as
flue gas, so that dehydration and devolatilization of the
carbon occurs. For this stage temperatures usually do
not exceed 700 C. Carbonization reduces the volatile
content of the source material to under 20%. A coke is
produced which has pores that are either small or too
restricted to be used as an adsorbent.
The second stage is the activation stage which enlarges
the pore structure, increases the internal surface area
and makes it more accessible. The carbonized product
is activated with steam at a temperature between 900C
and 1100C. The chemical reaction between the carbon
and steam takes place on the internal surface of the
carbon, removing carbon from the pore walls and
thereby enlarging the pores. The steam activation
process allows the pore size to be readily altered and
carbons can be produced to suit specific end-sues. For
an example, the pore structure has to be opened up
more for the adsorption of small molecules from a
solution, as in water purification, than for the
adsorption of large colour molecules in sugar
decolourization.
Chemical Activation is generally used for the
production of activated carbon from coconut shells,
sawdust, wood or peat. Chemical activation involves
mixing the raw material with an activating agent,
usually strong acids (H3PO4), bases (KOH) or acidic salts
(ZnCl2, FeCl3). The paste of raw material and the
activating agent is dried and then carbonized, usually
in a rotary kiln, at a relatively low temperature of 400C
to 500C. On carbonization, the chemical acts as a
support and does not allow the char produced to
shrink. It dehydrates the raw material resulting in the
charring of the carbon, creating a porous structure and
an extended surface area.
Activity is controlled by altering the proportions of raw
material to reagent used. This is called impregnation
ratio. Activity increases with higher reagent
concentration and is also affected by the temperature
and residence time in the kiln.
Activated carbons produced by this method have a
suitable pore distribution to be used as an adsorbent
without further treatment. This is because the process
used involves an “acid wash” which is used as a
purifying step in steam activated carbons, post
activation. Chemically activated carbons, however,
have a lower purity than specifically acid-washed
steam activated carbons.
Equipment and Materials used
 Equipment
o Hot air oven
o Incubator
o Muffle Furnace
o Magnetic Stirrer
 Materials
o Commercially available activated carbon
o Sun-dried coconut shells
o Chemicals:
 Potassium Hydroxide Pellets
 Sulphuric Acid, Hydrochloric Acid
 Potassium Iodide
 Iodine(resublimated)
 Sodium Thiosulphate, Sodium Carbonate
 Starch
 Methylene Blue
Method of Preparation of Activated Carbon
1. The hemispherical coconut shells were
hammered down to tiny pieces and placed in
the hot air oven at 120C for 24 hours. The oven
took about 45 minutes to heat up.
2. The pieces were cooled to room temperature.
For the chemical activation process, 5 grams of
KOH was dissolved in 100ml distilled water
along with 10 grams of the sample. The mixture
was placed in the hot air oven for another 24
hours at 90C.
3. To remove the water content, the sample was
once against dried in the hot air oven for 24
hours at 110-120C.
4. The dried sample was then put in a crucible and
placed in a muffle furnace at 600C for 90
minutes. The furnace took about 55 minutes to
preheat. The furnace was then switched of and
the sample was left undisturbed for another 12
hours.
5. The sample was washed with warm water at
80C for 2 hours and the solution’s pH (12-14)
was noted. The water was filtered out.
6. The next washing was done with 0.05N HCl for
1 hour at room temperature. The pH drops
down to 2-3. The acid was again filtered out.
7. The sample was washed with distilled water at
room temperature for 2 hours and its pH was
checked. The washing was continued till a
neutral pH range of 6-7 was achieved.
8. The entire mass of carbon was filtered out
carefully and placed in a foil covered beaker and
kept in the hot air oven to remove any
remaining moisture.
9. After 24 hours, the activated carbon was ready.
Most of it was powdered with some granules
present as well.
Characterization
 Bulk Density: Bulk density is defined as weight
per unit volume of material. It is basically used
for the powder of materials. This test of bulk
density represents the flow consistency and
packaging quantity of solid sample. It is
expressed in terms of kilograms per cubic meter
(kg/m³)
First the mass of the measuring cylinder was
determined. Our sample of activated carbon
was then placed into this cylinder and
reweighed.
(𝑚2 − 𝑚1 )
𝐷=
𝑣
m1= mass of measuring cylinder in grams
m2= mass of measuring cylinder + its contents
v= volume of the measuring cylinder in litre
 Moisture Content: Small amount of the
activated carbon sample weight was measured
and then taken in a petri dish. It was spread
evenly on the dish. It was then heated in an
oven at a temperature of (105-110) ˚C for
90mins. The petri dish was left open during
heating process. After heating petri dish was
removed and cooled in a desiccator. After
 cooling the weight of dried sample was and known amounts of activated carbon were added
measured. and placed in the incubator. The commercially
available sample and our prepared sample were kept
Moisture: side by side and compared after regular intervals.
(𝐵 − 𝐹) To obtain parameters of practical use, test conditions
𝑀= × 100
(𝐵 − 𝐺) including a) Temperature b) Incubator Shaking RPM
and c) Amount of Carbon added were varied and the
B=weight of petri dish +original sample solutions were qualitatively compared.
F=weight of petri dish+ dried sample We observed that our prepared sample was able to
G= weight of petri dish adsorb the dye in some capacity, however, the results
 Ash Content: 1 g of the sample was taken in a would only be visible after a period of sedimentation.
silica crucible. It was heated in a muffle furnace The possible reason for this is due to the large fraction
to 750˚c for 90mins. During this heating process of impurities and ash content present in our sample.
the crucible was left open. After the required When agitated, these impurities would disperse
heating, the crucible was cooled in a desiccator through the bulk of the solution and impart a blackish
and then weight of the ash was measured. color that would hide the performance of the useful
activated carbon particles. Nevertheless, after an
Ash: extended period of sedimentation followed by
(𝐹 − 𝐺) filtration, the adsorption potency of the prepared
𝐴= × 100
(𝐵 − 𝐺) samples was clearly visible.

Iodine Number Test

G=Mass of empty crucible
B=Mass of crucible + sample
F=Mass of crucible+ ash sample
 Volatile Matter Content: A known quantity of
the sample was taken in a cylindrical crucible
closed with a lid. It was then heated to 925˚c for
exactly 7minutes in a muffle furnace. The
crucible was cooled in a desiccator and
weighted. Volatile matter on dry basis:
[100 × (𝐵 − 𝐹) − 𝑀 × (𝐵 − 𝐺)]
𝑉= × 100
[(𝐵 − 𝐺) × (100 − 𝑀)]
B=Mass of crucible, lid and sample before
heating
F=Mass of crucible, lid and contents after
heating
G=Mass of empty crucible & lid
M=percentage of moistures determined above
Adsorption Test
One of our primary tests to check the performance of
our prepared activated carbon was the adsorption test.
Activated carbons, due to their large surface area and
intricate pore structure, are well known for the
adsorption of colors, organic matter, certain gaseous
compounds and also some inorganic salts.
The test that would give the most reliable qualitative
and visible results is adsorption of the dye compounds
from a dye solution. The dye used was methylene blue.
Dye solutions of known concentrations were prepared
The second test to check the performance of the
sample was the Iodine number test. This test method
covers the determination of the relative activation
level of unused or reactivated carbons by adsorption of
iodine from aqueous solution. The amount of iodine
absorbed (in mg) by 1 g of carbon using test conditions
listed herein is called the iodine number. The iodine
number is a relative indicator of porosity in an
activated carbon. It does not necessarily provide a
measure of the carbon’s ability to adsorb other species.
Iodine number may be used as an approximation of
surface area for some types of activated carbons.
The two main solutions required for the test are 0.1N
Iodine solution and 0.05N Sodium Thiosulphate
solution. The former is made by weighing 4g of
Potassium Iodide in a glass stopped flask and dissolving
it in a minimum amount of distilled water. 1.27g of
resublimated Iodine is added and the solution is shaken
till all the solids are dissolved. 2 drops of 37% HCl is
added to stabilize the further reactions and the
solution is made up to 100ml by adding distilled water.
The latter is made by dissolving 0.5g of Sodium
Thiosulphate and 20mg of Sodium Carbonate in 100ml
distilled water. The solution is then diluted to 0.05N.
10ml of the Iodine solution was taken in a conical flask,
2 drops of starch solution were added and was titrated
against the thiosulphate solution till the color
disappeared. This was the blank reading (B). 40ml of
the iodine solution was taken in a flask, 0.2g of the
activated carbon sample was added and shaken for five
minutes for the Iodine to be absorbed. The solution
was filtered and 10ml was again titrated against the
thiosulphate solution. The volume of the thiosulphate
solution consumed is the activated carbon reading (A).
127 × 0.1 × 40 × (𝐵 − 𝐴)
𝐼𝑛=
0.2 × 𝐵
Discussion
1. Physical-Properties:
Bulk Density: The bulk density of the prepared
sample was found to be 0.67 g/cm3. The literature
value for the same for activated carbon from
coconut shells is 0.58 g/cm3. This elevated value
could be attributed to the presence of ash in the
sample. Ash being lightweight and practically
inseparable without harsh conditions adds to the
bulk density.
Proximate Analysis: The proximate analysis is a
basic test performed on samples containing a high
carbon percentage. The higher the fixed carbon
content, the purer the sample. Ash is an impurity
and adds to the mass and bulk density without
contributing much to the parameters of practical
use. The tests were performed on the prepared
sample and literature values were taken for the
commercially available activated carbon.
The results were as follows:
a. Moisture-content: 4.3%, 2.2%
b. Volatile-matter-content: 10.6%, 7.4%
c. Ash-Content: 8.2%, 1.5%
d. Fixed-Carbon-content: 76.9%, 88.9%
The second set of values are the literature values
of a general activated carbon sample derived from
coconut shells. The ash content in our sample was
much greater than that of the standard sample
because of the difficulty in washing the sample
without losing out on yield. Moisture content was
also higher probably because of the repeated
washing processes and exposure to the
atmosphere.
2. Adsorption of dye:
3. Iodine-Number:
The Iodine number test gives an approximate value
of the fraction of micro-pores present in the bulk
of the activated carbon sample. A greater Iodine
number indicates a larger micro-pore distribution.
After performing the test using Iodine and
standard thiosulphate solutions, the results were
as:
Trial No. Sample Impregnation Ratio C Iodine Number
0 Commercial - 7.8 991
1 Prepared 0.5 5.9 750
2 Prepared 0.25 5.3 673
3 Prepared 1 5.7 724
4 Prepared 1.25 5.6 711
4. Yield:
In general, it was observed that the yield decreased
with an increase in the impregnation ratio. The
exact yield was not accurately determined as part
of the prepared sample was lost during the
processes of washing and filtration, and due to
material handling inaccuracies. The highest yield
was approximately at 20% wherein a final mass of
3.96g was obtained from a 20g precursor.
5. Impurities:
One of the sources of impurities were the ovens
and furnaces used during the heating. As our
samples were not present in isolation during the
heating, dust particles and smaller gaseous
compounds might have creeped in the sample.
Impurities attracted during the manual crushing
cannot be vouched for as well and ash and unburnt
particles formed during the activation also add to
the contaminants list. The major role played by the
impurities was in reducing the adsorption
efficiency of the activated carbon. An added step
of sedimentation was required to purify the
solutions due to these impurities.
Outcomes
The primary objective of this project and lab work was
to prepare activated carbon from a readily available
carbon source such as coconut shells and compare its
characteristics and performance with a commercially
available activated carbon sample.
This was the first step in creating a prototype portable
water filter; testing the practicality of the purification
on a macro and laboratory setup before scaling it down
to fit inside a water bottle.
The chemical activation method was selected to
prepare our sample because the furnace conditions for
steam, or physical activation are quite extreme such as
temperatures above 1000 C and not feasible in our
circumstances. The physical activation method is also
much more time consuming and given the small
amount of sample we were aiming to prepare; it was
not fully practicable. By using the chemical activation
method using Potassium Hydroxide as the activating
agent, we were also able to study the effect of
impregnation ratio on the yield’s characteristics.
The first hurdle faced during the experimentation was
bringing down the precursor size to very fine particles.
To prevent the infringement in the procedure by dust,
debris and other contaminants we physically broke
down the shells into tiny pieces using a hammer.
Ideally, a ball mill or gyratory crusher would have been
used but separating the precursor from the multitude
of impurities gathered inside the crushing equipment
would have been difficult. Furthermore, for effective
mechanical crushing, a very large precursor mass
would have been required. Due to this factor, the
drying and chemical activation stages were possibly not
at full efficiency as the surface area per unit mass of the
precursor was not sufficiently large.
Creeping in of gaseous and micro solid impurities
during the storage, heating or transportation are
another aspect we could not fully vouch for. As it was
difficult to store the samples in air-tight or vacuum
conditions at all times, atmospheric impurities could
have creeped in and compromised the porous
structures of the samples.
In the adsorption test, quantification of the data, and
observing the kinetics of the unit operation were quite
impracticable. The first reason being that during the
adsorption, the samples taken were in solutions not
exceeding 100ml and filtering out a part of this solution
for analysis in the spectrophotometer each time would
increase the instantaneous amount of carbon present
before each analysed sample and this would affect our
results. Also, the mass transfer of the dye molecules
and the pores would not be effective with the reducing
solution amount. For this reason, rather than going for
absolute absorbance tests to determine concentration
using the spectrophotometer, we preferred image
processing using software to find a relative metric to
check and compare the reducing dye concentrations.
A major reason why activated carbon is used in a
variety of filtration applications is for the adsorption of
organic matter. Testing the prepared carbon on its
affinity for organic matter would have given substantial
results about its performance. To measure the total
organic content of the water sample before and after
being treated with the activated carbon, a TOC
analyser would have been used to directly measure the
concentration of dissolved organic matter. However, a
TOC analyser was unavailable during our testing. As an
alternative, a physical method using titration was tried
to determine the total organic content but it was not
successful as the organic content of regular tap water
is very low and such a manual method is not sensitive
to such accuracies.
Summary
 Samples of activated carbon were prepared as
the product from readily available coconut
shells
 The physical characteristics of our prepared
samples were compared with a commercially
available carbon
 The basic parameters for carbon to be activated
were achieved by virtue of its ability to adsorb
dye compounds from colored water solutions
 The fractional micro-pore structure

Another factor that affected this analysis was the

presence of ash and floating impurities that dispersed
themselves in the solution’s bulk during the
adsorption. As the commercially available sample was
mostly free from such contaminants, the decolourizing
of the solution was instantly visible after removing the
flask from the incubator. However, this was not the
case for our prepared carbon. An extended period of
sedimentation was needed for all the impurities to
settle down and make the decolourization visible. An
alternative was filtration but then it would have been
impossible to check the concentration at subsequent
intervals with the carbon being removed.