CHEMICAL ENGINEERING LAB II

(CDB 3052)
EXPERIMENT 2:
ACTIVATED CARBON ADSORPTION ISOTHERM
& KINETICS
GROUP 1 MEMBERS

1) NAZRIL DANIEL BIN ABDULLAH

18996

2) NOOR HAFIZAINIE BINTI MOHD ZOHAN

19323

3) SAIDATUL SYAFIQAH BTE ABDUL RASHID

19417

4) AHMAD FARHAN BIN AHMAD AZHAR

18806

5) KOI ZI KANG

18868

LAB DEMONSTRATOR

: MS. FAEZAH ISA

DATE

: 18th FEBRUARY 201

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INDEX
1. INTRODUCTION

2. RESULT AND ANALYSIS

3. DISCUSSION

14

4. CONCLUSION

17

5. REFERENCES

18

6. APPENDICES

19

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1. INTRODUCTION
Adsorption is a process of removing surface-active material (atom, ions, and molecules) from a
gas/solid by using a porous material as the absorbent. This process creates a film of the
adsorbate on the surface of the adsorbent. Basically, adsorption is a surface-based process
differs from absorption that is volume-based.
The process is widely applied in environmental engineering field and treatment process such as
removal of soluble organics, dyes, pesticides, lignin, etc., from wastewaters. Besides, it is also
widely used in removing colour, taste and odor-producing substances from natural waters that
are to be used as potable water supplies.
The adsorbent used for this experiment is activated carbon. Activated carbon is basically carbon
that has been heated or treated in order to increase its adsorptive power. Charcoal and high
porosity bio-char are usually used to produce activated carbon and that is the reason why it is
usually called as activated coal also. Activated carbon are famous as adsorbent because it has
high porosity and high ratio of surface are to unit weight up to 100 acres per pound, enable it to
have high capacity for adsorption process.
The main objective of this experiment is to archive a 70% removal of methylene blue using
activated carbon. In order to analyze the removal process, three methylene blue solution with
concentration of 50 mg/L , 100 mg/L and 150 mg/ L are prepared. To identify the absorption
capacity of the activated carbon, the amount of activated carbon is fixed to 100 g in each
beaker. The stirrer speed is kept constant for those 3 beakers at 150 rpm.

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The data was analyzed by studying equilibrium isotherms, determine the adsorption kinetics
(Pseudo-first-order or Pseudo-second-order) and its respective kinetic constant(s) and
operational characteristics of a lab-scale packed-bed reactor.

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PROCEDURE
1. Three methylene blue solution are prepared by weighing methylene powder with the
mass of 50mg, 100mg, and 150mg respectively and diluted into three 1L distill water to
obtain 50mg/L, 100mg/L & 150mg/L solution.
2. A sample of the solution are taken from each beaker and put into sampling bottle.
3. The bottle are all put into spectrometer and the initial intensity readings are recorded
before putting it back into the beaker.
4. 100 g of activated carbon are weighted and put into the each and every beaker.
5. The beaker is put under a stirrer with a speed of 150 rpm and the time was recorded.
6. In 5 minutes time interval, the stirrer is stopped and a samples are taken from each
beaker.
7. The reading from the spectrometer are recorded and the solution are put back into the
beaker.
8. The reading are continuously taken with 5 minutes interval until it become constant or
70% removal efficiency are achieved.

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2. RESULT AND ANALYSIS

2.1 Determination of Concentration at Time t

Absorbance of the sample of methylene blue is measured using spectrophotometer every 5
minute until 25 minutes. Concentration of methylene blue is determined by using the linear
equation of calibration curve (assuming the trendline passes through the origin) which is
absorbance vs concentration graph whereby y=0.011x.

Absorbance
Concentration (mg/L)
TIME(min)

50
100
0
0.5450
1.1520
5
0.9000
0.9850
10
1.0810
1.0690
15
1.1740
1.1680
20
1.2280
1.2440
25
1.2560
1.3480
Table 2.1.1: Data of absorbance at time t

150
1.6240
1.0820
0.9740
0.7070
1.0130
1.0200

ABSORBANCE vs CONCENTRATION
1.8
y = 0.011x

1.6

Absorbance

1.4
1.2
1
0.8

0.6

Linear (1)

0.4
0.2
0
0

50

100

150

200

Concentration (mg/L)

Graph 2.1.1: Graph of absorbance vs concentration

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Concentration
of Methylene
Blue (mg/L)

0
5
10
15
20
25

100 mg/L

150 mg/L

Concentration
Concentration
Concentration
Absorbance
(mg/L)
Absorbent
(mg/L)
Absorbent
(mg/L)
0.5450
50.0000
1.1520
100.0000
1.6240
150.0000
0.9000
81.8182
0.9850
89.5455
1.0820
98.3636
1.0810
98.2727
1.0690
97.1819
0.9740
88.5455
1.1740
106.727
1.1680
106.1820
0.7070
64.2727
1.2280
111.636
1.2440
113.0910
1.0130
92.0909
1.2560
114.182
1.3480
122.545
1.0200
92.7273
Table 2.1.2: Table of adsorbance and concentration

Concentration vs Time
160
140

Concentration (mg/L)

TIME

50mg/L

120
100
80

50

60

100

40

150

20
0
0

10

15

20

25

30

Time(min)

Graph 2.1.2: Graph of concentration vs time

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2.2 Removal Efficiency

The removal efficiency in this carbon adsorption experiment indicates how much methylene
blue being adsorbed by granular activated carbon at certain times and the formula is given as
follow:

= ( )

[Eq 2.2]

where
ct = concentration of methylene blue solution at certain times
c0 = concentration of methylene blue solution at initial time

TIME (min)
0
5
10
15
20
25

Mass of solute adsorbed (mg)

C=50mg/L
C=100mg/L C=150mg/L
0.0000
0.0000
0.0000
-31.8181
10.4545
51.6363
-48.2727
2.8181
61.4545
-56.7272
-6.1818
85.7272
-61.6363
-13.0909
57.9090
-64.1818
-22.5455
57.2727

Table 2.2.1: Table of mass of solute adsorbed

Time
(min)
0
5
10
15
20
25

Removal Efficiency(%)
C=100mg/L
C=150mg/L
0.0000
0.0000
10.4545
34.4242
2.8181
40.9696
-6.1818
57.1515
-13.0909
38.6060
-22.5454
38.1818
Table 2.2.2: Table of removal efficiency

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Removal Efficiency vs Time

70

Removal Efficiency (%)

60
50
40
30
20

100

10

150

0
-10 0

10

15

20

25

30

-20
-30

Time(min)

Table 2.2: Graph of removal efficiency

(As removal efficiency of 50mg/L results in negative values thus we eliminate it in the graph)
2.3 Determination of
is equilibrium concentration of adsorbate on adsorbent at time t which can be determined
from the graph of vs t.

Time (min)
0
5
10
15
20
25

C=50mg/L
0.0000
-0.3181
-0.4827
-0.5672
0.6427
-0.6418

C=100mg/L
0.0000
0.1045
0.0281
-0.0618
-0.1309
-0.2254

C=150mg/L
0.0000
0.5163
0.6145
0.8572
0.5790
0.5727

Table 2.3: Table of vs time

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qt vs t
1
0.8

qe=0.62

0.6
0.4

qt

100

0.2

qe=0.15

150

0
-0.2

10

-0.4

15

20

25

30

Time (min)

Graph 2.3: Graph of vs time

2.4 Pseudo-first Order and Pseudo-second Order
In adsorption process, kinetic study is important as it illustrate the uptake rate of adsorbate
and control the residual time for the whole process. Therefore in adsorption kinetic studies,
how fast a chemical reaction occurs and the factors affecting the adsorption reaction rate is
explained. The adsorption kinetics in most cases mostly follows either the pseudo-first
order or pseudo-second order. The linearization of pseudo-first order and pseudo-second
order is given below:

ln(1

) = ln K1 t

+ ( )

[Eq 2.4.1]

[Eq 2.4.2]

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where
K1 = kinetic constant for pseudo-first order (min-1)
K2 = kinetic constant for pseudo-second order (gmg1min1)
qt = concentration of adsorbate on adsorbent at time t
qe = equilibrium concentration of adsorbate on adsorbent at time t
Time(min)
0
5
20
25

ln(1-qt/qe)
0.0000
-1.7888
-2.7183
-2.5737

Table 2.4.1: Table of Pseudo-first- order data

Ln(1-qt/qe) vs t
0
0

10

20

30

Ln(1-qt/qe)

-0.5
-1
-1.5
Ln(1-qt/qe)
-2
-2.5
-3

-3.5

Linear (Ln(1-qt/qe))

y = -0.0921x - 0.619
R = 0.7706
Time (min)

Graph 2.4.1: Graph of Ln(1-qt/qe) vs t

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Time (min)
0
5
10
15
20
25

t/qt
0.0000
9.6830
16.2721
17.4973
34.5368
43.6507

Table 2.4.2: Table of Pseudo-second-order data

t/qt vs t
50
45

y = 1.6802x - 0.7295
R = 0.9524

40

35

t/qt

30
25

t/qt

20

Linear (t/qt)

15
10

5
0
-5 0

10

15

20

25

30

Time (min)

Graph 2.4.2: Graph of t/qt vs t

Pseudo-first-order
Pseudo-second-order

R
0.7706
0.9524

0.5385
0.5952

y-intercept
-0.619
-0.7295

1
0.0921
-

2
-3.8694

Table 2.4.3: Table of values of R, y-intercept, and K for pseudo 1st and pseudo 2nd order

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Errors and Recommendations

After conducting this experiment, we have identified several weaknesses that had affected our
experimental results and therefore, we have listed some improvements to increase the
efficiency of the results. Before starting this experiment of activated carbon adsorption, proper
experimental procedures must be prepared so that the experiment will be carried out
smoothly. As this experiment needs to identify the absorption capacity of the activated carbon,
we need to prepare a fixed amount of activated carbon. However, in order to achieve a better
adsorption of methylene blue by activated carbon, the amount of carbon need to correspond to
the three concentrations of methylene blue solutions. As for our experiment, the amount of
carbon used is not convenient to the concentration of methylene blue solution. The first step to
do is to estimate some amount of carbon to put in the methylene blue solution. If adsorption
goes smoothly at the first trial, then we can proceed with the fixed amount of carbon for all the
three methylene blue solutions and take the reading from spectrophotometer for each interval
of 5 minutes. The spectrophotometer reading might vary due to some factors and thus, we
need to calibrate it to zero reading before using it. The measurement surfaces of
spectrophotometer must be cleaned and when taking the samples of methylene blue solution,
use calibrated pipettes and make sure there is no carbon in the sample so that no error occur
when taking the readings. In our experiment, there is some errors when taking readings from
spectrophotometer so, when stirring the solution of methylene blue with carbon, make sure
that the stirrer speed is not too high so that the carbon will not disintegrate and affect the
solution.

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3. DISCUSSION
For this experiment, we chose Task B and so we have two objectives which are to
achieve a 70% removal efficiency of methylene blue and also to determine the adsorption
kinetics (pseudo-first-order or pseudo-second-order). Activated carbon was used as the
adsorbent and methylene blue which is a dye was used as adsorbate. 50mg, 100mg and 150mg
of methylene blue were added to three 1L beaker of distilled water respectively to obtain 3
different concentration: 50mg/L, 100mg/L and 150mg/L. 100g of activated carbon was added to
each beaker and all beakers were then agitated with mechanical stirrer at the speed of 150rpm.
The absorbance of methylene blue sample of each beaker were measured every 5 minutes for
25 minutes.
The concentration was calculated using the linear equation obtained from the
calibration curve (absorbance vs concentration) whereby y=0.011x. From the concentration
graph, it shows an increasing trend for 50mg/L sample which opposes our goal. For 100mg/L
sample, It decreases and increases which also opposes our goal. One of the reasons for both
increasing trend can be due to the disintegration of the activated carbon which affects the
reading of absorbance using spectrophotometer. Another reason can be that the adsorption
happens in a very short duration and the activated carbon reaches its breakthrough very soon.
For 150mg/L sample, it shows a decrease in its concentration overall.
Therefore, only 100mg/L and 150mg/L sample data are used for calculation of removal
efficiency. Based on the removal efficiency vs time graph, it shows that the 150mg/L sample
managed to achieve an approximately 41% removal efficiency. One of the reasons that it

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cannot reach 70% removal efficiency is because the activated carbon used are not fully
regenerated. Also, it can be due to its early breakthrough point and the disintegration of
activated carbon which causes the reduction of active adsorption sites. From the graph of vs
time, we managed determine the value of which is 0.62 when it is at equilibrium state.

For adsorption kinetics, we only use the data of 150mg/L to plot ln(1 )vs time and

( ) vs time graph. From both the graphs, we can deduce that the adsorption kinetics follows

pseudo-second-order (Ho and McKay model) rate reaction because the ( ) vs time graph

yields a good straight line and has a higher 2 value (0.9524) and a closer value of (0.5952) to

the (0.62) obtained from the graph of vs time as compared to ln(1 ) vs time graph.

This relies on the assumption that chemisorption may be the rate limiting step. In
chemisorption (chemical adsorption), the metal ions stick to the adsorbent surface by forming a
chemical (usually covalent) bond and tend to find sites that maximize their coordination
number with the surface. The kinetic constant for pseudo-first-order graph is 0.0921 while for
pseudo-second-order graph is -3.8694.

Weaknesses & Possible Methods to Improve

After conducting this experiment, we have identified several weaknesses that had affected our
experimental results and therefore, we have listed some improvements to increase the
efficiency of the results. Before starting this experiment of activated carbon adsorption, proper
experimental procedures must be prepared so that the experiment will be carried out
15 | P a g e

smoothly. As this experiment needs to identify the absorption capacity of the activated carbon,
we need to prepare a fixed amount of activated carbon. However, in order to achieve a better
adsorption of methylene blue by activated carbon, the amount of carbon need to correspond to
the three concentrations of methylene blue solutions. As for our experiment, the amount of
carbon used is not convenient to the concentration of methylene blue solution. The first step to
do is to estimate some amount of carbon to put in the methylene blue solution. If adsorption
goes smoothly at the first trial, then we can proceed with the fixed amount of carbon for all the
three methylene blue solutions and take the reading from spectrophotometer for each interval
of 5 minutes. The spectrophotometer reading might vary due to some factors and thus, we
need to calibrate it to zero reading before using it. The measurement surfaces of
spectrophotometer must be cleaned and when taking the samples of methylene blue solution,
use calibrated pipettes and make sure there is no carbon in the sample so that no error occur
when taking the readings. In our experiment, there is some errors when taking readings from
spectrophotometer so, when stirring the solution of methylene blue with carbon, make sure
that the stirrer speed is not too high so that the carbon will not disintegrate and affect the
solution.

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4. CONCLUSION

In this experiment, we were not able to achieve a removal efficiency of 70% due to the
disintegration of activated carbon, usage of not fully regenerated activated carbon and early
breakthrough point of activated carbon. Instead, we only managed to achieve a removal
efficiency of 41%. In terms of adsorption kinetics, we deduce that the adsorption kinetics

follows a pseudo-second-order (Ho and McKay model) rate equation because because the ( )

vs time graph yields a good straight line and has a higher 2 value and a closer value of to the

obtained from the graph of vs time as compared to ln(1 ) vs time graph. Therefore,

the assumption that chemisorption or chemi-adsorption took place in the experiment is valid
and the adsorption kinetics is determined.

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5. REFERENCES
B.H. Hameed, A.T.M. Din & A.L. Ahmad. (2007). Adsorption of methylene blue onto bamboo-based
activated carbon: Kinetics and equilibrium studies. Journal of Hazardous Materials, 141(3), 819825. Retrieved from http://www.sciencedirect.com/science/article/pii/S0304389406008739

Fogler, H.S., Elements of Chemical Reaction Engineering, 3rd Edition, Prentice Hall PTR, 1999.
Norit. (n.d.). CABOT. Retrieved from Norit Activated Carbon: http://www.norit.com/carbonacademy/introduction/

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6. APPENDICES
1. Absorbance vs concentration
From the data obtained from experiment, graph of absorbance vs concentration are
plotted. The relation obtained are as follows:
= 0.011
Where y=absorbance and x= concentration. In order to determine the concentration at
time t, the equation are re-arranged as:

() =

()
0.011

At t=5, concentration methylene blue = 150mg/L:

(5 ) =

(5 )
0.011

(5 ) =

1.082
= 98.3636 /
0.011

At t=10, concentration methylene blue = 150mg/L:

(10 ) =

(10 )
0.011

(10 ) =

0.974
= 88.5454 /
0.011

2. Removal efficiency (%)

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The relation for removal efficiency are given by :

= (1 ) 100
0

At t=5, concentration methylene blue = 150mg/L:

= (1

= (1

=5
0

) 100

98.3636
150

) 100 = 34.42 %

At t=10, concentration methylene blue = 150mg/L:

= (1

= (1

=10
0

) 100

88.5454
150

) 100 = 40.97 %

3. Mass of adsorbate adsorbed (L)

The formula to find mass adsorbate adsorbed is given by:
Mass Adsorbate Adsorbed = (0 ) 1
At t=5, concentration methylene blue = 150mg/L:

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= (0 =5 ) 1
= (150 98.3636) 1 = 51.6364 mg
At t=10, concentration methylene blue = 150mg/L:
= (0 =10 ) 1
= (150 88.5454) 1 = 61.4546 mg

4. Concentration of adsorbate on adsorbent at time t (qt )

At t=5, concentration methylene blue = 150mg/L:

=5 =
=5 =

= 5

51.6364 mg
100

= 0. 516364

At t=10, concentration methylene blue = 150mg/L:

=5 =
=5 =

= 10

61.4546 mg
100

= 0. 614546

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5. Equilibrium concentration of adsorbate on adsorbent at time t (qe)

From the graph of qt vs t, the value of qe is obtained at breakthrough point for

methylene blue concentration = 150mg/L. the theoretical value of qe for this particular
concentration is qe = 0.62.

6. Pseudo First Order

ln( ) = ln K1 t

Mass of activated carbon=150mg

From the graph, y= -0.0921x 0.619
K1 = gradient = 0.0921
ln qe = y-intercept = -0.619, qe = 0.5385
R2 = 0.7706

7. Pseudo Second Order

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+ ( )

Mass of activated carbon=150mg

From the graph, y= 1.6802x 0.7295

= gradient = 1.6802, qe = 0.5952

= y-intercept = -0.7295, K2 = -3.8694

R2 = 0.9524

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