Gas Absorption

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Experiment 4: Gas Absorption

SUMMARY
Gas absorption is a unit operation in which soluble components of a gas mixture are dissolved in
a liquid. The inverse operation, called stripping or desorption, is employed when it is desired to
transfer volatile components from a liquid mixture into a gas. The term absorption as used in this
experiment refers to the transfer of one of a gas phase to a liquid phase in which it is soluble.
Technically, the liquid used in a gas absorption process is referred to as the absorbent and the
component absorbed is called the absorbate.
In practical usage, the absorbent often is designated as the lean solution or the rich solution
depending on whether it is entering or leaving the absorber Both absorption and stripping, in
common with distillation, make use of special equipment for bringing gas and liquid phases into
intimate contact.
A common apparatus used in gas absorption and certain other operations is the packed tower.
Packed Beds are usually employed in Chemical and Process Industries for Mass Transfer
operations. A gas Stream is usually interacted with a Liquid Stream flowing counter currently in
order to affect the Mass Transfer. Supported mass of inert solid shapes (tower packing) and
packing provides a large area of contact between the liquid and gas and encourages intimate
contact between phases.
At first parameter of air flow rate which is 40L/min, the volumes of HCL required is
28.2mL which constant at minutes 60. At second parameter of air flow rate which is 60mL/min,
the volumes of HCL consumed is 28.5mL which constant at minutes 50. Meanwhile at third
parameter of air flow rate which is 80mL/min, the total volumes of HCL used is 27.3mL which
constant at minutes 40. The increases of flow rate and increases of water absorb for CO 2 in water
is due to the time taken for the process completely.

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

OBJECTIVES

Operate Vapor Liquid Separation Experiment using a Packed Column Gas Absorption
Process Unit.

Analyze the sample using the method of direct Titration in order to determine the amount
of unreacted NaOH in the mixture with the sample.

Determined the condition for loading and flooding in a packed bed.

Determine the function of Packed Column.

Determine the removal percentage of CO2 in the Packed Column.

INTRODUCTION
Absorption, in chemistry, is a physical or chemical phenomenon or a process in which atoms,
molecules, or ions enter some bulk phase - gas, liquid or solid material. This is a different
process from adsorption, since molecules undergoing absorption are taken up by the volume, not
by the surface (as in the case for adsorption). A more general term is sorption which covers
adsorption, absorption, and ion exchange. Absorption is basically where something takes in
another substance.
If absorption is a physical process not accompanied by any other physical or chemical process, it
usually follows the Nernst partition law: "The ratio of concentrations of some solute species in
two bulk phases in contact is constant for a given solute and bulk phases"

The value of constant KN depends on temperature and is called partition coefficient. This
equation is valid if concentrations are not too large and if the species "x" does not change its
form in any of the two phases "1" or "2". If such molecule undergoes association or dissociation
then this equation still describes the equilibrium between "x" in both phases, but only for the

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

same form - concentrations of all remaining forms must be calculated by taking into account all
the other equlilibria.
In the case of gas absorption, one may calculate its concentration by using e.g. the Ideal gas law,
c = p/RT. Alternatively, one may use partial pressures instead of concentrations.
In many technologically important processes, the chemical absorption is used in place of the
physical process, e.g. absorption of carbon dioxide by sodium hydroxide - such processes do not
follow the Nernst partition law.
For some examples of this effect see liquid-liquid extraction, it is possible to extract from one
liquid phase to another a solute without a chemical reaction. Examples of such solutes are noble
gases and osmium tetroxide.
METHODOLOGY

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

Figure 1: Process Flow Diagram of Gas Absorption Process Unit

PROCEDURES
General Start-up
1.

The equipment was inspected visually for any damaged components or glass breakage.

2.

The Cylindrical Re-circulation Vessel was filled with distilled water until the level of
distilled water is satisfactory.

3.

Valves FCV4, V7, V8, V9, V10, V11 were opened and valve V12 is closed.

4.

Valve FCV3 slowly closed so that the Re-circulation vessel is filled until the water
commences to overflow through V11 and valves FCV3 and FCV4 are closed.

5.

The Re-circulation Vessel is never be filled with water to block the air inlet lines to any of
the columns. In such an event, the water needs to be drained out until the gas inlets are
cleared. After that all valves are closed except V11.

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

7.

Since we only use the column 1, so the following valves have been adjusted according to
the table below.
VALVES
V1
V2
V3
V4
V5
V6
V7
V8
V9
V10
V11
V12
FCV3
FCV4

COLUMN 1
OPEN
CLOSED
X
X
X
X
X
X
X
X
X
X
X
X
X
X

Absorption of CO2 into water from Air/CO2 Mixture


1.

The water feed valve was opened gradually until the desired flow rate 1.5 l/min is
achieved as indicated in FI3. The water flow rate also has been ensured to allow stabling
for about 10 minutes after each change until the desired value is reached.

2.

The Compressed Air Valve was opened and the pressure was setting and maintained 1.5
bar gauge.

3.

Valve V3 was opened because the column 3 is only used.

4.

The feed valve FCV1 was gradually opened for Air flow until the desired flow rate about
40 L/min is indicated in the flow meter FI1. Keep on monitoring the Green Oil from the
manometer to ensure that there is no sudden jump of the level. The water flow rate is

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

ensured allowed to stable for about 10 minutes after each change until the desired value is
reached.
5.

Valve FCV2 was gently open after it reached the steady state condition until CO2 rate is
1.5Ll/min is achieved.

6.

Allow further period of 15 minutes for the Absorption process to attain steady state.

7.

10 ml sample was drawed from the outlet valve, V12 for every 15 minutes.

8.

30 ml of prepared 0.01 M NaOH solution was added to the sample. The volume of
NaOH was in excess to ensure that all CO2 has reacted with NaOH in the mixture.

9.

A few drops of an indicator ( Phenolpthalein ) was added to the solution.

10.

Titrate the mixture with already prepared 0.01 M HCl solution. This is meant to
determine the amount of unreacted NaOH with CO2 in the sample mixture.

11.

The measurements is repeated every 15 minutes and carry out the titration with fresh
samples until constant concentration of NaOH has been achieved.

General shut-down procedures


1.

CO2 supply IS closed at valve SG.

2.

The Compressed Air flow closed at CA.

3.

The Circulation Pump stopped and valve V11 was opened.

5.

Fresh Water was allowed to enter the column for a few minutes to drain off the water.

6.

The Fresh Water Flow was closed at FW.

7.

The drain valve V11 was closed when the flow of water has stopped.

RESULT/DATA:

VNaOH

VCO2 sample = 10mL

= 30mL

Table 1: Result for titration of HCL.


Air Flow rate,
L/min
Time/min
10
20
30

CLB 20804 Mass Transfer 1

40

60

80

VHCl, mL
29.5
28.6
28.4

VHCl, mL
28.5
27.2
28.5

VHCl, ml
28.5
27.3
27.3

Experiment 4: Gas Absorption

40
50
60

28.2
28.2
28.2

28.5
28.5
-

27.3
-

Figure 2: HCL (mL) versus Time (min) for 40 L/min

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Experiment 4: Gas Absorption

Figure 3: HCL (mL) versus Time (min) for 60 L/min

Figure 4: HCL (mL) versus Time (min) for 80 L/min

CLB 20804 Mass Transfer 1

Experiment 4: Gas Absorption

Air Flow rate = 40


Table 2: Concentration values of carbon dioxide CO2

Time, min
CO2 in inlet gas
CO2 in water
CO2 in outlet gas

0
0
0
0

10
0.1100
0.1053
0.0048

20
0.0550
0.0507
0.0043

30
0.0367
0.0324
0.0042

40
0.0275
0.0234
0.0041

50
0.0022
0.0179
0.0041

60
0.0183
0.0142
0.0041

Air Flow rate = 60


Table 3: Concentration values of carbon dioxide CO2
Time, min
CO2 in inlet gas
CO2 in water
CO2 in outlet gas

0
0
0
0

10
0.0730
0.0687
0.0043

20
0.0370
0.0334
0.0036

30
0.0240
0.0197
0.0043

40
0.0180
0.0137
0.0043

50
0.0150
0.0107
0.0430

Air Flow rate = 80


Table 4: Concentration values of carbon dioxide CO2
Time, min
CO2 in inlet gas
CO2 in water
CO2 in outlet gas

CLB 20804 Mass Transfer 1

0
0
0
0

10
0.0550
0.05075
0.00425

20
0.02750
0.02385
0.00365

30
0.01830
0.01465
0.00365

40
0.01375
0.01010
0.00365

Experiment 4: Gas Absorption

Percentage removal of CO2 from the column


Table 5: Percentage removal of CO2 from the column
Air flow rate, L/min

40

60

80

Time, min

VHCL, mL

VHCL, mL

VHCL, mL

10

95.7%

94.1%

92.3%

20

92.2%

90.3%

86.7%

30

88.3%

82.1%

40

85.1%

76.1%

80.1%
73.5%

50

81.4%

71.3%

60

77.6%

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Experiment 4: Gas Absorption

ANALYSIS & DISCUSSION:


Absorption is a physical or chemical process in atoms, molecules, or ions that is enter
some bulk phase as gas, liquid or solid material. The process is different from adsorption because
the molecules are not taken up by surface but by the volume. In many important processes
technology, the chemical absorption is used in place of the physical process.
The gas absorption is an operation where a gas mixture is contacted with a liquid for the
purposes of prefers dissolve one or more components of the gas and to provide a solution of
them in the liquid. For this process, gas absorption a soluble component is absorbed by contact
with a liquid phase in which the component is soluble. The system is used for scrubbing gas
streams of carbon dioxide components in this experiment. In this experiment, water is used to
remove CO2 from air.
In gas absorption a soluble component is absorbed by contact with a liquid phase in
which the component is soluble. This system is used for scrubbing gas streams of components
such as sulphur dioxide, carbon dioxide and ammonia. In this experiment, absorber is used to
mix the water and CO2 to become acidic.
The performance of a packed gas-liquid absorption column is evaluated. A water steam
entering the top of the column and exiting the bottom is used to absorb carbon dioxide (CO 2) gas
from air. The CO2 composition of the inlet gas stream is controlled by valves for CO 2 and air.
Flow rates of inlet gas and liquid streams can be measured using flow indicator.
The packing factor is obtained value that depends on the packing size, shape, and
material of construction. Packing is inert material that is used to increase the rate of mass transfer
in the column by increasing the contact surface area between the countercurrent streams. Packing
material found in a wide range of sizes, shapes, and material types where each has a unique
packing factor value.

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Experiment 4: Gas Absorption

Based on the theory, a common instrument used in gas absorption or stripping is a packed
tower. A packed tower consists of the a cylindrical tube with inert packing material; a gas inlet at
the bottom with an exit out the top and a liquid inlet at the top with its exit out the bottom in an
ideal operation the liquid will move down through the packed column and distribute uniformly
over the packing surface in films. The gas will enter the column from below the packed section
and rise upward countercurrent to the liquid flow through the small spaces between the packing
materials. The large amount of close contact between the liquid and gas streams allows for an
efficient transfer of mass.
The gas to be absorbed is carbon dioxide and would be taken from a pressure cylinder
that is standing adjacent to the column. This gas passes through a calibrated variable area flow
meter and is mixed with an air stream also of known flow rate from a rotary compressor
positioned in the framework. The ratio of gas to air in the mixture entering the column is
therefore known and is easily varied. By entering at the base of the column, the gas mixture rises
up through the packed bed and counter-currently contracted with the liquid flowing down the
column.
According to this experiment, the sample is in OH - has been mixed with NaOH solution
to produce the strong bond of OH- before titration. By titrate the HCl that is acid make know
identify how many HCl needs to neutralize the sample that is in base when the changes of
phenolpthalein indicator change from purple to colorless. The purpose of titration process is to
identify how many CO2 from air in the packed column during the gas absorption process
dissolve in the water.
Regarding this experiment, the column 1 which is packed column known as Rasching
Rings has been used in this experiment. This ring type is made from ceramic is small has large
surface area make the contact area in the packed column is large, the wetted area also become
large. So, easy to contact with the CO2 and water. When the packed column is in wet condition,
means the air contain CO2 has been react and dissolve with the water.

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Experiment 4: Gas Absorption

Based on the result obtained, there are three sets reading of HCL recorded for the
different parameters air flow rate by using second packed column (Rasching Rings) as refer as to
Table 1. At first parameter of air flow rate which is 40L/min, the volumes of HCL required is
28.2mL which constant at minutes 60. At second parameter of air flow rate which is 60mL/min,
the volumes of HCL consumed is 28.5mL which constant at minutes 50. Meanwhile at third
parameter of air flow rate which is 80mL/min, the total volumes of HCL used is 27.3mL which
constant at minutes 40.
The increases of flow rate and increases of water absorb for CO 2 in water is due to the
time taken for the process completely. Therefore, the pressure drop is depending with the high of
the packed column. The lower of solubility affect the pressure drop to become increase.
The values of X is NaOH and Y is HCL concentration were calculated in order to
determine the value of CO2 inlet gas and CO2 outlet gas concentration as refer as to the Table 2,
Table 3 and Table 4 with the differences parameters of flow rate. According to the results from
Table 5 shows the removal percentage is known by calculated the inlet and outlet of CO 2. The
gas concentration of CO2 inlet and outlet is not same with the CO 2 is dissolved in water. Time of
experiments and flow rate of water have an important role in order to removed CO 2 from the air.
The longer time of experiments, the lower amount of CO 2 will remove from the air. Therefore,
the optimum flow rate is the best flow rate in order to remove the high amount of CO 2 from air in
the column.

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Experiment 4: Gas Absorption

CONCLUSION & RECOMMENDATION:


As a conclusion, regarding the experiment conducted, a packed column gas absorption
process unit can be operating as a vapor liquid separation experiment. Based on the result
obtained, by done the direct titration using HCL enables to determine the amount of unreacted
NaOH in the mixture of the sample as well as at the same time it able to determine the amount of
CO2 which is dissolved in the water from the absorption process by several calculation. Using
the packed column 1 in the experiment contains Rasching Ring. The surface area of the ring is
large than ring in the other column. So, the ring is absorbing more CO2. Then, large surface area
also makes water flooding in packed column faster and higher than another column.
As a recommendation, this experiment can be done further by try to run for those three
types of packed columns in order to compare the characteristics value percentage of removal
CO2. This is essential because the mass transfer rate is affected by gas flow rate, especially as the
column approaches loading and flooding points.

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Experiment 4: Gas Absorption

TUTORIAL:
1. By making proper mass balance, calculate the percentage removal of CO2 from the column.
*Refer the calculation on the appendix.
2. Do the concert ratio calculation using
The reaction:
2 NaOH + CO2 Na2CO3 = H3
2 moles of NaOH results with 1 mole of CO2
Let x = moles of NaOH added = 0.01V1
y = moles of HCL used = 0.01V2
Then,
g moles of NaOH reacted = (x-y)
g moles of CO2 reacted = 0.5 (x-y)
Hence,
CO2 concentration = 0.5 (x-y) / (VCO2 sample)
= gmol / Liter
* Refer the calculation on the appendix.

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Experiment 4: Gas Absorption

REFERENCES:
1. Manual lab Mass Transfer 1 (CLB 20804), Gas Absorption, 2008
2. Coulson & Richardson, Chemical Engineering, Volume 2 Pergamon Press, Oxford.
3. J F Richardson, J H Harker, J R Backhurst (2002), Chemical Engineering, Fifth Edition,
London: Butterworht Heinemann.
4. Christine John Geankoplis, (2003), Transprot Processes and Separation Process
Principles, Fourth Edition, United States, America: Prentice Hall.
5. Treybal, R.E., Mass Transfer Operations, 3rd ed., Mc-Graw-Hill, 1981
6. McCabe & Smith, Unit Operations of Chemical Engineering, 5th ed., Mc-Graw Hill,
1993.

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Experiment 4: Gas Absorption

APPENDICES:
Calculation the amount use of pure 0.01 M HCL and 0.01 M NaOH that are use in this
experiment;

This is the calculation of 0.01 M NaOH

MV
MW
1000

0.01(1000ml )
g
40
1000
mol

0.01 40
0.04

g
mol

g
mol

This is the calculation of 0.01 M HCL

M1V1 = M2V2
(0.01)(1000ml ) (1.0) V2

10 1.0 V2
10
V2
1.0

V2 = 10 ml

Sample Calculation:
CLB 20804 Mass Transfer 1

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Experiment 4: Gas Absorption

Flow rate: 40
Time: 10 minutes

Inlet stream
CO2 outlet

40

x 10 min = 400L

1 mol CO2

= 0.5(0.0003L 0.000205L)
0.01

= 44

CO2 inlet

= 44

= 0.00475
x

= 0.11

CO2 in water = inlet outlet


= 0.11

- 0.00475

= 0.1053

Outlet stream

V1 = Volume NaOH
V1

= 30 ml x
= 0.03 L

Removal %

= 0.0334 g mol/L x 100%


0.0037 g mol/L
= 95.7%

x = mole of NaOH added = 0.01V1


NaOH, x
= 0.01V1
= 0.01 (0.03L)
= 0.0003L
V2 = Volume HCL needed
V2

= 20.5 ml x
= 0.0205 L

y = moles of HCL used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0205L)
= 0.000205 L

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Experiment 4: Gas Absorption

y = moles of HCL used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0214L)
= 0.000214 L

CO2 outlet

= 0.5(0.0003L 0.000214L)
0.01

Time: 20 minutes

40

Inlet stream

= 0.0043

x 20 min = 800L

1 mol CO2

= 44

CO2 inlet

= 44

CO2 in water = inlet outlet


= 0.055

= 0.055

- 0.0043

= 0.0507

Outlet stream

V1 = Volume NaOH
V1

= 30 ml x

Removal %

= 0.0507 g mol/L x 100%


0.055 g mol/L
= 92.2%

= 0.03 L
x = mole of NaOH added = 0.01V1
NaOH, x
= 0.01V1
= 0.01 (0.03L)
= 0.0003L
V2 = Volume HCL needed
V2

= 21.4 ml x
= 0.0214 L

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Experiment 4: Gas Absorption

= 0.0003L
V2 = Volume HCL needed
V2

= 21.6 ml x
= 0.0216 L

y = moles of HCL used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0216L)
= 0.000216 L

CO2 outlet
Time: 30 minutes

40

= 0.5(0.0003L 0.000216L)
0.01

Inlet stream

= 0.0042

x 30 min = 1200L

1 mol CO2

= 44

CO2 inlet

= 44

CO2 in water = inlet outlet

= 0.0367

= 0.0367

= 30 ml x
= 0.03 L

- 0.0042

= 0.0324

Outlet stream

V1 = Volume NaOH
V1

Removal %

= 0.0324 g mol/L x 100%


0.0367 g mol/L
= 88.3%

x = mole of NaOH added = 0.01V1


NaOH, x
= 0.01V1
= 0.01 (0.03L)
CLB 20804 Mass Transfer 1

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Experiment 4: Gas Absorption

V1 = Volume NaOH
V1

= 30 ml x
= 0.03 L

x = mole of NaOH added = 0.01V1


NaOH, x
= 0.01V1
= 0.01 (0.03L)
= 0.0003L
V2 = Volume HCL needed
V2

= 21.8 ml x
= 0.0218 L

y = moles of HCl used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0218L)
= 0.000218 L

CO2 outlet

= 0.5(0.0003L 0.000218L)
0.01

Time: 40 minutes

40

Inlet stream

= 0.0041

x 40 min = 1600L

1 mol CO2
CO2 inlet

= 44
= 44
= 0.0275

CO2 in water = inlet outlet


= 0.0275

- 0.0041

= 0.0234

Outlet stream

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Experiment 4: Gas Absorption

Removal %

= 0.0234 g mol/L x 100%


0.0275 g mol/L
= 85.1%

1 mol CO2

= 44

CO2 inlet

= 44

x 1 mol CO2
2000L

= 0.022

Outlet stream

V1 = Volume NaOH
V1

= 30 ml x
= 0.03 L

x = mole of NaOH added = 0.01V1


NaOH, x
= 0.01V1
= 0.01 (0.03L)
= 0.0003L
V2 = Volume HCL needed
V2

= 21.8 ml x
= 0.0218 L

y = moles of HCl used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0218L)
= 0.000218 L
Time: 50 minutes

40

Inlet stream
x 50 min = 2000L

CO2 outlet

=
= 0.5(0.0003L 0.000218L)
0.01
= 0.0041

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Experiment 4: Gas Absorption

Time: 60 minutes
CO2 in water = inlet outlet
= 0.022

- 0.0041

= 0.0179

40

Inlet stream
x 60 min = 2400L

1 mol CO2
Removal %

= 0.0179 g mol/L x 100%


0.0022 g mol/L
= 81.4%

= 44

CO2 inlet

= 44

x 1 mol CO2
2400L

= 0.0183

Outlet stream

V1 = Volume NaOH
V1

= 30 ml x
= 0.03 L

x = mole of NaOH added = 0.01V1


NaOH, x
= 0.01V1
= 0.01 (0.03L)
= 0.0003L
V2 = Volume HCL needed
V2

= 21.8 ml x
= 0.0218 L

y = moles of HCL used = 0.01V2


HCL, y
= 0.01V2
= 0.01 (0.0218L)
= 0.000218 L
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Experiment 4: Gas Absorption

CO2 outlet

=
= 0.5(0.0003L 0.000218L)
0.01
= 0.0041

CO2 in water = inlet outlet


= 0.0183

- 0.0041

= 0.0142

Removal %

=0.0142 g mol/L x 100%


0.0183 g mol/L
= 77.6%

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