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.

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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

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Experiment 4: Gas Absorption

association or dissociation then this equation still describes the equilibrium between "x"
in both phases, but only for the 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

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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.

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Experiment 4: Gas Absorption

7. Since we only use the column 1, so the following valves have been adjusted
according to the table below.

COLUMN 1
VALVES
OPEN CLOSED
V1 X
V2 X
V3 X
V4 X
V5 X
V6 X
V7 X
V8 X
V9 X
V10 X
V11 X
V12 X
FCV3 X
FCV4 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

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Experiment 4: Gas Absorption

water flow rate is 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 = 30mL
 VCO2 sample = 10mL

Table 1: Result for titration of HCL.

Air Flow rate, 40 60 80

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Experiment 4: Gas Absorption

L/min
Time/min VHCl, mL VHCl, mL VHCl, ml
10 29.5 28.5 28.5
20 28.6 27.2 27.3
30 28.4 28.5 27.3
40 28.2 28.5 27.3
50 28.2 28.5 -
60 28.2 - -

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

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Experiment 4: Gas Absorption

 Air Flow rate = 40

Table 2: Concentration values of carbon dioxide CO2

Time, min 0 10 20 30 40 50 60
CO2 in inlet 0 0.1100 0.0550 0.0367 0.0275 0.0022 0.0183
gas
CO2 in water 0 0.1053 0.0507 0.0324 0.0234 0.0179 0.0142
CO2 in outlet 0 0.0048 0.0043 0.0042 0.0041 0.0041 0.0041
gas

 Air Flow rate = 60

Table 3: Concentration values of carbon dioxide CO2

Time, min 0 10 20 30 40 50
CO2 in inlet 0 0.0730 0.0370 0.0240 0.0180 0.0150
gas
CO2 in water 0 0.0687 0.0334 0.0197 0.0137 0.0107
CO2 in outlet 0 0.0043 0.0036 0.0043 0.0043 0.0430
gas

 Air Flow rate = 80

Table 4: Concentration values of carbon dioxide CO2

Time, min 0 10 20 30 40
CO2 in inlet gas 0 0.0550 0.02750 0.01830 0.01375
CO2 in water 0 0.05075 0.02385 0.01465 0.01010
CO2 in outlet gas 0 0.00425 0.00365 0.00365 0.00365

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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% 80.1%
40 85.1% 76.1% 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 (CO2) gas from air. The CO2 composition of the inlet gas stream is controlled by
valves for CO2 and air. Flow rates of inlet gas and liquid streams can be measured
using flow indicator.

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Experiment 4: Gas Absorption

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.

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 CO 2 from air in the packed column during the
gas absorption process dissolve in the water.

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Experiment 4: Gas Absorption

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 CO 2 and water. When the
packed column is in wet condition, means the air contain CO 2 has been react and
dissolve with the water.

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 CO2. The gas concentration of CO2 inlet and outlet is not same with the
CO2 is dissolved in water. Time of experiments and flow rate of water have an important
role in order to removed CO2 from the air. The longer time of experiments, the lower
amount of CO2 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 CO 2 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 CO 2. 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 CO 2 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, 5 th 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
g
 0.01  40
mol
g
 0.04
mol

 This is the calculation of 0.01 M HCL

M1 V 1 = M 2 V 2
(0.01)(1000ml )  (1.0) V2

10  1.0 V2

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Experiment 4: Gas Absorption

10
 V2
1.0
V2 = 10 ml

Sample Calculation:
= 0.03 L

Flow rate: 40
x = mole of NaOH added = 0.01V1
NaOH, x = 0.01V1
Time: 10 minutes = 0.01 (0.03L)
= 0.0003L
 Inlet stream
V2 = Volume HCL needed
40 x 10 min = 400L V2 = 20.5 ml x

= 0.0205 L
1 mol CO2 = 44

CO2 inlet = 44 x y = moles of HCL used = 0.01V2

HCL, y = 0.01V2
= 0.01 (0.0205L)
= 0.11 = 0.000205 L

 Outlet stream

V1 = Volume NaOH

V1 = 30 ml x

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Experiment 4: Gas Absorption

CO2 outlet =

= 0.5(0.0003L –
0.000205L)
0.01
Time: 20 minutes
= 0.00475
 Inlet stream

CO2 in water = inlet – outlet 40 x 20 min = 800L

= 0.11 - 0.00475
1 mol CO2 = 44

CO2 inlet = 44 x
= 0.1053
= 0.055

Removal % = 0.0334 g mol/L x 100%

0.0037 g mol/L  Outlet stream
= 95.7%
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 = 21.4 ml x

= 0.0214 L

y = moles of HCL used = 0.01V2

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

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Experiment 4: Gas Absorption

= 0.000214 L

CO2 outlet =

= 0.5(0.0003L –
0.000214L)
0.01

= 0.0043

CO2 in water = inlet – outlet

= 0.055 - 0.0043 Time: 30 minutes

 Inlet stream

40 x 30 min = 1200L
= 0.0507

1 mol CO2 = 44

Removal % = 0.0507 g mol/L x 100%

0.055 g mol/L CO2 inlet = 44 x
= 92.2%
= 0.0367

 Outlet stream

V1 = Volume NaOH

V1 = 30 ml x

= 0.03 L

x = mole of NaOH added = 0.01V1

NaOH, x = 0.01V1

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Experiment 4: Gas Absorption

= 0.01 (0.03L)
= 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 =

= 0.5(0.0003L – 0.000216L)
0.01

= 0.0042

CO2 in water = inlet – outlet

= 0.0367 - 0.0042 Time: 40 minutes

 Inlet stream

= 0.0324 40 x 40 min = 1600L

1 mol CO2 = 44
Removal % = 0.0324 g mol/L x 100%
0.0367 g mol/L CO2 inlet = 44 x
= 88.3%
= 0.0275

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Experiment 4: Gas Absorption

= 0.0275 - 0.0041
 Outlet stream

V1 = Volume NaOH

V1 = 30 ml x = 0.0234
= 0.03 L

Removal % = 0.0234 g mol/L x 100%

x = mole of NaOH added = 0.01V1 0.0275 g mol/L
NaOH, x = 0.01V1 = 85.1%
= 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

= 0.0041

CO2 in water = inlet – outlet

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Experiment 4: Gas Absorption

Time: 50 minutes
CO2 outlet =
 Inlet stream
= 0.5(0.0003L –
0.000218L)
40 x 50 min = 2000L 0.01

= 0.0041
1 mol CO2 = 44

CO2 inlet = 44 x 1 mol

CO2
2000L
CO2 in water = inlet – outlet

= 0.022 = 0.022 - 0.0041

 Outlet stream
= 0.0179
V1 = Volume NaOH

V1 = 30 ml x
Removal % = 0.0179 g mol/L x 100%
= 0.03 L 0.0022 g mol/L
= 81.4%
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

= 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: 60 minutes
CO2 outlet =
 Inlet stream = 0.5(0.0003L –
0.000218L)
40 x 60 min = 2400L 0.01

= 0.0041
1 mol CO2 = 44

CO2 inlet = 44 x 1 mol

CO2 CO2 in water = inlet – outlet

2400L
= 0.0183 - 0.0041
= 0.0183

 Outlet stream
= 0.0142
V1 = Volume NaOH

V1 = 30 ml x
Removal % =0.0142 g mol/L x 100%
= 0.03 L 0.0183 g mol/L
= 77.6%

x = mole of NaOH added = 0.01V1

NaOH, x = 0.01V1
= 0.01 (0.03L)

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Experiment 4: Gas Absorption

CLB 20804 Mass Transfer 1 25