Mass Transfer I

CLB 20804

Experiment 3
GAS ABSORPTION
1.0

OBJECTIVES

To operate vapor liquid separation process using a Packed Column Gas

Absorption Process Unit.

2.0

To determine percentage removal of carbon dioxide in absorption column.

OVERVIEW

Gas absorption is a widely unit operation in chemical engineering. There are numerous process
applications where particular components need to be selectively removed from a gas stream. The
type of contacting unit for the feed gas and the absorbing liquid can be tailored to the application
along with the choice of the absorbent which will have a high selectivity for the desired
components along with a high capacity for the absorbed components.
The unit consists of three individual packed absorber columns which operate at atmospheric
pressure. Each column has the same overall dimensions but contain a different type of packing.
The columns are arranged so that they can be operated independently and consequently the
performance characteristic of each of the packing can be separately evaluated and directly
compared. Here, a gas stream is usually interacted with a liquid stream flowing counter current in
order to affect the mass transfer. The flow rates of liquid and gas have to be carefully selected in
order to achieve effective mass transfer. This is achieved by recirculating water down the columns
and passing air up through them.

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Figure 1 shows the schematic diagram of the apparatus in this experiment.

Figure 1: Absorption Unit

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3.0

EXPERIMENTAL PROCEDURES

3.1

Chemicals and ancillary equipments required:

PART A: Chemical Preparation

Chemicals Required.

1.0 M HCl.

40 M NaOH.

Ancillary equipments required:

10 ml Pippette.

25 ml and 250 ml Beaker

2 of 1000ml Volumetric Flask

PART A: Chemical Preparation

PART A 1: 0.01M HCL standard solution of 1Litre
1. Pour 10ml of HCL (1.0 M) from the container into 50ml beaker.
2. Pipette 10 ml solution of HCL (1.0 M) into 1000ml volumetric flask.
3. Add dionized water up to marked level at volumetric flask.
4. Shake the solution for a while.
PART A2: 0.01M NaOH standard solution 1Litre
1. Weight 0.4g of 40M NaOH pellets.
2. Pour the 0.4g NaOH pellets into 100ml beaker.
3. Add dionized water into the 100ml beaker.
4. Use magnetic stirrer to dissolve the NaOH pellets into homogeneous solution.
5. Pour the dissolve the NaOH pellets into 1000ml volumetric flask.
6. Add dionized water up to marked level at volumetric flask.
7. Shake the solution for a while.

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PART B: Operate Vapor Liquid Separation Process using a Packed Column Gas
Absorption Process Unit.
PART B: Chemical Preparation
Ancillary equipments required:

3.3

Absorption column

Pails

Jugs (5.0L)

General start-up procedures

1. Ensure all valves are closed.
2. Fill the Cylindrical Re-circulation Vessel is charged with pipe water until liquid level
is satisfactory (Refer to your lecturer or technician).
3. Switch the selector valve SV1 to connect to the column chosen
4. Adjust the valves depending on the column desired to be used by refer Table 1.
Table 1

V1
V2
V3
V4
V5
V6
V7
V8
V9
V10
V11
V12
FCV3
FCV4
SV1

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

COLUMN 2
OPEN
CLOSED
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X

COLUMN 3
OPEN
CLOSED
X
X
X
X
X
X
X
X
X
X
X
X
X
X
X

5. Check valves V11, V12 and FCV3 is closed and open valves V7.

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6. Turn on the power switch of recirculation pump.

7. Slowly open valve FCV4 to give the required flowrate of 0.5 L/min as indicated by
F13.
8. Ensure that the liquid overflow from the unit is connected to a suitable drain.
9. OPEN valve V11 and CLOSE V7.
10. Ensure the liquid inlet valve of the column, i.e. V4, V5 or V6 depending on the
column to be used is OPEN.
PART C: Experiment: Absorption of CO2 into Water from Air / CO2 Mixture.
1. Open the water feed valve gradually until the desired flow rate 1.5 L/min is achieved
as indicated in FI3.
2. Ensure that the water flow rate is allowed to stable for about 10 minutes after each
change until the desired value is reached.
3. Depending on the column to be operated, OPEN the valve V1, V2, or V3.
4. Set air flowrate by gradually OPEN the feed valve FCV1 until the desired flow rate
about 40 L/min is indicated in the flow meter FI1. Ensure that the water flow rate is
allowed to stable for about 10 minutes after each change until the desired value is
reached.
5. After steady state conditions are reached, set CO 2 flowrate by OPEN valve FCV2
GENTLY until CO2 rate is 2 L/min is achieved.
6. Allow further period of 10 minutes for the Absorption process to attain steady state
(Consult your lecturer or technician).
7. Draw 20 ml sample from the outlet valve, V12 for every 5 minutes.
8. Repeat the experiments for 60 L/min air flowrate
PART D: Analyze the Sample using the Method of Direct Titration in order to determine the
amount of unreacted NaOH in the sample.
Chemicals Required.

0.01 M HCl .

0.01 M NaOH.

Phenolpthalein Indicator.

Ancillary equipments required:

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50 ml Burette and Stand.

10 ml Graduated Cylinder.

50 ml Pippette.

10 ml Pippette.

100 ml or 250 ml Conical Flask.

25 ml Beaker

250 ml Beaker

PART D: Analyze the Sample using the Method of Direct Titration in order to determine the
amount of unreacted NaOH in the sample.
1. Fill the 0.01M HCL solution into 50ml Burette.
2. Pipette 10 ml of sample into 250ml conical flask.
3. Pipette 30 ml of solution 0.01M NaOH into 250 ml conical flask that containing 10
ml of sample.
4. Add 1-5 drops of an indicator (Phenolpthalein) to the solution.
5. Titrate the mixture with 0.01 M HCl solution. Stop titration process once first
permanent pale pink appear (Consult your lecturer or technician on how to determine
changes of your color sample). This is meant to determine the amount of unreacted
NaOH with CO2 in the sample mixture.
6. Repeat the measurements every 5 minutes and carry out the titration with FRESH
samples until CONSTANT concentration of NaOH has been achieved.
7. Record your results in the provided table in APPENDIX A.

3.4

General shut down procedures.

1. Close CO2 supply at valve SG.
2. Close the Compressed Air flow at CA.
3. Stop the Circulation Pump.
4. Open Valve V11.
5. Allow Fresh Water to enter the column for a few minutes to drain off the water.
6. Close the Fresh Water Flow at FW.
7. Close the drain valve V11 when the flow of water has stopped.

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4.0

CLB 20804

ANALYSIS AND DISCUSSION

Discuss all your results. The questions below only serve as a guideline. Your discussion
should not only limit to these questions.
1. By making proper mass balance, calculate the percentage removal of CO 2 from the
absorption column.
2. Plot graph percentage removal percentage removal of CO 2 versus air flow rate and
discuss the effect of air flow rate on the percentage removal of CO 2.
3. Discuss any possible errors in the experiment and state any recommendation to
improve the process.

5.0

REFERENCES
1. Treybal, R.E., Mass Transfer Operations, 3rd ed., Mc-Graw-Hill, 1981
2. McCabe & Smith, Unit Operations of Chemical Engineering, 5th ed, Mc-Graw-Hill,
1993
3. Geankoplis,C. J. Z., Mass Transport Phenomena, 4th Ed., Rine Hart Winston, New
York.
4. Coulson & Richardson, Chemical Engineering. Vol. 2 Pergamon Press, Oxford

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APPENDIX A
Tables of Results
Volume of NaOH

= _______________ mL

Volume of CO2 in sample

= _______________ mL

Table 1

Air Flowrate

Time, t (min)

Volume of HCl, mL

0
5
10
15
40 L/min

20
25
30
35
40
5
10
15

60 L/min

20
25
30
35

Air flow rate

Concentration of

Concentration of

Concentration of

Percentage

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CO2 at inlet

CO2 in water

CO2 at outlet

Removal of CO2

40 L/min
80 L/min

Table 2

STEP BY STEP CALCULATION GUIDE

To determine Concentration of CO2 at outlet

Water Inlet

H2O + CO2

Conc. (CO2 +air) outlet

Conc. (CO2 +air) inlet

Based on below reaction:

2 NaOH + CO2 Na2CO3 + H2O

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Na2CO3 + HCL CO2 + H2O+ NaCl

2 moles of NaOH results with 1 mole of CO2
Let x = moles of NaOH added = 0.01V1
V1= volume of NaOH,

V2 = volume of HCL

y = moles of HCl used = 0.01V2

Then,
moles of NaOH reacted = (x-y)
moles of CO2 reacted = 0.5 (x-y)
Hence,
concentration CO2 outlet = 0.5 (x-y)/ (VCO2 sample)
= mol/Liter

Concentration of CO2 at inlet

CO2 Inlet stream:
2.0

L
x5 min 10 L =0.01m3
min

Density of CO2=1.98

kg
m3

mass
volume

Mass of CO2 = 1.98

kg
x 0.01m 3 0.0198kg
m3

Mol of CO2 =mass CO2 / molar mass CO2

n=

19.8 g

mole
0.45mole
44 g

10

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conc, c

CLB 20804

n 0.45mol

0.045 mol
L
v
10 L

CO2 inlet = 0.045 mol L

CO2 in water
CO2 in water = conc. CO2 inlet conc. CO2 outlet
Percentage removal of CO2 from the column.

% removal of CO2

Conc.outlet
x100%
conc.inlet

11

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