EXPERIMENT # 05

OBJECT:
Calculate the amount of CO2 absorbed in column from analysis of gas samples of inlet and
outlet. (Gas Absorption Column).

APPARATUS:
1. Arm Field, UOP7 (Gas Absorption) Unit.
2. CO2 gas Cylinder
3. Volumetric Flask, 500 ml
4. Conical Flask, 250 ml
5. Burette, 50 ml
6. Measuring Cylinder, 100 ml
7. Hempl Apparatus

CHEMICALS:
1. 1 M NaOH Solution
2. Distilled Water

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EQUIPMENT DESCRIPTION:
The equipment consists of a 75mm diameter column in which there are two lengths of
Raschig ring packing material. Pressure tappings are provided at the base, centre and top of
the column to determine pressure drops across the column. Sampling points are also provided
for the gas at the same three points. The liquid outlet stream and feed solution are also
equipped with sampling points. Suitable manometric measurement is included. Water is taken
from a sump tank, and pumped to the column via a calibrated flowmeter. Gas is taken from a
pressure cylinder (not supplied) through a calibrated flowmeter, and mixed with air supplied
and monitored from a small compressor in a predetermined (but variable) mixed ratio. The
mixture is fed to the base of the tower, in which a liquid seal is provided. The effluent gas
leaves the top of the column and is intended to be exhausted to atmosphere outside the
laboratory building. The apparatus is designed to absorb carbon dioxide/air mixture into an
aqueous solution flowing down the column. Gas analysis apparatus is provided for this
system.

THEORY:
The consideration of gas absorption under unsteady sate regime is quite novel. Most of the
gas absorption systems operate under steady state regime. Such unsteady state processes find
application in a variety of chemical process industries. The absorption of carbon dioxide into
sodium hydroxide is accompanied by chemical reaction to form sodium carbonate as product.
This process is known as chemisorptions. It is used in the extraction of carbon dioxide from
refinery gases and the product is usually not striped since it has some economic value. The
steady state process absorption of the CO2-NaOH system has been studied previously [1]
where the rate of absorption, the rate of transfer of material through the gas film will be the

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same as that through the liquid film, and the generation for mass transfer of a component is
described by equation:
N'A = KG (PAG – PAi) = KL (CAi – CAL)

The removal of one or more selected components from a mixture of gases by absorption into
a suitable liquid is the second major operation of chemical engineering that is based on
interface mass transfer controlled largely by rates of diffusion. Gas absorption is an operation
in which a gas mixture is contacted with a liquid for the purposes of preferentially dissolving
one or more components of the gas and to provide a solution of them in the liquid.
Absorption processes can be divided into two groups, those in which the process is solely
physical and the one accompanied by a chemical reaction. In gas absorption equipment
design, intimate contact of the gas with the liquid is required. When CO2 is absorbed in a
solution of NaOH, a chemical reaction occurs, the nature of which influences the actual rate
of absorption.

PROCEDURE:
1) First fill the two globes of the absorption analysis equipment on the left of the panel with
1.0 Molar caustic soda. Adjust the level in the globes to the '0' mark on the sight tube, using
drain valve C into a flask to do this. (See step A in sketch overleaf).
2) Fill the liquid reservoir tank to three-quarters full with fresh tap water.

3) With gas flow control valves C2 and C3 closed, start the liquid pump and adjust the water
flow through the column to approximately 6 litres/minute on flowmeter Fl by adjusting
control valve C1.

4) Start the compressor and adjust control valve C2 to give an air flow of approximately 30
litres/minute in flowmeter F2.

5) Carefully open the pressure regulating valve on the carbon dioxide cylinder, and adjust
valve C3 to give a value on the flowmeter F3 approximately one half of the air flow F2.
Ensure the liquid seal at the base of the absorption column is maintained by, if necessary,
adjustment
of control valve C4.

6) After 15 minutes or so of steady operation, take samples of gas simultaneously from

sample points S1 and S2. Analyze these consecutively for carbon dioxide content in these gas
samples as shown in the accompanying sketch and following notes.

7) Flush the sample lines by repeated sucking from the line, using the gas piaton and
expelling the contents of the cylinder to atmosphere. Note that the volume of the cylinder is
about 100cc. Estimate the volume of the tube leading to the device. Then decide how many
times you need to suck and expel. (Steps B and C).

8) With the absorption globe, isolated and the vent to atmosphere closed, fill the cylinder
from the selected line by drawing the piston out slowly (Step B). Note volume taken into
cylinder Vl, which should be approximately 20ml for this particular experiment (see

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WARNING note below). Wait at least two minutes to allow the gas to come to the
temperature of the cylinder.

9) Isolate the cylinder from the column and the absorption globe and vent the cylinder to
atmospheric pressure. Close after about 10 seconds (Step D).

10) Connect cylinder to absorption globe. The liquid level should not change. If it does
change, briefly open to atmosphere again.
11) Wait until the level in the indicator tube is on zero showing that the pressure in the
cylinder is atmospheric.

12) Slowly close the piston to empty the cylinder into the absorption globe. Slowly draw the
piston out again (Steps E and F).
Note the level in the indicator tube.

Repeat steps E and F until no significant change in level occurs. Read the indicator tube
marking = V. This represents the volume of the gas sampled.

HEMPLE APPARATUS FOR GAS ANALYSIS

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NOMENCLATURE:
F = Flow (litres/second)
P = Pressure at column top (atm)
V1 = Volume of gas sample taken in Hempl apparatus (ml)
V2 = Corresponds to amount of gas absorbed in Hempl apparatus (ml)
N = Rate of absorption (g.moles/second)

Subscripts
T =Total
i = Inlet conditions to column
o = Outlet conditions to column

OBSERVATIONS:

Pressure at the column Top (by regulating the gas flow from sample Point S1 to manometer)
=_________ mm H2O =_________ atm
Pressure at the column base (by regulating the gas flow from sample Point S3 to manometer)
=_________ mm H2O =_________ atm
Room Temperature = _________ oC = _________ K

1. CO2 content of gas samples:

READINGS AT INLET
F2 F3
V1 V2
(CO2) (air)
ml ml
litres/s litres/s
0.5 0.25 80 5.8
0.5 0.25 60 4.9
0.5 0.25 40 4.1
From flowmeters From Hempl apparatus
with sample drawn
from point S3

2. For calculation of amount of CO2 absorbed in column from analysis of samples at

inlet and outlet.
INLET CONDITIONS OUTLET

GAS FLOWS GAS FROM GAS FROM

litres/second SAMPLE SAMPLE
POINT S3 POINT S1

F2 F3 Total
F2 + F3 V1 V2 V1 V2
(CO2) (air)
ml ml ml ml
litres/s litres/s litres/s

0.5 0.25 0.75 80 5.8 100 8.7

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 0.5 0.25 0.75 60 4.9 80 7.4
0.5 0.25 0.75 40 4.1 60 5.1

CALCULATION STEPS:
1. CO2 content of gas samples:
𝑉2
From use of Hempl apparatus, volume fraction of CO2 =
𝑉1
For ideal gases, volume fraction = mole fraction = Y. Check that the sample taken from
the inlet to the absorption column should give the same value of CO2 fraction as that
indicated by the inlet flowmeters.
𝑉2 𝐹3
= 𝑌𝑖 =
𝑉1 𝐹2 + 𝐹3
𝟓.𝟖
I. 𝒀𝒊 = = 𝟎. 𝟎𝟕𝟐𝟓
𝟖𝟎
𝟒.𝟗
II. 𝒀𝒊 = = 𝟎. 𝟎𝟖𝟐
𝟔𝟎
𝟒.𝟏
III. 𝒀𝒊 = = 𝟎. 𝟏𝟎𝟐𝟓
𝟒𝟎

𝟎. 𝟐𝟓
𝒀𝒊 = = 𝟎. 𝟑𝟑𝟑
𝟎. 𝟕𝟓
READINGS AT INLET CALCULATIONS
F2 F3 𝐹3 𝑉2
V1 V2 ( ) = 𝑌𝑖
(CO2) (air)
ml ml 𝐹2 + 𝐹3 𝑉1 𝑖
litres/s litres/s
0.5 0.25 80 5.8 0.333 0.0725
0.5 0.25 60 4.9 0.333 0.082
0.5 0.25 40 4.1 0.333 0.1025

From flowmeters From Hempl apparatus For comparison of mole

with sample drawn fraction of inlet gas
from point S3

2. Calculation of amount of CO2 absorbed in column from analysis of samples at inlet

and outlet.

From Hempl apparatus, the outlet volume fraction of CO2 can be calculated by the formula:
𝑉2
𝑂𝑢𝑡𝑙𝑒𝑡 𝑣𝑜𝑙𝑢𝑚𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑎𝑏𝑠𝑜𝑟𝑏𝑒𝑑 𝐶𝑂2 , 𝑌𝑜 =
𝑉1
Assuming the mixture of CO2 and Air to be ideal gas, the inlet volume fraction of CO2 can be
calculated by the formula:
Inlet volume fraction = mole fraction = Yi

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 𝐹3
𝑌𝑖 =
𝐹2 + 𝐹3
You can also determine the inlet volume fraction of CO2 using the Hempl apparatus.
Where,
F1= water (lit/sec)
F2= air (lit/sec)
F3= CO2 (lit/sec)
Yi= Volume fraction of CO2 in gas stream at inlet
Yo =Volume fraction of CO2 in gas stream at outlet
If FA is lit/sec of CO2 absorbed between top and bottom, then:

(𝑌𝑖 −𝑌𝑜 )(𝐹2 +𝐹3 ) (𝑌𝑖 −𝑌𝑜 )

Therefore: 𝐹𝐴 = = × 𝑇𝑜𝑡𝑎𝑙 𝑔𝑎𝑠 𝑖𝑛𝑙𝑒𝑡 𝑓𝑙𝑜𝑤
1−𝑌𝑜 1−𝑌𝑜

(𝟎.𝟎𝟕𝟐𝟓−𝟎.𝟎𝟖𝟕)×𝟎.𝟕𝟓
i. 𝑭𝑨 = = −𝟎. 𝟎𝟏𝟐 𝒍𝒊𝒕𝒓𝒆/𝒔𝒆𝒄
𝟏−𝟎.𝟎𝟖𝟕
(𝟎.𝟎𝟖𝟐−𝟎.𝟎𝟗𝟐𝟓)×𝟎.𝟕𝟓
ii. 𝑭𝑨 = = −𝟎. 𝟎𝟎𝟖𝟕 𝒍𝒊𝒕𝒓𝒆/𝒔𝒆𝒄
𝟏−𝟎.𝟎𝟗𝟐𝟓
(𝟎.𝟏𝟎𝟐𝟓−𝟎.𝟎𝟖𝟓)×𝟎.𝟕𝟓
iii. 𝑭𝑨 = = 𝟎. 𝟎𝟏𝟒𝟑𝟒 𝒍𝒊𝒕𝒓𝒆/𝒔𝒆𝒄
𝟏−𝟎.𝟎𝟖𝟓

INLET CONDITIONS ABSORBED

OUTLET
CO2
GAS FLOWS GAS FROM GAS FROM
litres/sec SAMPLE SAMPLE
POINT S3 POINT S1 Fa
F2 F3 Total
𝑉2 𝑉2 litres/sec
(CO2) (air) F2 + F3 ( ) = 𝑌𝑖 ( ) = 𝑌𝑜
litres/s litres/s litres/s 𝑉1 𝑖 𝑉1 𝑜
0.5 0.25 0.75 0.0725 0.087 -0.012
0.5 0.25 0.75 0.082 0.0925 -0.0087
0.5 0.25 0.75 0.1025 0.085 0.01434

RESULT AND DISCUSSION:

Discuss all your results. The questions below only serve as a guideline. Your discussion
should not only be limited to these questions.
1. Compare the results of inlet composition of CO2 gas using both the methods
mentioned in calculation steps.
CALCULATIONS
𝐹3 𝑉2
( ) = 𝑌𝑖
𝐹2 + 𝐹3 𝑉1 𝑖
0.333 0.0725
0.333 0.082
0.333 0.1025

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2. Compute the value of rate of absorption across the column. Show detailed
calculations using extra sheet.
INLET
OUTLET ABSORBED CO2
CONDITIONS
GAS FROM GAS FROM
SAMPLE POINT S3 SAMPLE POINT S1 Fa
𝑉2 𝑉2 litres/sec
( ) = 𝑌𝑖 ( ) = 𝑌𝑜
𝑉1 𝑖 𝑉1 𝑜
0.0725 0.087 -0.012
0.082 0.0925 -0.0087
0.1025 0.085 0.01434

3. Report the amount of CO2 absorbed in g.mole/sec [Hint: Use Ideal Gas Equation and
Standard Conditions]. Also, compare the solubility of CO2 at room temperature with
the amount absorbed in the tower.

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