EXPERIMENT # 06

OBJECT:
Determination of overall mass transfer co-efficient of 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

CHEMICALS:
1. 0.1 M NaOH Solution
2. Distilled Water
3. Phenolphthalein Indicator Bottle

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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 familiar equation for packed tower absorption is

𝑌𝑜
𝑑[𝐺. 𝑌]
𝐻 = ∫
𝑌𝑖 𝐾𝑂𝐺 . 𝑎𝐴. (𝑌 ∗ − 𝑌)

where Y* is the mole fraction of gas in equilibrium with the liquid at any point in the
tower and where Y is the bulk mole fraction; A is the cross-sectional area of the tower;
H is the packing height and a is the specific area of packing/unit volume of packing.

For dilute gases in an otherwise inert gas stream, the above equation can be simplified: -

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 𝑌𝑜
𝐻. 𝑎𝐴. 𝐾𝑂𝐺 𝑑𝑌
= ∫ ∗
𝐺 𝑌𝑖 (𝑌 − 𝑌)

The right hand side of this equation is difficult to integrate and KOG is more simply (but less
accurately) evaluated from the definition of KOG as:

N =KOG x aAH x log mean

Where, N = rate of absorption (g.moles/second)

aAH = area for mass transfer (m2)
log mean = driving force (pressure in atm)

Therefore:
𝑃
𝑁 ln 𝑃𝑖
𝑜
𝐾𝑂𝐺 = ×
𝑎𝐴𝐻 𝑃𝑖 − 𝑃𝑜

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:
a = Effective interfacial area per unit packed column (cm-1)
A = Cross sectional area of the tower (m2 )
F = Flow (litres/second)
P = Pressure in the column (atm)
Kog = Gas-side mass transfer coefficient (g.moles/second.cm2.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
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)
= 760 mm Hg = 1 atm
Pressure at the column base (by regulating the gas flow from sample Point S3 to manometer)
=_________ mm H2O =_________ atm
Room Temperature = 29oC = 302K
Specific area of packing/unit volume of tower (9 mm Raschig rings), a = 440 m2 / m3
Diameter of Absorption Column = 0.075 m
Height of Absorption Column = 1.4 m
π
Area of Column = 4 ∗ 0.0752 = 4.42 × 10−3 𝑚2

1. 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
V1 V2 V1 V2
(CO2) (air) F2 + F3
ml ml ml Ml
litres/s litres/s litres/s

0.5 0.25 0.75 40 4.1 60 5.1

CALCULATION STEPS:
1. 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:

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 𝑉2
𝑂𝑢𝑡𝑙𝑒𝑡 𝑣𝑜𝑙𝑢𝑚𝑒 𝑓𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑎𝑏𝑠𝑜𝑟𝑏𝑒𝑑 𝐶𝑂2 , 𝑌𝑜 =
𝑉1
𝟓. 𝟏
𝒀𝒐 = = 𝟎. 𝟎𝟖𝟓
𝟔𝟎
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
𝐹3
𝑌𝑖 =
𝐹2 + 𝐹3
𝟎.𝟐𝟓
𝒀𝒊 = = 𝟎. 𝟑𝟑𝟑
𝟎.𝟐𝟓+𝟎.𝟓
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. 𝟑𝟑𝟑 − 𝟎. 𝟎𝟖𝟓)
𝑭𝑨 = × 𝟎. 𝟕𝟓
𝟏 − 𝟎. 𝟎𝟖𝟓
𝑭𝑨 = 𝟎. 𝟐𝟎𝟑𝟑 𝒍/𝒔𝒆𝒄
Litres/second of absorbed CO2 can be converted intto g.moles/second of CO2 absorbed as
follows:-

𝐹𝑎 1 + 𝐶𝑜𝑙𝑢𝑚𝑛 𝑃𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝐷𝑟𝑜𝑝 273

𝑁= × ×
22.42 1 𝑅𝑜𝑜𝑚 𝑇𝑒𝑚𝑝
𝟎. 𝟐𝟎𝟑𝟑 𝟏 + 𝟏 𝟐𝟕𝟑
𝑵= × ×
𝟐𝟐. 𝟒𝟐 𝟏 𝟐𝟗 + 𝟐𝟕𝟑
𝑵 = 𝟎. 𝟎𝟏𝟔𝟒 𝒈𝒎𝒐𝒍/𝒔

2. Volume of Column/Tower, A.H :

𝜋
𝐴. 𝐻 = 4 × 𝐷𝑖𝑎𝑚𝑒𝑡𝑒𝑟 𝑜𝑓 𝐶𝑜𝑙𝑢𝑚𝑛 × 𝐻𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐶𝑜𝑙𝑢𝑚𝑛, m3
𝝅
𝑨. 𝑯 = × 𝟎. 𝟎𝟕𝟓 × 𝟏. 𝟒
𝟒
𝑨. 𝑯 = 𝟎. 𝟎𝟖𝟐𝟓 𝒎𝟑
3. Partial pressures (of CO2):

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Partial pressure = mole fraction x total pressure
Partial pressure = volume fraction x total pressure
:. Inlet, Pi = Yi x PT atm
𝑷𝒊 = 𝟎. 𝟑𝟑𝟑 × 𝟏 = 𝟎. 𝟑𝟑𝟑 𝒂𝒕𝒎
Outlet, Po = Yo x PT atm
𝑷𝒐 = 𝟎. 𝟎𝟖𝟓 × 𝟏 = 𝟎. 𝟎𝟖𝟓 𝒂𝒕𝒎
4. Overall Mass Transfer Coefficient, KOG
𝑃
𝑁 ln 𝑖
𝑃𝑜
𝐾𝑂𝐺 = ×
𝑎𝐴𝐻 𝑃𝑖 − 𝑃𝑜
0.333
0.0164 𝑙𝑛
𝐾𝑂𝐺 = × 0.085
440 × 0.0825 0.333 − 0.085
𝑔𝑚𝑜𝑙
𝐾𝑂𝐺 = 2.463 × 10−3 2
𝑠. 𝑚 . 𝑑𝑟𝑖𝑣𝑖𝑛𝑔 𝑓𝑜𝑟𝑐𝑒

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. Compute the value of rate of absorption across the column. Show detailed
calculations using extra sheet.
INLET
OUTLET ABSORBED CO2 ABSORBED CO2
CONDITIONS
GAS FROM GAS FROM
SAMPLE POINT S3 SAMPLE POINT S1 Fa N
𝑉2 𝑉2 litres/sec g.moles/sec
( ) = 𝑌𝑖 ( ) = 𝑌𝑜
𝑉1 𝑖 𝑉1 𝑜
0.333 0.085 0.2033 0.0164

2. What measures must be taken, if you are asked to conduct scale up studies? Discuss in
detail.

3. Compare the value of mass transfer coefficient with values found in literature. Also
find some suitable correlation that could be used for the determination of mass
transfer coefficient for CO2/Air/Water system and compare with your experimental
value.

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