1

INDEX
SR NO SUBJECT PAGE NO
1. INTRODUCTION 2–4
2. DESCRIPTION OF INSTRUMENT 5
3. SAFETY 6
4. EXPERIMENTAL MANUAL 7–9
5. PRECAUTIONS 10
6. LINE DIAGRAM 11

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INTRODUCTION:
The chemical industry affords numerous examples of processes in which a gas
is dissolved by a liquid and then undergoes a chemical reaction in the liquid phase.
For example, in the contact process for the manufacture of sulfuric acid the sulfur
trioxide formed by the catalytic oxidation of sulfur dioxide is absorbed in a mixture of
sulfuric acid and water with which it reacts chemically to produce more sulfuric acid.
Similarly, the nitrogen oxides formed by the catalytic oxidation of carbon dioxide are
absorbed in water and react to from nitric acid. In some cases, an unwanted impurity
in a gas is removed by scrubbing with a liquid capable of reacting with it, as in the
removal of sulfur dioxide from flue gas by absorption in an alkaline solution or a
suspension of slaked lime. The separation and recovery of one constituent of a gas
mixture may be affected by absorption in liquor with which it undergoes a reversible
chemical reaction. For example, carbon dioxide is removed from gases by absorption
in mono-or diethanolamine, with which it reacts to form carbonates, and
subsequently recovered by heating the solution. The regenerated amine is then
returned to the absorption plant. In this case the advantage over a process involving
physical solution, e.g. in water, is the much higher solubility of carbon dioxide in the
amine and the consequent reduction in the rate of circulation of liquid through the
absorber and regenerator.

The effect of a chemical reaction in the liquid phase is to increase the

solubility of the absorbed component and reduce its equilibrium partial pressure. If
the chemical reaction is irreversible, the equilibrium partial pressure is zero as long
as any free reactant remains in the liquid phase. Since the molecules of absorbed
component must diffuse into the liquid phase until they meet the reactant, and after
the reaction, the product must diffuse into the bulk of the liquid, the rate of
absorption must depend on the concentration and diffusivities of the reactant and
products, on the rate of chemical reaction and on the depth of the liquid film in

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which the reaction occurs. The sequence of events for a fast-irreversible reaction is
illustrated by Figure 1.

Component A diffuses from the gas to the liquid surface (X), where its partial
pressure is pi and the equilibrium concentration in the liquid is ci. It then diffuses in
the liquid to a plane Y, where it meets reactant B which is diffusing in the opposite
direction from the bulk of the liquid, Z. Owing to the instantaneous reaction the
concentrations of A and B fall to zero, and the product AB is formed. This diffuses
back to the plane Z, representing the bulk of the liquid.

AB
B
A ci
pi

A B

X Y Z

Fig. 1 Concentration gradients in a liquid film when a component A dissolves at the

surface XX and reacts with component B in solution

The distance XY traversed by A is only a fraction of the total film thickness XZ

and the concentration gradient is greater than would be the case in physical
absorption. In consequence the mass transfer coefficient for absorption in the liquid
film is enhanced considerably when a rapid chemical reaction occurs. For example,
the absorption of sulfur dioxide by water is controlled by both the gas and liquid
films, but when it is absorbed by a dilute solution of caustic soda the liquid film
coefficient is increased to such an extent that the rate of absorption is controlled
almost entirely by the gas film.

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INDUSTRIAL PROCESSES INVOLVING ABSORPTION WITH CHEMICAL REACTION:

The principal industrial processes involving absorption with chemical reaction

may be grouped under the following headings.
1. Absorption of carbon dioxide by caustic soda or potash solutions. Owing to
the expensive nature of the absorbent this is mainly used for removing the
last traces of carbon dioxide from a gas.
2. Absorption of carbon dioxide by sodium or potassium carbonate solutions.
The solution may be regenerated by heating to decompose the bicarbonate.
3. Absorption of carbon dioxide by mono-or diethanolamine solutions, followed
by desorption and regeneration at a higher temperature.
4. Absorption of carbon dioxide by carbon dioxide Cal solutions to produce
ammonium carbonate. This reaction is used in the Solvay process for
manufacture of sodium carbonate.
5. Absorption of hydrogen sulfide by sodium hydroxide or carbonate solutions.
6. Absorption of hydrogen sulfide by ethanolamine solutions, followed by
desorption and regeneration.
7. Absorption of sulfur dioxide by water and alkaline solutions.
8. Absorption of sulfur trioxide by sulfuric acid.
9. Absorption of chlorine.
10. Absorption of nitrogen oxides and manufacture of nitric acid.
11. Absorption of hydrogen fluoride.

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DESCRIPTION OF EQUIPMENT
The equipment consists of approx. 55 mm inner diameter & 750 mm long
borosilicate glass column filled with Rasching ring (12 mm). Pressure tapings are
provided at the base and top of the column to determine pressure drop across the
column with Mercury manometer. The liquid outlet streams and feed solution are
also equipped with sampling points. Water/ Aq. NaOH soln./ Dil. KOH soln. is taken
from a Closed Air Operated Feed tank and feed enters the column via a calibrated
flow meter.

CO2 Gas is taken from a pressure cylinder through a calibrated flow meter, and
mixed with air supply and monitored from an air compressor in a predetermined (but
variable) mixture ratio. A suitable mixing length and mixer are included to mix Air
and CO2 thoroughly. The mixture is fed to the base of the tower. The exhaust gas
leaves at the top of the tower and is intended to be exhausted to atmosphere
outside the laboratory building.

• 55 mm dia. 750 mm long borosilicate column with bed of Rasching ring (12
mm)
• Air compressor (1.0 HP) and Rotameter.
• CO2 cylinder (6.8 kg) with pressure regulator and Rotameter
• Water/ dilute NaOH Solvent circulation system with Feed tank (20 Liters
approx. SS 304) and Rotameter.
• Liquid and Air Distributor.
• Suitable manometric measurement arrangement with pressure taps at the
bottom and top.

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SAFETY
• Carbon Dioxide is both toxic and combustible. If a major carbon dioxide leak

develops, evacuate the laboratory immediately, without attempting to shut

off the cylinder valve. Open the main cylinder valve only about one-half turn,
to prevent discharge at high rates.
• Wear safety glasses at all times. Be sure the lab ventilation system is operating
before using carbon dioxide. Be sure the carbon dioxide cylinder valve is
closed before ending the experiment. Know the safety shower and eye wash
station locations.
• Wear jeans or slacks, a long-sleeved shirt, and sturdy shoes that give good
traction on possibly wet floors.
• Guard against electrical hazards by making sure that all equipment is well
grounded using three-wire plugs and other means.
• Handle with great care any solvents or other potentially volatile, flammable,
toxic, or otherwise dangerous chemicals. In this experiment air, water, carbon
dioxide, and a solution of Potassium/ Sodium chloride are used. Potassium/
Sodium chloride is toxic if ingested in large amounts. Carbon dioxide is toxic in
higher concentrations.
• Guard against falls, burns, cuts, and other physical hazards. Use heavy gloves
to open or close hot steam or condensate valves.
• THINK FIRST OF SAFETY IN ANY ACTION YOU TAKE. If not certain, ask the TA or
a faculty member before you act.

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GAS ABSORPTION STUDY APPARATUS EXPERIMENTAL MANUAL

AIM:
➢ To study the flooding conditions and the absorption of CO2 from Air using a
NaOH/ water solution in a packed column.
➢ To gain experience with the packed bed gas absorption column and its
analysis system.

PREPARATION OF SOLUTIONS:
FEED SOLUTION
Prepare the dilute NaOH solution in the tank. Add 60 gm of NaOH pellets in to
15 liters water to make 0.1 N solution of the NaOH. Stir the solution well to dissolve.
Do not let the pellets clump in the bottom.

PROCEDURE:

• Feed the supply tank with the prepared 0.1 N NaOH/ Water solution about 15
liters.
• Check the concentration of the feed solution by titration against 0.1 N HCl.
• Connect the Air Compressor to the single-phase power supply.
• Initially start the air compressor and collect sufficient air in the pressure tank
so as the pressure is about 3-4 kg/ cm2.
• Open the valve of the pressure tank and allow the air to pass through the
column.
• Set the air flow at the desired value and then open the valve of the CO2
cylinder and adjust the flow rate to predetermined value. The inlet
concentration of CO2 in Air should not be more than 10%. (For example, if rate
of Air is 30 LPH insert CO2 at 3 LPH.

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• Now start the feed (NaOH soln.) by allowing air in to feed tank and using
rotameter set the desired value of flow rate.
• After sometime take the sample at various points and analyze them.
• Initially start the liquid flow at sufficiently high rate (VL = 0.03 m/s) to ensure
that all the packing is wetted.
• The flow rates of gas and liquid are adjusted at predetermined values with the
help of rotameters.
• The CO2 flow rate should be such that the %CO2 in the mixed gas is about 8-
10%. The gas velocity has no effect on the interfacial area in a packed column.
Hence a value of VG between 0.1 - 0.2 m/s may be chosen for all the
experiments and keeping it constant.
• The linear superficial liquid velocity V is the most important variable. The
range for V should be fixed between 0.001 - 0.007 m/s.
• The system is allowed to reach steady state after fixing the liquid level in the
bottom section at a marked height.
• Inlet and outlet liquid samples are withdrawn for analysis.

COLLECTING THE SAMPLE:

• Collect the Samples by means of opening the sample tap.
• Note the temperature at the time of collection.

OBSERVATIONS:

System : (CO2 + Air) - Aq. NaOH Solution

Packing Used : Rasching ring of size 12 mm
Column Dia. : 55 mm (ID)
Pressure : 101.325 k N/m2
Packed Height : 600 mm
VG : m / sec

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TITRATION:
• Pour 50 ml of 0.1 N HCL solution in burette.
• Take 10 ml sample of NaOH in to flask.
• Add 3 drops of Phenolphthalein in to flask.
• Stir flask firmly and start to pour 0.1 N HCl solution from the burette.
• Stop when pink color indicates in to flask.
• Note down the burette reading.
FEED ANALYSIS
Burette = 0.1 N HCL solution (N2)
Pipette = 10 ml feed solution (V1)
Indicator – Phenolphthalein
OBSERVATION TABLE:
NORMALITY OF NAOH BURETTE NORMALITY OF
BURETTE READING
SR. NO. (BEFORE EXPERIMENT) READING OF NAOH (AFTER
OF HCL (ML) (V2)
(N1) HCL (ML) (V2) EXPERIMENT) (N1)
1.
2.
3.

CALCULATIONS:

1. Normality of NaOH Before Experiment

N1V1 = N2*V2
= N2*V2 / V1
N1 = _____ N

2. Normality of NaOH After Experiment

N1V1 = N2*V2
= N2*V2 / V1
N1 = _____ N

RESULT:

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PRECAUTIONS:

• CO2 IS HAZARDOUS GAS SO, HANDLE WITH CARE EVERYTIME.

• Sufficient Ventilation system is required to perform this experiment.
• Wear Mask, Goggles, Gloves etc. during experiment.
• Every time open CO2 cylinder slightly to avoid any accident.
• Maintain CO2 flow very slow (About 8-10 % in CO2+Air Mixer) with the
help of rotameter.
• Every time store sufficient air in to Air Compressor prior to experiment.
• Every time after experiment close CO2 cylinder tightly by spanner
provided.
• Drain out any remaining feed after completion of experiment by opening
drain valve provided below the feed Tank.
• Pour clean water in to feed tank twice or thrice to remove any traces of
NaOH present in the feed tank.
• Then fill clean water in to feed tank and run clean water into system
after completion of experiment to remove any traces of NaOH.

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GAS ABSORPTION STUDY APPARATUS EXPERIMENTAL MANUAL