ABSTRACT

The aim of the practical is to determining the rate of absorption and the amount of
absorbed carbon dioxide (CO2) into dilute sodium hydroxide (NaOH) solution. Gas

absorption column and titration techniques were used for the analysis absorbed CO2. The
total concentration of carbonate and the amount of carbon dioxide absorbed was
determined using gravimetric methods (titration). It also explains how flooding velocity
occurs, by using different flow rates as the main objective of the practical.
The main learning objective of this laboratory exercise was to gain the experience in fully
characterizing the behavior of a gas absorption column.

1
INTRODUCTION
Gas absorption column is used for selectively stripping individual gases from a mixture of
gasses by absorption into a separate liquid. Packed towers are used extensively in the
Chemical Industry for Mass Transfer operations , whereby a solute is transferred between a
gas and a liquid phase. The liquid and gas are contacted. Based on the solubility of the gas,
components can be absorbed into the liquid. In order to do this, the two streams can be sent
through several different media. Successful design demands satisfactory performance with
regards to both fluid dynamic and mass transfer considerations
The absorption is a basic operation of the mass transfer consisting in the separation of some
components of a gas mixture by means of contact with an appropriate solvent. The mass transfer
separation operations imply the contact of two or non-miscible phases that shall
sometimes be intermittent, as in the stage columns, and other times it shall be continuous, as in
the packed columns.
The gas absorption column is a unit designed for studying hydrodynamics and absorption
processes in packed columns.

2
NOMENCLATURE

ρ Density of material Kg/m3

V volumetric flow rate m3/s

Qslm flow rate in l/min

U velocity m/s

A Column sectional area m2

Pm Mean pressure K

Tm Mean temperature kPa

T Temperature K

C Concentration mol/dm3

∆P Pressure drop/difference KPa

m Mass flow rate Kg/s

Kog Overall mass transfer coefficient (g-mole/KPa.secm2)

N Absorption rate (g-mole/sec)

R Rotameter reading %

a Packing area per volume m2/m3

H Packing height m

n Number of moles mol

Pi Gas pressure at column inlet kPa

Po Gas pressure at column outlet kPa

3
THEORY

Packed columns are used in chemical industry to absorb a gas from a mixture of gases or strip a
volatile substance from a liquid. Units operation associated with this separation process include;
distillation, gas absorption, adsorption, leaching, liquid-liquid extraction, crystallization, drying,
and dehumidification.

The columns are usually countercurrent gas-liquid contactors in which gas flows upward and
liquid downward. To provide large interfacial area for mass transfer between gas and liquid, the
columns are filled with packing. Design of the column involves estimation of diameter of the
column and height of the packing required for specified separation. The diameter is determined
from flooding characteristics of the column and, the height is found from mass transfer
characteristics of the packing and the gas-liquid system. This is done by using column packing
such as Rashig or Pall rings, Beri or Intalox saddles.

Packed columns are used in chemical industry to absorb a gas from a mixture of gases or strip a
volatile substance from a liquid. Units operation associated with this separation process include;
distillation, gas absorption, adsorption, leaching, liquid-liquid extraction, crystallization, drying,
and dehumidification.

Flooding depends on pressure drop across the column, it being higher at the bottom and lower
at the top to allow the gas to flow upward. The gas flow is usually turbulent and in a dry column,
the pressure drop raises with gas flow, a typical feature of turbulent flow. The pressure drop rises
with an increasing flow of liquid because liquid fills up the column and the space for gas flow is
reduced. Up to the loading point, the pressure drop follows the same relation as in dry run.
Beyond the loading point, the pressure drop rises rapidly with gas flow and the liquid hold up in
the column also rises. Eventually, at the flooding point, the pressure drop rises drastically and
the liquid may splash back from the column. The gas velocity corresponding to the flooding point
is called flooding velocity and the column is operated at some fraction of this velocity, say 60%.

4
Tower height is determined by packing characteristics, namely, interfacial area, and mass transfer
coefficient of the gas-liquid system and extent of separation.

Most reactions utilized in the chemical process industries involve substances, which exist in
different phases. There may be two-phase (binary) and three-phase (tertiary) systems. For all the
differences between them, they have one thing in common. Before a chemical reaction can take
place, the reactants must be transported from the bulk of the stream and carry one phase to the
inter-phase boundary or into bulk of the other phase. Gas liquid absorption is a heterogeneous
process, which involves the transfer of a soluble component of a gas phase into a relatively non-
volatile liquid absorbent. Gas liquid absorption could be employed in purification of waste gases.

Gas absorption is greatly dependent on temperature, since gas solubility as well as chemical
reaction rates are very temperature dependant

Commercial packing is one of the common used types of packing which is available in sizes of
3mm to about 75mm. most of the tower packing are made of materials such as clay, por celain,
metal or plastic. High void spaces of 65-95% are characteristic of good packing. The packing
permit relatively large volumes of liquid to pass through the column counter currently to the gas
flow through the opening with relatively low pressure drops for the gas.

The Fick’s law mentions that the rate of transfer by diffusion is proportional to the concentration
gradient. This law is used when the concentration of the observed component is low, in cases of
high concentration bulk flow takes place and this increases the mass transfer rate by Stefan’s law

𝐶𝑇 𝑑𝐶𝐴
N’A= −𝐷𝑣 ∗ ……………………………………….1
𝐶𝐵 𝑑𝑍

The controlling factor will be the rate of diffusion through two-film where all the resistance is
considered. The change that take place between concentration of a component the through the
gas and liquid

Pa = HCA………………………………………….2

5
Diffusion in the liquid phase

The diffusion rate in liquid is lower than that of gases and it also take longer time for liquid
mixtures to reach its equilibrium, this comes as the result of short distances between molecules
as a result of molecular attraction.

NA=KL(CA1-CA2) …………………………………3

𝐷𝐿
KL= 𝑍𝐿 ……………………………………………..4

Rate of absorption

Where the steady state has been reached, the rate of transfer of material through the gas film
be the same as that of liquid film. The equation of mass transfer of a component

N’A=KL(CA1-CA2)= KG (PAG-PAi)…………………………………………5

The equation of overall mass transfer for the diluted gases is

𝑁 ln( 𝑃𝑖 )
𝑃𝑜
Kog=𝑎𝐴𝐻 ∗ (𝑃𝑖−𝑃𝑜) ………………………………………………………..6

The volume fraction of CO2 in air is obtained using a simple method using the Hempl apparatus.
This apparatus has a gas connected with a liquid reservoir. This can be shown using ideal gas flow

PV = nRT………………….……………………………………………….7

Where the volume of CO2 fraction in the gas sample is equal to the ratio of that sample at the
initial volume (1) to reservoir liquid leg volume (2)

𝑉2 𝑛2 𝑁𝑐𝑜2
= 𝑛1 = (𝑁𝑎𝑖𝑟−𝑁𝑐𝑜2) = %𝐶𝑂2 𝑖𝑛 𝑠𝑎𝑚𝑝𝑙𝑒 ….……….8
𝑉1

Liquid analysis of titration methods the amount of CO2 absorbed in water.

CO2→H2O

Carbon dioxide reacts with water to form carbonic acid

6
CO2+H2O→H2CO3

H2CO3+NaOH→H2O+ NaHCO3

EXPERIMENTAL METHOD

The reservoir was already filled with water. The equipment was switched on. The compressor
was switched on to provide air, valve CV3 adjusted to read 50% and 10 minutes of warm-up
period for air was allowed Pressure was set to 35 kPa using the pressure regulator PR2. With the
pump switched on, water flow rate was adjusted using valve CV1, Flowrates was increased

7
randomly from 20 up to 80 where flooding occurs.
The gas flow rate (manometer- R3) was then increased. by 20% and kept constant, and the same
procedure was followed as mentioned above, until another flooding point was reached

Sodium hydroxide crystals were dissolved in the water reservoir to make a NaOH solution. Valve
CV2 was fully closed and the primary regulator was fully unscrewed. The cylinder valve was
opened and the primary regulator was turned clockwise until the regulator cylinder pressure was
150 kPa. Further adjustment to inlet gas pressure was made with the secondary regulator. CV2
was opened and the rotameter R2 was adjusted to 50% and the secondary pressure regulator to
100kPa, and then CV2 was closed. The air flow rate was adjusted to 50% on the rotameter R3
using valve CV3 while the compressor was on.

The regulator PR2 was used to adjust air pressure to 35KPa followed by switching off the
compressor.
The pump was firstly switched on and the flow rate was adjusted to 50%, this was done by the
return line valve to the reservoir. The CV4 was fully opened; lastly the pump was switched on.
The apparatus was ready for use.

TITRATION PROCEDURE

100 ml of the sample (Caustic soda solution of 0.0277 M) was collected for test at 10
minutes, which was divided in to 50 ml portion of two separated conical flasks.

FLASK 1
Two 50ml portions of the sample were pipetted into separate conical flasks. A drop of
phenolphthalein indicator was added and titrated with standard HCl solution until the
pink color disappeared. A drop of methyl orange indicator was added and further titrated
with standard HCl solution until there was a color change. The neutralized bicarbonate
was indicated by this end point.

8
 FLASK 2

Complete precipitation of all the carbonates was ensured by an excess quantity of 5%

barium chloride solution which was added. 2 drops of phenolphthalein were added and
titrated with a standard solution of HCl until there was a color change.
Another sample was taken after few minutes and the same procedure was followed.

SHUT DOWN PROCEDURE

The tank was emptied using a hose pipe to a drain. The tank was half filled with fresh tap
water and valve CV1 was adjusted by running the pump for 5 minutes to give a full flow.
The pump was switched off and it was again drained, the liquid leg was drained through
the valve S2 while the reagent was flushed with water. The system was switched off. All
equipments used for titration was washed.

RESULTS

TABLE A: EFFECT OF FLOW RATE OF WATER AND AIR ON

PRESSURE DROPS AT 10% AIR FLOW

9
 R3 Air % P5 T6 (OC) R1 H2O % T2 (H2O) OC ∆P(P1-P2) ∆P(P2-P3)
(kPa) kPa kPa
10 14.8 25 10 24.3 0.1 0.1
10 14.8 25.5 20 24.4 0.1 0.1
10 14.7 26 30 24.4 0.1 0.09
10 13 27 40 24.5 0.1 0.12
10 12.5 28 50 24.6 0.1 0.18
10 12 29 60 24.7 0.2 0.3
10 11 29.5 70 24.7 0.3 0.9
TABLE B: EFFECT OF FLOWRATE OF WATER AND AIR ON

PRESSURE DROPS AT 15% AIR FLOW

R3 Air % P5 (kPa) T6 (OC) R1 H2O % T2 (H2O) ∆P(P1-P2) ∆P(P2-P3)

OC kPa kPa
15 6 34.5 10 25.2 0.1 0.1
15 6 37.1 20 25.3 0.1 0.1
15 5 38.5 30 25.4 0.1 0.1
15 4.8 40 40 25.5 0.19 0.15
15 4.8 41 50 25.6 0.2 0.1
15 4.8 42 60 25.7 0.5 0.8
15 4.8 43 70 25.9 0.6 2.7

DISCUSSION

In assessing the result of the experiment, the flooding point was found to be directly related to
the increase in air flow rate; this resulted from the fact that the flooding velocity is directly related
to the liquid flow rate. Flooding depends on pressure drop across the column, it being higher at

10
the bottom and lower at the top to allow the gas to flow upward. The concentration of absorbed
carbon dioxide was found to increase with the increase of time, which deduces that the
absorption rate increases as the time elapsed between the sets of readings gathered.

The overall mass transfer co-efficient differs different sizes, from this it can be deduced that the
overall mass transfer is high when the area occupied by the packing is small and decrease when
the area is increased. Since the overall mass transfer depends on the surface area, it implies that
the lager the surface area the higher the overall mass transfer and the lower the surface area the
lower the overall mass transfers.

CONCLUSION

Operation of the system shows that flooding velocity is directly proportional to the liquid
Flowrates, as the Flowrates increases it where overflowing of water occurs, since the flow rate
of the gas was held constant during the experiment. This was approved by measuring the
11
pressure drop across the absorption column. In the absorption of carbon dioxide using caustic
soda solution, it shows that time taken for the absorption of carbon dioxide affect absorption
rate. The sample of 10 minutes absorbs less concentration than that of 20 minutes. The reaction
between CO2 and caustic soda was proven to enhance the absorption rate, since the titration
results showed different concentrations when was titrated against a predetermined volume and
concentration of hydrochloric acid.

REFERENCES

Transport processes and separation processes principles (4th edition) By Christie John G eankoplis

Coulison and Richardson’s Chemical Engineering Vol 2 (4th edition)

www.edibon.com

12
APPENDIX

DATA

13
 CV3 (R3) CCV1 T1 oC T2 oC T3 oC T4oC Bottom Top
(%) (R1) (%) Pressure Pressure
(KPa) (Kpa)
20 10 27 31.5 27.3 30.1 0.6 0.6
20 20 27.1 31.9 27.6 30.3 0.65 0.65
20 30 27.5 32.4 27.9 30.5 0.65 0.65
20 40 27.8 33.3 28.2 30.8 0.63 0.6
20 50 27.7 33.9 28.4 31 0.61 0.85
20 60 27.9 34.3 28.6 31.1 0.15 0.16

Titration

Volume of acid V1= 41.7mℓ

V2= 35 mℓ

V= (V1+V2)1.2

= (41.7+ 35)1.2

= 92.04 ml

SAMPLE OF CALCULATIONS

A. Flooding velocity

14
R3  10% R1  80%

R3 : 100%  164.9slpm @101.3kPa abs,20 0 C

A  4.185  10 3 m 2

164.9slpm 1m 3 1 min
1. V1  16.7%     4.59  10 4 m 3 / s
100% 1000l 60s

P2  P3  P
P2  P  P3  0.6  101.3  101.9kPa

P1  P2  P
P1  P  P2  0.6  101.9  102.5kPa

P1V1 P2V2

T1 T2
P1V1 T2 102.5  0.000459  273  41.3
V2     0.000477m 3 / s
T1 P2 101.9  273  30.9

V2 0.000459 m
u  3
 0.109
A 4.185  10 s

15
 P1  P2 102.5  101.9
2. Pm    102.2kPa  1.02bar
2 2

t1  t 2 30.9  41.5
tm    36.2 0 C
2 2

Qn .air.equi
Qoperating 
sp.grav.corr. factor   press.corr. factor  temp.corr. factor

sp.grav.corr. factor  sp.grav.


1
1
1 1

 press.corr. factor  1.013


1.013
 0.706
Pm  1.013 1.02  1.013

t m  273 36.2  273

temp.corr. factor    1.03
293 293

0.167  164.9 l 1 min 1m 3 m3

 Qoperating   37.87    0.63  10 3
1  0.706  1.03 min 60s 1000l s
h

Qoperating 0.63  10 3 m
u  3
 0.151
A 4.185  10 s

3. Qslpm
 R3
 

 100   164.9
 
10
100
  164.9   16.07 slpm
101.3  273  T6  101.3  273  37.8
P5  101.3  295 0  101.3  295

16
B. Overall Mass Transfer Coefficient

mol
C HCL  0.01 Vsample  50m


VHCL3 10.8 mol

1.C NaOH  C HCL   0.01   2.16  10 3
Vsample 50 
2. VHCL  4.2m

VHCL2 4.2 mol

C NaHCO3  C HCL   0.01   8.4  10  4
Vsample 50 

VHCL1 2 3   13  4.2  10.8  6.4m

VHCL 1 23 6.4 mol

C NaCO3  C HCL   0.01   1.3  10 3
Vsample 50 

mol
CCO2  C NaCO3  1.3  10 3


C. Rate of absorption

1.3  10 3 mol 0.05 1 min mol

N    1.083  10 7
 10 min 60s s

17
 mol
N ave   1.195  10 3
s

P2  P3  0.25kPa
P2  P3  0.25  101.3  0.25  101..55kPa

P1  P2  0.25kPa
P1  P2  0.25  101.55  0.25  101.8kPa

P2  101.55kPa
P1  101.55  0.3  101.85kPa

101.85  101.8
P1   101.825kPa
2

P   101.825 
n i  7
 n 
N  Po  1.195  10  101.55  mol
K og      8.021  10 10
a. A.H Pi  Po  448.7  4.185  780  10
3 3
101.825  101.55 kPa
sec
m2

C. Concentration of CO2 in the exit stream

2.826 1m 3 1 min m3
VCO2     4.71  10 5
min 1000 60s s

kg g
m  V  1.53  4.71  10 5  7.2063  10 5  7.2063  10  2
s s

m 7.2063  10  2 molCO2
n   1.64  10 3
M 44.01 s

mol
t1  10 min, N  1.083  10 7
s

18
 mol molCO2
nco2 absorbed  1.083  10 7  1.083  10 7
s s

molCO2
nCO2 out   1.64  10 3  1.083  10 7  1.6399  10 3
s

t 2  20 min
nCO2  1.308  10 7  1.308  10 7 molCO2 absorbed

molCO2 Out 
nc 02 out   1.64  10 3  1.308  10 7  1.6399  10 3
s

19
EQUIPMENT

20