Abstract

Contents Page
Introduction

Theoretical Background

Experimental Procedure

Results and Analysis

16

Discussion

22

Error Analysis

24

Suggestions for Improvement

25

Experimental Safety Analysis

26

Conclusion

27

References

28

Appendix A Raw Data

29

Introduction
1 page (jia Ming)

2.Theoretical Background
2.1 Packed Bed
The packed bed essentially consists of a vertical cylinder that is packed with packing
material. In most cases, liquids flow downwards from the top of the bed due to gravitational
forces while the vapors/gases travel upwards through contacting with the wetted packing
which is present to increase the surface area for reactions to take place. Optimum recovery
of the solute is achieved when the liquids present are non-volatile and the gases do not
react with the liquids present.
Packed towers are mostly utilized in stripping/ gas-liquid absorption processes as they are
relatively cheaper as compared to other processes such as and because it is very feasible to
change the geometrical parameters of the bed such as the height if the bed, the type of
packing present and such. However, the drawbacks of such processes are that although
efficient stripping occurs at low flow rates, flooding can also occur at higher flow rates and
this may hinder the performance of the bed. In addition, it is relatively difficult to allow
efficient heat exchange with the surroundings; it would not be possible to use this process if
the temperature of either the gas or liquid is too high. The dissolving capacity of the gas in
the liquid also decreases with increasing temperature.
In this particular experiment, the packing used is the Raschig rings that are small cylindrical
structures and hollow. They are inert, affordable and most importantly increase the surface
area for chemical reactions and absorption to take place. The liquid and the gas are
introduced in the counter directions to maintain the concentration gradient between both
streams to increase the driving force of mass transfer.
The stripping process in the packed beds can be improved by allowing a chemical reaction to
occur concurrently to reduce mass transfer resistance and this enhancement of the process
is often referred to as chemisorption.
For instance, in this experiment, the following reaction takes place to improve the stripping
of CO2 gas:
CO2 + 2NaOH

Na2CO3 + H2O

Therefore, there are two processes occurring concurrently. The carbon dioxide from the gas
steam is reacting with sodium hydroxide as well as being absorbed by diffusion into the
liquid stream. The latter process is taken to be instantaneous.
2.2 Different Zones in a packed column
In every packed bed in which counter current absorption is taking place together with a
chemical reaction, three zones of absorption can be identified. They are the surface reaction
zone, the interior reaction zone and the physical absorption zone.

Lin
Absorpti
on Zone

Gout
CAbsorpti
on Zone

XB4

YA4

H3

Surface Reaction Zone

YA3

XB3

H2

Interior Reaction Zone

Physical Absorption Zone

YA2

H1
XB2=0

G, YA1

L, XB1=0

Where
Y: mole ratio of solute in gaseous phase
X: mole fraction of solute in liquid phase
H: height of each zone
A: Carbon Dioxide Gas
B: Sodium Hydroxide
G: Gas phase
L: Liquid phase
2.2.1 Surface Reaction Zone
This zone is present in the uppermost section identified in the column where the
concentration of liquid sodium hydroxide is the highest as compared to the concentration of
carbon dioxide gas that is the lowest. Thus, the reaction takes place at the gas-liquid
interface and as mentioned before, is taken to be instantaneous. An assumption is made
here that sodium hydroxide is non-volatile and that increasing its concentration does not
affect the rate of diffusion significantly. The rate of the reaction is governed by the mass
transfer rate of carbon dioxide from the air because the mass transfer resistance is usually
the highest in any gas phase.

Differing concentrations of
NaOH

At the liquid-gas interfaces: PAi =YAi Pinert =0

Then, using the governing equation for plug flow reactor,

or

And it is known that

So.........

Defining

or
,

Equations for surface reaction zone:

k Y P
1 dN A
rAs
k GA PA GA A T k GA Pinert Y A
S dt
1 YA
And
Y

G A3 dYA
G
h3

a YA 4 rAs k GA aPT

(1 YA )dYA
G Y A3

(YA3 YA4 )
ln
YA
k GA aPT YA4

YA 4
YA 3

An assumption that the solution is dilute is made.

So if YA << 1, pA= PTYA and
h3 =

Y
G
ln A 3
k gA aP
YA 4

Legend:
FA:

molar feed rate of A (mol/s)

6

xA:
Ax:
h3 :
YA :
G:
PA: :
PT:
kGA :
a:

fractional conversion of A
cross sectional area of the reactor (m2)
height of surface reaction zone (m)
mole ratio of reactant A to inert in gas bulk
molar flow rate of inert gas (mol/(m2.s))
partial pressure of gas (N/ m2)
total pressure of gas (N/ m2)
mass
transfer
coefficient
of
A
3
with chemical reaction (mol/m s.Pa)
interfacial area per volume packing (m-1)

in

gas

2.2.2 Interior Reaction Zone

Reaction locus

Gas-Liquid interface

The interior reaction zone can be found in the middle of the packed column. Since the
location of this section is lower than the section observed in the previous part, it can be
observed that the sodium hydroxide concentration decreases while the carbon dioxide
concentration increases. This change in concentrations is the reason as to why the reaction
locus shifts into the liquid film as shown above. The reaction locus will continue to shift
deeper into the liquid film until the concentration of sodium hydroxide reaches zero but will
not move into the liquid bulk. In this section, the mass transfer resistance is governed by
both the liquid and gas film resistances.
Using the Hatta equation, the overall rate equation for this section is,
PA
D C
B B
HA
D Ab
rA
1
1

o
k LA k GA H A
Using the same basis for reaction rate (interfacial mass transfer area, S),

 rAs

1 dN A
S dt

YA
PT
1 YA

DB H A
XB

CT
DA b
1 X B
H
1
oA
k GA k LA

Using material balance over differential area in the interior reaction zone and integrating,
Y

G A 2 dYA
G
h2

a YA3 rAs K GA aPT

YA 2

dYA

Y
G
ln A2

k GA aPT Y A3

DB m
XB
Y A
D Ab

D m
D mG
D mG
1 B
B X Bc B
YA3
Where
and
DA b
DA L
DA L
h2
=
height
of
interior
reaction
zone
[m]
HA
=
Henrys
law
constant*
[N.m/mol]
KGA
=
overall mass transfer coefficient (with chemical reaction)
[mol/m3s.Pa]
D A, D B =
diffusivities
of
A
and
B
respectively
[m2/s]
C, CT =
partial and total molar concentration in the liquid [mol/m3]
b
=
stoichiometric coefficient of NaOH in reaction equation
(*Note that this can only apply if solution is dilute such that Y A << 1; XB << 1, then PA = PTYA
and CB = CTXB)
YA 3

Experimental Procedures
Apparatus
2. 1 X Vertical packed bed column (Internal Diameter (ID): 0.05m, Height (H): 0.490m) along
with the following:
a. Raschig Rings as packing material (ID: 0.006m, Outer Diameter (OD): 0.008m and
Length (L): 0.009m),
b. Various valves, connecting pipes and flow meters,
c. Inlet Distributor,
d. By-passes for extraction of inlet and outlet gas samples,
e. Drainage Facility.
3. CO2 and fresh air supply system:
a. 1 X Compressed CO2 gas tank,
b. 1 X Air supply,
c. 1 X CO2 pump and air pump,
d. 2 X Flow meter with control valve,
e. Connecting pipes.
4. One large reservoir feed tank, greater than 25 L (to store NaOH) along with:
a. 1 X Fluid pump,
b. 1 X Flow meter with control valve,
c. Connecting pipes,
d. 1 X Large stirring stick,
e. 1 X Big funnel.
5. Tap Water supply system:
a. 1 X Water supply,
b. 1 X Flow meter with control valve,
c. Connecting pipes,
d. 1 X Filtration system.
6. Gas Chromatography analyser machine along with:
a. 1 X 1.0 mL Gas Syringe.
7. Acid-base Titration Apparatus:
a. 1 X 50.00 mL burette,
b. 1 X 10 mL,
c. 1 X 20 mL pipette,
d. 2 X Conical Flasks,
e. 1 X Small Funnel,
f. 2 X Beakers,
g. 1 X Retort Stand.

Reagents and Indicators

8. The following reagents and indicators were provided:
a. Deionised water,
b. 0.1084M HCl solution (titrant),
c. 0.1095M NaOH,
d. 2M NaOH solution (to be diluted for feed tank),
e. Methyl Orange indicator,
f. Phenopthalein indicator.
Experimental Set-up
9. Experiment R1 is set up as follows:
Figure 1: Schematic diagram of experimental set up

Experimental Procedure
10. The expertimental procedure can be summarised in Figure XXX.

10

Figure ??? Flow Chart of Experimental Procedure

Dilute and
prepare NaOH
Find concentration of NaOH
through backward titration
Configure setup for Run 1
Start Run 1

Sample and find composition of

inlet and outlet gas

Inconsistent

Consistent
Backward titrate to get
composition of liquid outlet
Consistent
Adjust flow rates to Run 2
values
Completed all
6 Runs

Continue with
next Run

End of experiment

11

Inconsistent

11. Preparation of diluted NaOH feed to approximately 0.2 M:

a. The 2 M NaOH solution was diluted with deionised water in the ratio of 1 L NaOH
to 19 L deionised water to make up approximately 20 L of NaOH feed.
b. Solution was stirred thoroughly with long stirrer to ensure homogeneity.
c. 20 mL of diluted NaOH solution was titrated with 0.1084M HCl solution using
phenolphthalein indicator to determine the exact NaOH concentration. The exact
concentration of NaOH was determined to be 0.180 M.
12. Configuring experimental set-up prior to experimental runs:
a. The large reservoir feed tank was filled up with 20 L of 0.180 M using the big
funnel.
b. Valves were ensured to be in their appropriate positions.
c. Compressed CO2 supply tank valve was adjusted to its open position.
d. Air supply was turned on.
e. Flow meter of CO2 and air was adjusted to attain 0.2 L/min and 1 L/min
respectively.
f. Water supply was turned on.
g. Water flow meter was adjusted to 0.7 L/min.
h. Water level in column was monitored to ensure that liquid fills the bulb at the
bottom of the column but does not overflow into the gas inlet. This was
continuously monitored by adjusted various valves.
i. The set-up was left untouched for 20 minutes to allow steady state to be reached.
j. Inlet gas and outlet gas was sampled using the gas syringe and composition of
inlet and outlet gas was identified using gas chromotography analyser system.
The was done repeatedly.
k. Once consecutive values of inlet and outlet gas mole fraction were consistent
(within 1 %), gas inlet/outlet sampling ceased and the consecutive readings were
recorded.
l. Liquid outlet was sampled by obtaining about 40 mL with a beaker.
m. 10.00 mL of outlet sample was each pipetted into 2 conical flasks.
n. Titration was conducted on both samples. If readings were consistent (within
0.20 mL), tritration readings were recorded. Otherwise, the same process was
repeated.
o. Steps g to n constituted Run 1 of Experiement R1. The steps were repeated in
their entirety for Runs 2 to 6 (except inlet gas concentration was no longer
sampled) by varying NaOH and water flow rates. The pump was switched on to
effect NaOH flow for Runs 2 to 6.
13. Adjust Flow rates:
a. Refer to the table below for the controlled flow rates for each experimental runs.
The first run used pure water and is known as the physical absorption run.
Subsequent runs involving NaOH are termed chemical absorption runs. The flow
rates of the CO2 Air mixture were kept constant and the concentration of NaOH
entering the packed bed varied.

12

Table 3.1: System flow rates for different runs

CO2(g)
Air
Flow Rate (L/min)
Run
1
(Physical
0.20
1.00
Absorption)
Run
2
(Chemical
0.20
1.00
Absorption)
Run
3
(Chemical
0.20
1.00
Absorption)
Run
4
(Chemical
0.20
1.00
Absorption)
Run
5
(Chemical
0.20
1.00
Absorption)
Run
6
(Chemical
0.20
1.00
Absorption)

Water

NaOH(aq)

0.60

0.00

0.55

0.05

0.50

0.10

0.45

0.15

0.40

0.20

0.35

0.25

14. Back titrate liquid outlet sample:

a. 5 mL of NaOH (0.1095M) was pipetted into 2 conical flasks in preparation of
titration.
b. 10 mL of liquid outlet sample was pipetted into the 2 conical flasks.
c. The mixure was swirled to ensure good mixing.
d. The solution mixtures were first titrated against HCl (0.1084M) using
phenolphthalein as the indicator. Two drop os phenolpthalein was added. End
point was reached when the solution colour changes from purple to colourless.
The amount of HCl used was recorded.
e. Next, the resulting solution continued to be titrated against HCl using methyl
orange as the indicator. 2 drops of methyl orange was added. End point was
reached when the solution changes colour from yellow to orange red. The
amount of HCl used was recorded again.
f. The readings from both conical flasks were compared. Consistency was taken to
have been achieved if readings were within 0.2 mL of each other.
g. This constituted the titration readings for Run 1 of experiment R1. The same
steps were repeated for Runs 2 to 6.

13

Results and Analysis

Raw Experimental Data

CO2(g)
Air
Flow Rate (L/min)
Run
1
(Physical
0.20
1.00
Absorption)
Run
2
(Chemical
0.20
1.00
Absorption)
Run
3
(Chemical
0.20
1.00
Absorption)
Run
4
(Chemical
0.20
1.00
Absorption)
Run
5
(Chemical
0.20
1.00
Absorption)
Run
6
(Chemical
0.20
1.00
Absorption)
Table 4.1: Experimental Inlet Flow Rates

Water

NaOH(aq)

0.60

0.00

0.55

0.05

0.50

0.10

0.45

0.15

0.40

0.20

0.35

0.25

Outlet (Vol %)
Run
Sample 1
Sample 2
Average
CO2(g)
Air
CO2(g)
Air
CO2(g)
Air
CO2(g)
1
18.5
81.5
13.7
86.3
14.1
85.9
13.9
2
18.5
81.5
7.07
92.9
6.77
93.2
6.92
3
18.5
81.5
2.40
97.6
2.70
97.3
2.55
4
18.5
81.5
0.783
99.2
0.738
99.3
0.761
5
18.5
81.5
0.254
99.8
0.239
99.8
0.247
6
18.5
81.5
0.118
99.9
0.0953
99.9
0.107
Table 4.2: Composition of CO2(g) and Air measured using Gas Chromatography
Inlet (Vol %)

Run
1
2
3
4
5
6

Volume of HCl(aq) used for titration

with phenolphthalein (mL)
Sample 1
Sample 2
Average
0.00
0.00
0.00
5.10
5.10
5.10
6.00
6.00
6.00
7.00
7.10
7.05
8.60
8.50
8.55
9.60
9.50
9.55
14

Volume of HCl(aq) used

with methyl orange (mL)
Sample 1
Sample 2
0.00
0.00
1.20
1.30
1.30
1.40
1.50
1.40
1.50
1.50
1.80
1.60

Air
86.1
93.1
97.5
99.2
99.8
99.9

for titration
Average
0.00
1.25
1.35
1.45
1.50
1.70

Table 4.3: Volume of HCl(aq) used for Titration with liquid sample drawn from Absorption
Column
Volume of liquid sample taken from absorption column outlet for back-titration = 10mL
Volume of NaOH(aq) added for back-titration = 5mL

Known Physical Properties and Experimental Information

Density of air, air (kg/m3)

Average molecular weight of air, Mair (g/mol)
Density of CO2(g), CO2 (kg/m3)
Molecular weight of CO2(g), MCO2 (g/mol)
Density of water, H2O (kg/m3)
Molecular weight of water, MH2O (g/mol)
Henrys constant, HA (atm.L/mol)
Henrys constant, HA (m3.Pa/mol)
Diffusivity of CO2(g) in water, DA (m2/s)
Diffusivity of NaOH(aq) in water, DB (m2/s)
System temperature, T (K)
System pressure, PT (Pa)
System pressure, PT (atm)
Concentration of de-ionised water, CT (mol/L)
Table 4.4: Physical Properties

1.177
28.85
1.788
44.01
1000
18.02
29.41
2979.97
1.77 x 10-9
2.17 x 10-9
298
101325
1.00
55.56

Height of absorption column, HC (m)

Inner diameter of absorption column, dC (m)
Inner diameter of Raschig Ring, dR (m)
Outer diameter of Raschig Ring, DR (m)
Length of Raschig Ring, LR (m)
Table 4.5: Absorption Column Data

0.49
0.05
0.006
0.008
0.009

[HCl(aq)]titration (mol/L)
[NaOH(aq)]stock (mol/L)
[NaOH(aq)]feed tank (mol/L)
[NaOH(aq)]titration (mol/L)
Table 4.6: Concentration of Reagents

0.1084
2.00
0.180
0.1095

Determining the concentration of NaOH(aq) for the feed tank

Acid-base titration of NaOH(aq) with HCl(aq) in the reaction:

15

Titration: 5mL of NaOH(aq) sample is withdrawn from the feed tank and titrated against
0.1084M of HCl.
Average volume of HCl(aq) used to fully titrate the 5mL NaOH(aq), VHCl = 8.3mL
Since the reaction occurs in a stoichiometric ratio of 1:1,
Concentration of NaOH(aq) in feed tank
=
8.3
x
0.1084
/
5
= 0.18M
Determining the inlet and outlet molar ratios
(i) Molar ratio for inlet CO2(g), YA,in
Since the inlet air remains the same for all the runs, the average inlet gas concentrations will
be used for calculations.
Inlet
molar
ratio
of
CO2(g),
YA,in = (average inlet CO2(g) conc.) / (average inlet air conc.)
=
18.5
/
81.5
= 0.227
(ii) Molar ratio for outlet CO2(g), YA,out
Sample calculation using Run 6:
Outlet
molar
ratio
of
YA,out =
(outlet
CO2
concentration)/(outlet
air
=
0.107
/
= 0.00107
The sample calculations are then repeated for Runs 1 to 5:
Run
Outlet molar ratio of CO2(g), YA,out
1
0.161
2
0.0743
3
0.0262
4
0.00767
5
0.00247
6
0.00107
Table 4.7: Outlet Molar Ratios of CO2(g)

CO2(g),
concentration)
99.9

(iii) Molar ratio for inlet NaOH(aq), XB,in

Sample calculation using Run 6:
Inlet molar flowrate of NaOH(aq)
=
0.25
L/min
x
0.18
mol/L
= 0.045 mol/min
Inlet molar flowrate of water
=
0.35
L/min
x
55.56
mol/L
= 19.45 mol/min
Inlet
molar
ratio
of
NaOH(aq),
XB,in = inlet molar flowrate of NaOH(aq) / inlet molar flowrate of water
=
0.045
/
19.45
= 0.00231
The sample calculations are then repeated for Runs 1 to 5:

16

Run
Inlet molar ratio of NaOH(aq), XB,in
1
0
2
0.000294
3
0.000648
4
0.00108
5
0.00162
6
0.00231
Table 4.8: Inlet Molar Ratios of NaOH(aq)
(iv) Molar ratio for outlet NaOH(aq), XB,out
Volume of outlet solution collected = 10mL
Volume of 0.1095M NaOH(aq) added
=
5mL
no. of moles of NaOH(aq) added
= 0.000548 mol
Sample Calculation using run 6:
No. of mol of unreacted NaOH(aq) =
(9.55

1.70)/1000
x
0.1084
= 0.000851 mol
Concentration of NaOH(aq) in outlet liquid = (0.000851 0.000548) / (20/1000)
= 0.0151 M
Molar flow rate of NaOH(aq) in outlet liquid
=
0.0151
M
x
0.35
L/min
= 0.00530 mol/min
Molar
ratio
of
NaOH(aq)
in
outlet
liquid,
XB,out = molar flowrate of NaOH(aq) / molar flowrate of water
=
0.00530
/
19.45
= 0.000273
Note that Run 1 is conducted without any NaOH(aq) in the inlet for pure physical absorption,
thus there will not be any NaOH(aq) present in the outlet liquid.
The sample calculations are then repeated for Runs 1 to 5:
Run
Outlet molar ratio of NaOH(aq), XB,out
1
-0.000493
2
-0.000118
3
-0.0000395
4
0.0000531
5
0.000195
6
0.000273
Table 4.9: Outlet Molar Ratios of NaOH(aq)
Negative values of XB,out indicate that all the NaOH(aq) have been reacted (amount of
NaOH(aq) left after reaction with dissolved CO2 is less than the amount added in), therefore
the negative values can all be taken to be zero.
Determining the mass transfer coefficients
(i) Overall gas mass transfer coefficient without reaction, KGAoa
To perform this calculation, only data from Run 1 is required (region of physical absorption).

17

Assume ideal gas behaviour for air at room temperature and pressure,

Taking Run 1 to consist only of the physical absorption zone,

(

(ii) Mass transfer coefficient in gas phase, kGAa

As the flow rate of NaOH(aq) used in Run 6 was the highest, it can be assumed that the
whole column was operating under the surface reaction zone.

(iii) Mass transfer coefficient in liquid without reaction, kLAoa

Determining the enhancement factor, E

CT
=
1000
g/kg
x
1000
m3/kg
PT = 1 atm
Sample calculation using run 6:
CB,in =
XB,in
=
0.00231
3
= 128.34 mol/m

18

18g/mol

x
x

55560

mol/m3

CT
55560

CB,out =
=
= 15.17 mol/m3
PA,in =
= 0.227 atm
Enhancement factor,

XB,out
0.000273

CT
55560

PT

YA,in

Calculating E at the top and bottom of the column and taking the average as the overall
enhancement factor:

Eaverage = 0.5 x (11.19 + 2.20) = 6.70

(i) Determining the mass transfer coefficient in liquid phase, k LAa
kLAa =
E
x
=
6.70
x
= 0.0817 s-1
(ii) Determining the overall gas mass transfer coefficient, KGAa

0.0122

The sample calculations are then repeated for Runs 1 to 5:

Run

PA (atm)

CB,in
(mol/m3)

CB,out
(mol/m3)

Etop

Ebottom

Eaverage

0.227

-27.39

1.00

-1.17

-0.085

0.227

16.33

-6.56

2.30

0.479

1.39

0.227

36.00

-2.19

3.86

0.826

2.34

0.227

60.00

2.95

5.76

1.23

3.50

0.227

90.00

10.83

8.15

1.86

5.01

0.227

128.34

15.17

11.19

2.20

6.70

Table 4.10: Calculations for CB,in, CB,out, E

19

Run

KGAa
kGAa
kLAa (1/s)
3
(mol/m .atm.s) (mol/m3.atm.s)

1
2
3
0.375
3.80
0.0122
4
5
6
Table 4.11: Summary of Mass Transfer Coefficients Values

kLAa (1/s)
-0.00104
0.0170
0.0285
0.0427
0.0611
0.0817

KGAa
(mol/m3.atm.s)
-0.0357
0.502
0.772
1.05
1.34
1.61

Determining the critical mole ratio, XBC

XBC is the critical mole ratio where the system is at the end of the surface reaction zone and
at the beginning of the interior reaction zone.

According to Table XXX, the types of reaction zones present are as follows:
Run
XBC
Types of reaction zones present
1
0.000311
Physical Absorption
2
0.000376
Physical Absorption, Interior Reaction
3
0.000562
Physical Absorption, Surface Reaction
4
0.000867
Surface Reaction, Interior Reaction
5
0.00128
Surface Reaction, Interior Reaction
6
0.00182
Surface Reaction, Interior Reaction
Table 4.12: Calculations for XBC and Types of Reaction Zones Present
Heights of various reaction zones

20

Figure 4.1: Visual Illustration of the 3 Absorption Zones

Calculation of YA,2, YA,3, XB,2, XB,3:
(i) Physical absorption zone only (Run 1):
The entire column height is h1 = H = 0.49 m
(ii) Physical absorption and interior reaction zones (Run 2):
Consider control area A, material balance gives:

YA,3 = YA,out = 0.0743

XB,3 = XB,in = 0.000294
XB,out = XB,2 = 0 (physical absorption zone present)

(iii) Surface reaction and physical absorption zones (Run 3):

Consider control area B, material balance gives:

YA,out = 0.0262
XB,in = 0.000648
XB,2 = 0 (physical absorption zone present)

This value of YA,2 is not possible as it has to be lower than YA,in (i.e. 0.227) after physical
absorption has taken place. This anomalous result may have occurred due to errors which

21

would be discussed below in the error analysis section. In the meantime, Run 3 will be
treated as though it does not possess a physical absorption zone in the further calculations.
Consider control area C, material balance gives:

XB,3 = XBC = 0.000562

(iv) Surface reaction and interior reaction zones (Runs 4, 5, 6):

Consider control area B, mass balance gives:

Consider control area C, mass balance gives:

XB,2
YA,2
XB,3 = XBC
Height of physical absorption zone,

=
=

XB,out
YA,in

Height of interior reaction zone,

Height of surface reaction zone,

Run
XBC
XB,in
XB,2
XB,3
XB,out
YA,in
YA,2

1
0.000311
0
0
0.227
-

2
0.000376
0.000294
0
0.000294
0
0.227
0.194

3
0.000562
0.000648
0
0.000562
0
0.227
0.290
22

4
0.000867
0.00108
0.0000531
0.000867
0.0000531
0.227
0.426

5
0.00128
0.00162
0.000195
0.00128
0.000195
0.227
0.583

6
0.00182
0.00231
0.000273
0.00182
0.000273
0.227
0.831

YA,3
YA,out

0.0743
0.0612
0.161
0.0743
0.0262
0.559
0.713
h1
0.49
0.173
h2
0.233
0.236
h3
0.0775
Total
0.49
0.406
0.314
Error (%)
17.1
35.9
Table 4.13: Summary of Final Experimental Values

0.0945
0.00767
1.10
0.158
0.230
0.388
20.8

0.141
0.00247
1.63
0.107
0.370
0.477
2.65

0.201
0.00107
2.32
0.0894
0.479
0.568
-15.9

Run 3 is taken to consist of the surface reaction zone only due to the unfeasible Y A,2
calculated previously above.

23

Discussion
The main aim of this experiment was to study the various reaction zones for a continuous,
counter-current gas-liquid absorption process carried out in a packed bed column. In
addition to that, the heights corresponding to the various reaction zones, as well as the mass
transfer coefficients pertaining to the entire experimental process were determined. In this
section, the assumptions made throughout the course of the experiment will first be stated,
followed by a discussion regarding the results of our experiment and whether they agree
with theoretical principles.
Assumptions
The following assumptions were made for this experiment:
1. The entire experiment was carried out under isothermal, isobaric, and continuous
steady state conditions. 20min-intervals were given after the settings were calibrated
for each run so as to ensure that the conditions were reached before the collection
of any samples.
2. Phase boundary occurs at thermodynamic equilibrium.
3. The solution in the absorption column was dilute enough (<0.05moldm-3) such that
Henrys law is valid and can be applied.
4. Reaction between the CO2(g) and NaOH(aq) was instantaneous and irreversible, such
that both the reactants cannot coexist at any point, and thus the process could be
considered as one that was mass-transfer controlled.
5. NaOH(aq) was non-volatile, no vaporisation of NaOH(aq) into the gaseous film or gas
bulk occurred.
6. The diffusion of CO2(g) from the bulk gas through the gas-liquid interface and into the
film was purely by mass transfer.
7. Run 6 had a sufficiently high NaOH(aq) concentration such that only the surface
reaction zone existed.
8. There was no other mutual exchange of materials between the gas phase and the
liquid phase except for the component (i.e. CO2(g) in this case) to be removed.
Effect of chemical reaction on the rate of absorption

Run

NaOH(aq)
flow rate Eaverage
(L/min)

kLAa (1/s)

0.00

-0.085

-0.00104

0.05

1.39

0.0170

0.10

2.34

0.0285

0.15

3.50

0.0427

0.20

5.01

0.0611

24

0.25

6.70

0.0817

Table 5.1: Values for NaOH(aq) Flow Rates, Eaverage, kLAa

The enhancement factor, E can be used to measure the extent at which absorption rate is
improved by chemical reaction. A large E signifies a higher ratio between the liquid film mass
transfer coefficients of CO2(g) with chemical reaction to that without chemical reaction (i.e.
with a larger E value, there is a greater extent of mass transfer that occurs with a chemical
reaction involved).
As shown from Table 5.1, increase in NaOH(aq) concentration in the liquid inlet stream
corresponds to the increase in enhancement factor, E, which also reflect similar
improvements in absorption rate. The reason for this is because the chemical reaction acts
as the main driving force for CO2(g) absorption, by continuously removing CO2(g) and thus
creates a concentration gradient at the interface. Hence, the efficiency of the absorption
column improves as the concentration of NaOH(aq) in the inlet feed increases.
However, it must be noted that the rate of absorption will not be able increase indefinitely.
When there is an excess amount of NaOH(aq), the liquid film resistance will approach to
zero. The overall resistance will consequently be controlled by the gas film resistance; and
we know that mass transfer of CO2 occurs within the gas film. Since the gas film resistance is
constant, the rate of absorption will correspondingly reach a limit. Further increasing
NaOH(aq) flow rate after that point will not increase the removal of CO 2(g) from the gas
stream as the entire column will be in the surface reaction zone.
Determining the heights of various zones
Run
1
2
3
4
5
6
h1
0.49
0.173
h2
0.233
0.236
0.158
0.107
0.0894
h3
0.0775
0.230
0.370
0.479
Total
0.49
0.406
0.314
0.388
0.477
0.568
Error (%)
17.1
35.9
20.8
2.65
-15.9
Table 5.2: Values for Heights Corresponding to the Various Zones and the % Errors Involved
As shown in Table 5.2, all the derived total heights deviate from the actual absorption
column height of 0.49m. This may be due to a number of reasons and sources of errors
which will be discussed under the error analysis section below.
As we have stated earlier, it is important to note that we have initially assumed Run 6 to
have a sufficiently high NaOH(aq) concentration such that only the surface reaction zone is
present. In view of that, we used the results from Run 6 to determine kGAa, and in turn
derived the other various heights from that.
However, the assumption was clearly just an approximation, because of that we would have
suffered some losses of accuracy in our results. In order to improve on the situation, another
run could be carried out with an even higher NaOH(aq) concentration to further ensure that
indeed only the surface reaction zone is present.

25

Nonetheless, we would still expect the calculated height to be less than the actual height
since the experimental absorption column itself is not 100% efficient. Apart from that, the
complexity of the calculations might also lead to large errors of uncertainty.

26

Error Analysis
Throughout the experiments, several assumptions made coupled with experimental errors
could have lead to the aberrations that are observed in the observed data.
1. The flow rates of some of the variables in the experiment such as air, water and
sodium hydroxide had to be manually controlled by the experimenter. Constant
fluctuations were observed in the flow rates of these variables. Everytime the water
level in the packed bed had to be adjusted, it was observed that the flow rates had to
be re-adjusted to desired values. Thus everytime a manual re-adjustment had to be
made, time may be required to establish a new equilibrium reading and therefore
the concentration of carbon dioxide recorded may not have been that at equilibrium.
2. During many steps of the experiment such as reading off carbon dioxide calculations
and titration results, the steps were repeated a few times to ensure the credibility
and therefore the average values were taken. Any random errors present may be
aggravated due to this averaging and might have led to larger deviations from the
ideal values.
3. The sodium hydroxide solution in the feed tank is assumed to be perfectly mixed.
However, when the experimenter manually diluted the stock solution of sodium
hydroxide, he might not have mixed the resulting solution with the stirrer for an
adequate time period. This would mean that there might be fluctuations in the
concentration of sodium hydroxide entering the packed column at any one time.
4. When taking the sample of carbon dioxide for testing its concentration, the sample
had to be taken from the end of a tube where it is possible for the sample and air to
intermingle. This suggests that although an accurate gas chromatography is utilized
to give us the concentration, the sample itself may be contaminated in the first place.
5. It was accepted that steady state had been attained when the carbon dioxide
concentrations with an interval of 5 minutes had less than a percent difference in
their values. However, this criteria may not be representative of a steady state
having been reached.
6. The reaction between sodium hydroxide and carbon dioxide is assumed to be
instantaneous. However, in reality, this assumption may not hold.
7. The usage of Henrys constants in calculations may cause a problem if the solutions in
question are not dilute enough as Henrys Law is only applicable for dilute solutions.

27

Suggestions for Improvement

1. The following areas of experiment design could be enhanced to increase the accuracy of
experimental results:
a. Usage of water mains (tap) as the source of water supply results in experimental
error. This is because water from water mains tend to have fluctuating flow rates.
Moreover, potable water contained ions that may potentially interfere with
experimental results. Instead, a pump can be used to draw water from another
large water reservoir containing pure deionised water. This essentially replicates
the set-up for the NaOH inlet.
b. The experiment assumes that concentration profile within the liquid and gas film
is a linear one. This assumption is valid if the Raschid rings have high diameter to
length ratio and hence can approximate a flat surface. Experimental accuracy can
be improved if Raschid rings with larger diameter to length ratio were used.
c. As mentioned in the error analysis, manual adjustment of flow meters is required
to maintain the flow rates at their designated values. This process can be
mechanised using process control knowledge to minimise human error such as
time lag before deviation from set points are noticed.
d. The NaOH reservoir can be enhanced to include a stirring device to reduce spatial
heterogeneity in the solution concentration during the experiment.

28

Experimental Safety Analysis

3.5.1 Carbon Dioxide
Handle gas cylinders with utmost care. If in doubt, ask the lab demonstrator. Do not open
the main valves too quickly as it may cause an explosion.
Emergency: If inhaled, conscious persons should be moved to uncontaminated area with
fresh air. Unconscious persons should be moved to uncontaminated area and given
resuscitation or supplemental oxygen.
3.5.2 Sodium hydroxide
Concentrated sodium hydroxide is caustic. Avoid direct contact by wearing gloves and safety
goggles.
Emergency: Upon contact with skin or eyes, wash with copious amount of water.
For disposal, dilute sodium hydroxide are washed down a sink with a large quantity of water.
Larger amounts should be neutralised or diluted before disposal.
3.5.3 General precautions
i. One group member should monitor the flow rates at all times to ensure that the
fluctuations are minimized. If the pump becomes very noisy, switch off the power
and inform the lab demonstrator immediately.
ii. The packed bed flow rate must also be monitored and the outlet flowrate adjusted
accordingly to prevent excessive flooding
iii. If water is spilled around the electrical sockets, inform the lab demonstrator
immediately. Do not attempt to touch the area.
iv. Be properly attired in personal protective equipment (PPE) like lab coat, goggles and
covered shoes during the experiment.
v. Handle glassware with care. In the event of breakage, sweep the broken pieces
immediately and report to lab demonstrator. Do not attempt to touch the broken
pieces with bare hands.

29

Conclusion
1 page Jia Ming

30

References
Wolfgang Bertsch. (2000). Two-dimensional gas chromatography. concepts,
instrumentation, and applications part 2: Comprehensive two-dimensional gas
chromatography. 23(3), 167.
W.E. McCabe, J.C. Smith, and P.Harriott 2001. Unit Operations of Chemical Engineering,
McGraw Hill, New York
th

Perrys Chemical Engineers Handbook, 7 Edition. 1997 (Ed: R.H. Perry, D.W. Green, and J.O.
Maloney), McGraw-Hill, New York.
P.V.Danckwerts. (n.d.). The absorption of gases in liquids. In Retrieved from
http://pac.iupac.org/publications/pac/pdf/1965/pdf/1004x0625.pdf
Hans T. Karlsson. (2010). Absorption with chemical reaction. Unpublished raw data, Energy
and
Environment
KET010,
Retrieved
from
http://www.chemeng.lth.se/ket010/Arkiv/Absorption_Reaction.pdf
M.A. Olutoye and A. Mohammed. (2006). Modelling of a gas-absorption packed column for.
(Master's
thesis)Retrieved
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Annex A Raw Data

31