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EXPERIMENT: GAS
ABSORPTION AMENDMENT
DATE:
FACULTY OF ENGINEERING TECHNOLOGY
DEPARTMENT OF CHEMICAL ENGINEERING TECHNOLOGY

SEPARATION ENGINEERING TECHNOLOGY LABORATORY

LABORATORY INSTRUCTION SHEETS

COURSE CODE BNQ 30104

EXPERIMENT NO. EXPERIMENT 5

EXPERIMENT TITLE GAS ABSORPTION

GROUP NO.
1)
2)
3)
GROUP MEMBERS
4)
5)
6)
LECTURER/INSTRUCTOR/ 1)
TUTOR 2)
DATE OF REPORT
SUBMISSION
ATTENDANCE/PARTICIPATION/DISCIPLINE: /5%
INTRODUCTION: /5%
PROCEDURE: /5%
RESULTS& CALCULATIONS /15%
ANALYSIS /15%
DISTRIBUTION OF MARKS
FOR LABORATORY DISCUSSIONS: /20%
REPORT: ADDITIONAL QUESTIONS /15%
CONCLUSION /10%
SUGGESTIONS& RECOMENDATIONS /5%
REFERENCES: /5%
TOTAL: /100%
EXAMINER COMMENTS: RECEIVED DATE AND STAMP:
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KOD ETIKA PELAJAR DATE:

(KEP)
JABATAN TEKNOLOGI KEJURUTERAAN KIMIA

FAKULTI TEKNOLOGI KEJURUTERAAN

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saya sendiri. Saya juga mengaku tidak menerima atau memberi sebarang bantuan dalam

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tersebut di dalamnya adalah benar.

Ketua Nama:

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Ahli 1 Nama:

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1.0 OBJECTIVES

1. To demonstrate the absorption of CO2 into water using a packed column.

2. To calculate the rate of absorption of CO2 into water.
3. To determine the saturation composition of CO2 in water.

2.0 LEARNING OUTCOMES

Conduct the separation engineering principles involved in pilot plant effectively.

3.0 INTRODUCTION / THEORY

Gas absorption is a unit operation in which soluble components of a gas mixture are dissolved in a liquid phase. The inverse
operation, called stripping or desorption, is employed when it is desired to transfer volatile components from a liquid mixture
into a gas phase. Both absorption and desorption processes, common to distillation, make use of special equipment for
bringing gas and liquid phases into intimate contact.

3.1 Gas-Liquid Equilibrium

Consider a system in which a gaseous component A is in equilibrium with both air and water at a given temperature. The
equilibrium relationship between the partial pressure, pA in the gas phase and the composition, xA in the liquid phase can often
be expressed by a straight line Henry’s Law equation at low concentrations.

pA = H xA [1]

where H is the Henry’s Law constant for the given system expressed in atm/mole fraction. If both sides of the equation is
divided by the total pressure, P in atm, the composition, yA in the gas phase can be related below:

yA = H’ xA [2]

where H’ is equal to H/P. However, H is more often used because it is independent of the total system pressure. Equilibrium
data for most systems follow Henry’s Law up to a concentration of about 1 mol% in the liquid phase.

pA
equilibrium
data
Henry’s Law

xA
Figure 1: Equilibrium data and Henry’s Law
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3.2 Single Stage Equilibrium Process

Before evaluating the design calculations of an absorption column, it is important to understand the principles of a single stage
equilibrium process. It is defined as one in which two different phases are brought into intimate contact with each other and
then are separated. Various components transfer between the two phases and are essentially at equilibrium with each other
after considerable mixing. The process can be represented in Figure 2 below.

V1, V2,
yA1 yA2

L0, L1,
xA0 xA1
Figure 2: Single stage equilibrium process

The following material balances can be carried out around the single-stage equilibrium process:

Total material: L0  V2  L1  V1 [3a]

Component A: L0 x A0  V2 y A2  L1x A1  V1y A1 [3b]

For a gas-liquid system, the solute A is usually in the gas phase V with inert gas and in the liquid phase L with inert liquid.
Assuming that the gas is insoluble in the liquid phase and that the liquid does not vaporize to the gas phase, both L and V
phases contain only binary components. Therefore, the component balance on A from equation [3b] can be rewritten as:

 x   y   x   y 
L'  A0   V '  A2   L'  A1   V '  A1  [4]
 1  x A0   1  y A2   1  x A1   1  y A1 
where L’ is the amount of inert liquid and V’ is the amount of inert gas, both of which are usually known in a process.

To solve the above equation, Henry’s Law can be used for dilute solutions, or else the actual equilibrium data must be
available.

3.3 Operating Line Equation

In a packed absorption column, variations in composition are continuous from one end to the other. Material balances for the
portion of the column above an arbitary section, as shown by the dashed box in Figure 3, are similar to the single stage
equilibrium process. However, the subscript for component A is dropped since it is the only component being transferred
between phases.

Total material: LT  V  L  VT [5a]

Component A: LT xT  Vy  Lx  VT y T [5b]

By rearranging the component A material balance in equation [5b], the relationship between x and y at any point in the column
can be obtained. This relationship is called the operating line equation.

L V y  LT xT
y x T T [6]
V V
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VT, yT

LT, xT

V, y L, x

LB, xB
VB, yB

Figure 3: Material balance diagram for packed absorption column

The operating line can be drawn on a graph along with the equilibrium curve, as shown in Figure 4. It must lie above the
equilibrium line in order for absorption to take place, since this gives a positive driving force for transfer of solute from the gas
phase into the liquid phase. The absorption process (solute transfer) will thus make the total gas rate V decrease as the gas
passes through the column, and the flow of liquid L increases. These changes cause the operating line to be slightly curved.

B
yB
equilibrium
operating line line

T
yT

x
xT xB
Figure 4: Operating line for absorption process

For the case of A being absorbed between inert gas and liquid phases, the material balance on component A around the
dashed box can take the form of:

 x   y   x   y 
L'  T   V '    L'    V '  T  [7]
 1  xT   1 y   1 x   1  yT 
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where L’ and V’ are flows of inert liquid and gas respectively throughout the column. These flows are always constant

However, for dilute mixtures containing less than 10% soluble gas, the effect of changes in total flow is usually neglected and
the design is based on the average flow rates. In this case, the terms (1–x) and (1–y) will be close to 1 and equation [7] will
become:

L' xT  V ' y  L' x  V ' y T

L'  L' x 
y  x   yT  T  [8]
V'  V' 

The operating line in equation [8] has a constant slope of L’/V’ and is essentially straight for dilute mixtures.

When the solute is being transferred from the liquid phase into the gas phase, the process is called desorption or stripping.
The operating line equation for the desorption process is similar to the above, but the location of the operating line is below
the equilibrium line, as shown in Figure 5. This will give a positive driving force for transfer of solute from the liquid phase into
the gas phase.

y
equilibrium
curve
T
yT

operating line
yB B
x
xB xT

Figure 5: Operating line for desorption (stripping) process

3.4 Mass Transfer in Absorption Process

In an absorption process, two immiscible phases (gas and liquid) are present in which the solute will diffuse from one phase to
the other through an interface between the two phases. For a solute A to diffuse from the gas phase V into the liquid phase L,
it must first pass through phase V, the interface, and then into phase L in series. A concentration gradient has to exist to allow
the mass transfer to take place through resistances in each phase, as illustrated in Figure 6.

The concentration in the bulk gas phase, yL decreases to yi at the interface, while the liquid concentration starts at xi at the
interface and drops to the bulk liquid phase concentration xL. There is usually negligible resistance to mass transfer across
the interface, thus xi and yi are in equilibrium with each other and are related in an equilibrium relationship.
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interface

liquid phase, L yV

xi yi
gas phase, V
xL

distance from interface

Figure 6: Concentration profile for diffusion across the gas-liquid interface

There are typically two types of diffusions in an absorption process:

(i) Equimolar counterdiffusion – two components diffusing across the interface, one from the gas to liquid phase, while the
other from the liquid to gas phase.
(ii) Diffusion through stagnant or nondiffusing phase – only one component diffuses across the interface through stagnant
gas and liquid phases.

For a gas absorption process, it is common that only one solute component diffuses through stagnant gas and liquid phases.
The mass transfer calculations for one-way diffusion are more complicated than equimolar counterdiffusion since it involves
unequal molar flux across the interface. Derivation of the mass transfer equations will not be discussed in detail and can be
consulted in any transport processes book.

Generally, the rates of mass transfer in a packed absorption column can be quantified by four different equations:

N A  k y a y  y i 
Gas film: [9a]
Liquid film: N A  k x ax i  x  [9b]
N A  K y a y  y * 
Overall gas: [9c]
Overall liquid: N A  K x ax * x  [9d]

in which:
NA = rate of absorption
kx,y = individual film mass transfer coefficient
Kx,y = overall mass transfer coefficient
a = interfacial area per unit packing volume
x = concentration in liquid phase
y = concentration in gas phase
xi = concentration at the liquid interface
yi = concentration at the gas interface
x* = liquid phase concentration in equilibrium with gas phase
y* = gas phase concentration in equilibrium with liquid phase

The coefficients kya, kxa, Kya and Kxa are based on unit volume. It is not necessary to calculate or predict the value of a
since it is incorporated into the volumetric coefficients.
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By combining equations [9a] and [9b], the interface composition (xi, yi) can be obtained as follows:

y  y i  k x a

x i  x  k y a [10]

A line drawn with the slope of (–kxa / kya) from the operating line will intersect the equilibrium line at the interface composition
(xi, yi). This is shown in Figure 7.

y
m
operating line

equilibrium
y line

yi

y* slope = (–kxa /
kya)

x
x xi x
* compositions
Figure 7: Interface and equilibrium

The overall driving forces for absorption are represented by the vertical or horizontal line distances on the x-y diagram. The
overall coefficients Kya and Kxa can be related to the gas or liquid film coefficients kya and kxa by the local slope of the
equilibrium curve, m as follows:

1 1 m
 
Kya kya kxa
[11a]
1 1 1
 
K x a k x a mk y a
[11b]

The resistances to mass transfer in the gas film and liquid film are characterized by the terms 1/(kya) and 1/(kxa) in equations
[11a & b] respectively. When these two coefficients are of roughly the same magnitude, and m is very much larger than 1.0,
the mass transfer is said to be liquid film controlling. This means that any change in the liquid film coefficient kxa will effect a
nearly proportional change on both Kya and Kxa, while change in the gas film coefficient kya will have little effect.

For example, Henry’s Law coefficient for CO2 in water at 20°C and 1 atm is 1430 (which equals the value of m). This shows
that the absorption of CO2 in water is a liquid film controlling process. Therefore, the CO2 absorption rate can be increased by
increasing the value of kxa (i.e. increase liquid velocity) but not by increasing the value of kya (i.e. increase gas velocity).

Inversely, when the solubility of a gas is very high in liquid (such as HCl and NH3 in water), the value of m is very small and
the mass transfer is said to be gas film controlling. This means that a change in kya will have a much larger effect on the
overall values of Kya and Kxa, thus absorption rate, than a change in kxa. However, gases with intermediate solubility are
somewhat equally controlled by both gas and liquid film resistances.
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where L’ and V’ are flows of inert liquid and gas respectively throughout the column. These flows are always constant

However, for dilute mixtures containing less than 10% soluble gas, the effect of changes in total flow is usually neglected and
the design is based on the average flow rates. In this case, the terms (1–x) and (1–y) will be close to 1 and equation [7] will
become:

L' xT  V ' y  L' x  V ' y T

L'  L' x 
y  x   yT  T  [8]
V'  V' 

The operating line in equation [8] has a constant slope of L’/V’ and is essentially straight for dilute mixtures.

When the solute is being transferred from the liquid phase into the gas phase, the process is called desorption or stripping.
The operating line equation for the desorption process is similar to the above, but the location of the operating line is below
the equilibrium line, as shown in Figure 5. This will give a positive driving force for transfer of solute from the liquid phase into
the gas phase.

y
equilibrium
curve
T
yT

operating line
yB B
x
xB xT

Figure 5: Operating line for desorption (stripping) process

3.4 Mass Transfer in Absorption Process

In an absorption process, two immiscible phases (gas and liquid) are present in which the solute will diffuse from one phase to
the other through an interface between the two phases. For a solute A to diffuse from the gas phase V into the liquid phase L,
it must first pass through phase V, the interface, and then into phase L in series. A concentration gradient has to exist to allow
the mass transfer to take place through resistances in each phase, as illustrated in Figure 6.

The concentration in the bulk gas phase, yL decreases to yi at the interface, while the liquid concentration starts at xi at the
interface and drops to the bulk liquid phase concentration xL. There is usually negligible resistance to mass transfer across
the interface, thus xi and yi are in equilibrium with each other and are related in an equilibrium relationship.
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interface

liquid phase, L yV

xi yi
gas phase, V
xL

distance from interface

Figure 6: Concentration profile for diffusion across the gas-liquid interface

There are typically two types of diffusions in an absorption process:

(iii) Equimolar counterdiffusion – two components diffusing across the interface, one from the gas to liquid phase, while the
other from the liquid to gas phase.
(iv) Diffusion through stagnant or nondiffusing phase – only one component diffuses across the interface through stagnant
gas and liquid phases.

For a gas absorption process, it is common that only one solute component diffuses through stagnant gas and liquid phases.
The mass transfer calculations for one-way diffusion are more complicated than equimolar counterdiffusion since it involves
unequal molar flux across the interface. Derivation of the mass transfer equations will not be discussed in detail and can be
consulted in any transport processes book.

Generally, the rates of mass transfer in a packed absorption column can be quantified by four different equations:

N A  k y a y  y i 
Gas film: [9a]
Liquid film: N A  k x ax i  x  [9b]
N A  K y a y  y * 
Overall gas: [9c]
Overall liquid: N A  K x ax * x  [9d]

in which:
NA = rate of absorption
kx,y = individual film mass transfer coefficient
Kx,y = overall mass transfer coefficient
a = interfacial area per unit packing volume
x = concentration in liquid phase
y = concentration in gas phase
xi = concentration at the liquid interface
yi = concentration at the gas interface
x* = liquid phase concentration in equilibrium with gas phase
y* = gas phase concentration in equilibrium with liquid phase

The coefficients kya, kxa, Kya and Kxa are based on unit volume. It is not necessary to calculate or predict the value of a
since it is incorporated into the volumetric coefficients.
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3.5 Limiting Liquid to Gas Ratio

In an absorption process, the inlet gas flow, VB and its composition, yB are generally known. The outlet gas concentration, yT is
also fixed as a requirement for the absorption column, and the inlet liquid concentration, xT is also set by the process
requirements. This leaves the amount of entering liquid flow, LT to choice.

Referring to Figure 9, if the liquid flow is decreased, the upper end of the operating line will shift to the direction of the
equilibrium line, and the concentration of the outlet liquid, xB will obviously increase. The maximum possible outlet liquid
concentration and minimum possible liquid flow rate are obtained when the operating line just touches the equilibrium line at
point B1. In some cases if the equilibrium line is concaved downwards, the minimum liquid flow rate is reached when the
operating line becomes tangent to the equilibrium line.

y equilibrium
line

B B1
yB
operating line
yB*
operating line with
T minimum L/V
yT

x
xT xB xB*

Figure 10: Limiting liquid to gas ratio

At this limiting condition, an infinitely high packed absorption column is necessary, since the driving forces for mass transfer
become zero at point B1 at the bottom of the column. In an actual column, the liquid flow rate must be greater than this
minimum to achieve the required change in the outlet gas composition.

The choice of optimum liquid to gas ratio, L/V must obviously be more than the minimum ratio. Since the driving force for
mass transfer (y – y*) is proportional to the vertical distance between the operating line and the equilibrium line, increasing the
L/V ratio will increase the driving force along the column, thus reducing the height of the column. However, the higher liquid
flow rate will give a more dilute product, which makes it more difficult to recover the solute by desorption. This in turn
increases the energy cost for desorption.

As a general rule, the optimum liquid flow rate should be between 1.1 and 1.5 times the minimum value, unless the liquid is
meant to be discarded and not regenerated.
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4.0 EQUIPMENTS & MATERIALS

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5.0 PROCEDURES

5.1 General Start-up Procedures

1. Ensure all valves are initially closed.

2. Check that all gas connections are properly fitted.
3. Switch on the air compressor and allow the pressure to build up until 5 bar.
4. Open the valve at the CO2 cylinder. Set the supply pressure to between 4 to 5 bars by turning the air filter regulator knob
clockwise.
5. Open the valve at the air gas supply. Set the supply pressure to between 2 to 3 bars by turning the gas regulator knob
clockwise.

5.2 General Shut-Down Procedures

1. Switch off the circulation pumps P1 and air compressor.

2. Close valves V1, V2 and V3.
3. Close the valve on the air compressor and release the supply pressure by turning the air filter regulator knob
counterclockwise all the way.
4. Close the valve at the CO2 gas supply and release the supply pressure by turning the gas regulator knob
counterclockwise all the way.
5. Drain all liquid in the column K1 by opening valve V5.
6. Drain all liquid from the sump tanks B1 and B2 by opening valves V7 and V9.

5.3 Liquid Sampling Procedures

Samples can be taken from the liquid in the sump tank B1 for analysis. The sampling valve is located at V5 for outlet liquid
from absorption column K1.

The procedures for collecting a sample are as follows:

(i) Place a vial below the sampling valve.

(ii) Collect about 150 mL of sample using vial.
(iii) Use pipette to collect 100ml of sample from the sample collected and analyze the acidity of sample using method
described in section 5.4 or section 5.5.

5.4 Analysis of Dissolved Carbon Dioxide, CO2 in Water, H2O

Water for absorption experiment should be deionised because presence of dissolved salts could affect the analysis method
as described below.

CHEMICALS NEEDED:

a) Deionised and CO2 free water

b) Phenolphthalein indicator (AR grade)
c) 1 L of standard 0.05 M sodium hydroxide (NaOH) solution
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PROCEDURES:

1. Obtain a sample as in Section 5.3.

2. Prepare exactly 100 mL of sample in a conical flask.
3. Add 5–10 drops of phenolphthalein indicator. If the sample turns red immediately, no free CO 2 is present. If the sample
remains colorless, titrate with the standard 0.05 M NaOH solution.
4. Measure the volume of 0.05 M NaOH required reaching the end point. The end point occurs when a definite pink colour
persists in the solution for longer than 30 seconds.

5.5 EXPERIMENT: Absorption of Carbon Dioxide from Air into Water

1. Perform the general start-up procedures as described in Section 5.1.

2. Fill the sump tank B1 with up to 40-L of fresh water. Open valve V4 and V6.
3. Switch on circulation pump P1 and allow the water to bypass into the sump tank B1 via valve V4.
4. Introduce air and CO2 mixtures into the absorption column K1 as follows:
i. Determine the appropriate air and CO2 gas flow rate in order to achieve the desired inlet gas composition for the
absorption process.
ii. Open and adjust valve V1 to set the flow rate of gas CO2, FT-101.
iii. Open and adjust valve V2 to set the flow rate of air, FT-102
5. Record the initial CO2 concentration in the sump tank B1 as the feed composition value.
6. Introduce liquid into the absorption column K1 as follows:
i. Slowly open valve V3 and fully open V5.
ii. Observe liquid entering the top of the absorption column, flowing down the column and back into the sump tank B1.
iii. Adjust valve V3 to fix the desired inlet liquid flow rate at FT-103
7. At regular intervals of 5 minutes, collect a sample from the outlet liquid of the absorption column K1 as described in
Section 5.3. Analyze the collected sample to determine the concentration of dissolved CO 2 in water as described in
Section 5.4.
8. Continue to record data and collect liquid and gas samples until the CO2 composition in the sump tank B1 and the outlet
gas has reached a steady value.
9. Repeat the experiment by changing the gas flow rate, gas inlet composition and liquid flow rate.
10. Stop the experiment and perform the general shut-down procedures as described in Section 5.2.

RECOMMENDATIONS:

Variables Range
Air flow rate 3 M3/Hr
CO2 gas flow rate 4-8 L/min
Inlet gas composition 9-16 vol%
Liquid flow rate 4.0 L/min
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6.0 RESULTS & CALCULATION

EXPERIMENTAL RESULTS FOR GAS ABSORPTION UNIT (BP50-80G)

Experiment 1: Absorption of Carbon Dioxide from Air into Water

Experimental condition:
Concentration of NaOH for Titration: 0.05 M

Data set 1: 9% CO2 in Gas Feed

CO2 Feed Rate: 4 LPM
Air Feed Rate: 6 M3/Hr
H2O Feed Rate: 4 LPM
Volume of water in Sump Tank, B1 = 40L

Data Set 2: 16% CO2 in Gas Feed

CO2 Feed Rate: 7 LPM
Air Feed Rate: 4 M3/Hr
H2O Feed Rate: 4 LPM
Volume of water in Sump Tank, B1 = 40L
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Table 1.1: Experimental result for CO2 absorption

Time Vol. NaOH for Titration (mL)
(min) 9% CO2 16% CO2
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: SEPARATION
REVISION NO:
ENGINEERING TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: GAS
ABSORPTION AMENDMENT
DATE:

Table 1.2: Concentration of CO2 in Feed Tank, B1

Time Conc. Of CO2 in Feed Tank (mole/L)
(min) 9%CO2 16%CO2
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: SEPARATION
REVISION NO:
ENGINEERING TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: GAS
ABSORPTION AMENDMENT
DATE:

7.0 DATA ANALYSIS

1. Plot the CO2 concentration in the inlet water flow as a function of time.

Sample calculation of Concentration of CO2 in Feed Tank

Let say volume of NaOH needed to reach end point = y ml,

Molarity of NaOH = 0.05 mol/L,
Volume of sample collected = 0.1 L

Thus,
y mol
L  0.05
1000 L
Concentration of CO2 in Feed Tank = 0.1L

By using the calculated concentration of CO2 in Feed Tank, plot the graph of Concentration of CO2 in Feed Tank versus Time.

2. Calculate the rate of absorption of CO2 into water

[conct  x  conct 0 ]
Rate of absorption of CO2 into water =  VT
sec
x min  60
min

In which VT = volume of water in feed tank, B1 (L)

Conc t=x = concentration of CO2 at t = x
 FACULTY: ENGINEERING EDITION:
TECHNOLOGY
LABORATORY: SEPARATION
REVISION NO:
ENGINEERING TECHNOLOGY

EFFECTIVE DATE: 1/3/2014

EXPERIMENT: GAS
ABSORPTION AMENDMENT
DATE:

8.0 DISCUSSION & CONCLUSION

Prepared by / Disahkan oleh: Approved by / Disahkan oleh :

Signature/Tandatangan: Signature / Tandatangan :

Name/Nama: DR. NOR FAIZAH BINTI RAZALI Name / Nama : DR. NOOR AKHMAZILLAH BINTI MOHD
FAUZI
Date/Tarikh :
Date / Tarikh :