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TITLE OF EXPERIMENT

Experiment 6: Gas Absorption

OBJECTIVE

 To determine the mass transfer coefficient of oxygen (O2) through a wetted wall
absorption column.

INTRODUCTION

Gas absorption is a common process where a gaseous mixture is contacted with a


liquid to selectively dissolve one or more components, by means of mass transfer
from the gas stream to the liquid stream. The gas components transferred to the liquid
is known as the solute or absorbate, whereas the liquid itself is called the solvent or
absorbent. This process is carried out in the industry primarily to remove impurities or
recover valuable chemicals (Seader, Henley and Roper, 2010).

In this experiment, a gas absorption demonstration unit is used to calculate the


mass transfer coefficient of oxygen into water. To begin, a stream of nitrogen gas is
passed through water in a deoxygenation column to effectively remove oxygen from
the water. This deoxygenated water is directed into a column, flowing down its wall
uniformly. A stream of air from the surroundings is then passed upwards through the
core of the column to “re-oxygenate” it.

By varying the flow rate of deoxygenated water at constant air flow rate, the inlet
and outlet concentrations of oxygen in the water can be obtained. With this, the mass
transfer coefficient of oxygen, KL can be determined by relating its two dimensionless
quantities – Reynolds number, Re and Sherwood number, Sh. The Reynolds number
is the ratio of inertial forces to viscous forces whereas the Sherwood number is the
ratio of mass transfer rate to its diffusion rate (Subramanian, 2014).
MATERIALS AND EQUIPMENT

1. Gas absorption demonstration unit


2. Nitrogen gas, N2 supply
3. Air supply from surroundings
4. Water stored in tank

Figure 1.0: Gas Absorption Demonstration Unit


RESUTLS

Table 1.1: Definition of Variables Used in Tables

Variable Definition
FI1 Flow rate of air entering column C1
FI2 Flow rate of deoxygenated water exiting column C2

AI1 Properties of deoxygenated water before entering column C1


AI2 Properties of deoxygenated water after exiting column C1

NA Rate of mass transfer

cAi ∗ Concentration of oxygen in aqueous phase

KL Overall mass transfer coefficient


Re Reynolds number

Sh Sherwood number

Constant Flow Rate of Air (FI1)

Table 1.2: Concentration of O2 and Temperature of Deoxygenated Water at


Constant Flow Rate of Air at 50 nL/h

AI1 AI2
FI1 FI2
Concentration Temperature Concentration Temperature
(nL/h) (L/h)
of O2 (mg/L) (°C) of O2 (mg/L) (°C)
50 5.0 0.56 26.4 6.39 24.6
50 7.5 0.33 27.4 6.47 25.7

50 10.0 0.17 28.8 6.50 27.5


50 12.5 0.17 29.1 6.41 28.1
50 15.0 0.16 28.8 6.19 28.2
Table 1.3: Calculated Parameters for Gas Absorption Process at Constant Flow
Rate of Air at 50 nL/h

FI1 FI2 NA cAi ∗ KL


Re Sh ln Re ln Sh
(nL/h) (L/h) (g/m2·s) (mg/L) (m/s)
50 5.0 8.426×10-5 8.881 1.013×10-5 58.06 3645 4.061 8.201
50 7.5 1.331×10-4 8.881 1.557×10-5 87.08 5604 4.467 8.631

50 10.0 1.830×10-4 8.881 2.101×10-5 116.11 7562 4.755 8.931


50 12.5 2.255×10-4 8.881 2.588×10-5 145.14 9318 4.978 9.140
50 15.0 2.614×10-4 8.881 2.998×10-5 174.17 10793 5.160 9.287

Table 1.4: Concentration of O2 and Temperature of Deoxygenated Water at


Constant Flow Rate of Air at 200 nL/h

AI1 AI2
FI1 FI2
Concentration Temperature Concentration Temperature
(nL/h) (L/h)
of O2 (mg/L) (°C) of O2 (mg/L) (°C)
200 5.0 0.13 28.4 6.41 27.6
200 7.5 0.20 28.3 6.49 27.4
200 10.0 0.15 29.2 6.54 28.0
200 12.5 0.14 29.8 6.46 28.6
200 15.0 0.13 29.6 6.23 28.8

Table 1.5: Calculated Parameters for Gas Absorption Process at Constant Flow
Rate of Air at 200 nL/h

FI1 FI2 NA cAi ∗ KL


Re Sh ln Re ln Sh
(nL/h) (L/h) (g/m2·s) (mg/L) (m/s)
200 5.0 9.076×10-5 8.881 1.037×10-5 58.06 3734 4.061 8.225
200 7.5 1.364×10-4 8.881 1.571×10-5 87.08 5655 4.467 8.640
200 10.0 1.847×10-4 8.881 2.116×10-5 116.11 7616 4.755 8.938
200 12.5 2.284×10-4 8.881 2.613×10-5 145.14 9405 4.978 9.149
200 15.0 2.645×10-4 8.881 3.022×10-5 174.17 10881 5.160 9.295
Constant Flow Rate of Deoxygenated Water (FI2)

Table 1.6: Concentration of O2 and Temperature of Deoxygenated Water at


Constant Flow Rate of Deoxygenated Water at 5.0 L/h

AI1 AI2
FI1 FI2
Concentration Temperature Concentration Temperature
(nL/h) (L/h)
of O2 (mg/L) (°C) of O2 (mg/L) (°C)
50 5.0 0.11 29.1 6.09 28.2

100 5.0 0.16 29.8 6.08 27.9


150 5.0 0.16 29.5 6.12 27.9
200 5.0 0.16 29.8 6.08 28.1
250 5.0 0.16 30.3 6.01 28.3

Table 1.7: Concentration of O2 and Temperature of Deoxygenated Water at


Constant Flow Rate of Deoxygenated Water at 10.0 L/h

AI1 AI2
FI1 FI2
Concentration Temperature Concentration Temperature
(nL/h) (L/h)
of O2 (mg/L) (°C) of O2 (mg/L) (°C)
50 10.0 0.13 31.5 6.13 29.8
100 10.0 0.13 31.3 6.10 29.9
150 10.0 0.13 30.8 6.14 29.5
200 10.0 0.13 30.5 6.28 29.2
250 10.0 0.11 30.3 6.34 28.9
CALCULATIONS

Column height, h = 0.9 m

Column diameter, d = 0.034 m

Molecular weight of oxygen, O2 = 32 g/mol

Henry’s law constant for oxygen, H = 756.7 L·atm/mol

Mass diffusivity of oxygen in water, D = 2.5 × 10-9 m2/s

Wetted perimeter, 𝑊 = 𝜋𝑑 = 𝜋(0.034 m) = 0.1068 m

𝑑
Surface area between gas & liquid = 2𝜋𝑟ℎ = 2𝜋 ( ) ℎ = 𝜋𝑑ℎ
2

= 𝜋(0.034 m)(0.9 m)

= 0.0961 m2

From Perry’s Chemical Engineer Handbook,

The viscosity of water at 25oC can be found by interpolation.

Temperature (K) Viscosity × 10-6 (Pa·s)


290 1084
298.16 𝜇𝑓
300 853.84

𝜇𝑓 − 853.84 298.16 − 300


=
1084 − 853.84 290 − 300

kg
𝜇𝑓 = 8.96 × 10−4
m. s

Henry’s law states that at certain fixed temperature, the partial pressure will be
directly proportional to concentration.

𝑝𝐴𝑖 = 𝐻𝑐𝐴𝑖 ∗

𝑝𝐴𝑖 0.21 × 1 atm


𝑐𝐴𝑖 ∗ = = = 8.881 mg/L
𝐻 L. atm mol 1g
756.7 × ×
mol 32 g 1000 mg
From Table 1.2,

At constant flow rate of FI1 = 50 nL/h and FI2 = 5.0 L/h

Rate of mass transfer,

1
𝑁𝐴 = FI2 × (𝑐out − 𝑐in ) ×
gas − liquid interface area

L 1h mg 1g 1
= 5.0 × × (6.39 − 0.56) × ×
h 3600 s L 1000 mg 0.0961 m2

g
= 8.426 × 10−5
m2 . s

Rate of mass transfer in terms of bulk liquid concentration

𝑁𝐴 = 𝐾𝐿 (𝑐𝐴𝑖 ∗ − 𝑐𝐴𝐿 )

Where 𝑐𝐴𝐿 is the concentration of oxygen in water going into the column.

g
𝑁𝐴 8.426 × 10−5 2
𝐾𝐿 = ∗ = m .s
𝑐𝐴 − 𝑐𝐴𝐿 (8.881 − 0.56) mg 1 g 1000 L
× ×
L 1000 mg 1 m3

g
8.426 × 10−5 2
= m .s
g
8.321 3
m

= 1.0126 × 10-5 m/s

The dimensionless equation,

(Sh)L ∝ (Re)𝑛L

Let k be the proportionality constant.

(Sh)L = 𝑘 (Re)𝑛L

ln(ShL ) = ln[𝑘 (ReL )𝑛 ]

ln(ShL ) = ln(ReL )𝑛 + ln 𝑘

ln(ShL ) = 𝑛 ln(ReL ) + ln 𝑘
Sherwood number,

−5 𝑚
𝐾𝐿 𝐿 1.0126 × 10 𝑠 × 0.9 𝑚
Sh = = = 3645.4
𝐷 2.5 × 10−9 𝑚2 /𝑠

ln Sh = 8.201

Reynolds number,

4𝑤
Re =
𝜇𝐿 𝑊

L kg 1 m3 1h
4 (5.0 × 1000 3 × 1000 L × 3600 s)
h m
=
𝑘𝑔
8.96 × 10−4 𝑚. 𝑠 × 0.1068 m

= 58.056

ln Re = 4.061

These remaining values for ln Re and ln Sh at constant flow rate of air at 5 L/h are
tabulated in Table 1.3, then used to plot the graph as in Figure 1.1 below.

Graph of ln Sh against ln Re
9.4

9.2

8.8
ln Sh

ln Sh = 0.9968 ln Re + 4.1686
8.6 R²= 0.9979

8.4

8.2

8
4 4.2 4.4 4.6 4.8 5 5.2 5.4
ln Re

Figure 1.1: Graph of ln Sh against ln Re for constant flow rate of air at 50 nL/h
From graph in Figure 1.1,

The equation of the straight line in the general linear equation form, y = m x + c is

ln Sh = 0.9968 ln Re + 4.1686

And by comparison with the dimensionless quantity relation,

ln(ShL ) = 𝑛 ln(ReL ) + ln 𝑘

The gradient of this straight line is 0.9968, and the y-intercept value is 4.1686.

So, n = 0.9968 which is almost equal to 1, which shows these dimensionless


quantities have directly proportional relationship.

Also, the proportionality constant can be found as,

ln 𝑘 = 4.1686

𝑘 = 𝑒 4.1686 = 64.625
From Table 1.5, the following graph in Figure 1.2 is plotted.

Graph of ln Sh against ln Re
9.4

9.2

8.8
ln Sh

ln Sh = 0.9836 ln Re + 4.242
8.6 R²= 0.9985

8.4

8.2

8
4 4.2 4.4 4.6 4.8 5 5.2 5.4
ln Re

Figure 1.2: Graph of ln Sh against ln Re for constant flow rate of air at 200 nL/h

The equation of the straight line in the general linear equation form, y = m x + c is

ln Sh = 0.9836 ln Re + 4.242

ln(ShL ) = 𝑛 ln(ReL ) + ln 𝑘

Gradient, n = 0.9836

y-intercept value, ln 𝑘 = 4.242

With n = 0.9836 which is almost equal to 1, this shows these dimensionless quantities
have directly proportional relationship.

Also, the proportionality constant can be found as,

ln 𝑘 = 4.242

𝑘 = 𝑒 4.242 = 69.547
DISCUSSIONS

A wetted-wall gas absorption demonstration unit was used in this experiment to


determine the mass transfer coefficient of oxygen. A schematic diagram of the
apparatus used is illustrated as below.

Figure 2.1: Schematic Diagram of the Wetted-Wall Absorption Column

Firstly, a stream of nitrogen gas supply is passed through the deoxygenated


column (C2) to sweep out the oxygen from water supplied by pump G1. For this,
valves V1 and V3 are opened. The gas in column C2 then leaves through an opening
at the top of the column to the surroundings.

The deoxygenated water will flow into absorption column (C1) with the help of
pump G2, with its flow rates manipulated by rotameter FI2. In column C1, a stream of
air is supplied by compressor P1 and controlled by rotameter FI1. This stream of air
will oxygenate the water flowing down along the absorption column C1. The two
probes AI1 and AI2 functions to measure the inlet and outlet concentration of
dissolved oxygen in the water through column C1, and displays these readings at the
control panel together with their temperature measurements.

Findings

Based on the overall results, the outlet deoxygenated water leaving column C1
has higher concentration of oxygen compared to the inlet of deoxygenated water
entering the same column. This is because mass transfer occurred between gas and
liquid as the oxygen molecules from air stream diffused into the deoxygenated water
when in contact with each other in the column. From Table 1.3 with constant flow
rate of air at 50 nL/h, the rate of mass transfer, NA increases as the flow rate of
deoxygenated water increases. This increasing rate of mass transfer is due to the
increasing water flow rate that allows more oxygen from the air stream to diffuse into
the deoxygenated water stream.

As for Table 1.5, when the constant air flow rate increased to 200 nL/h, the rate
of mass transfer values are slightly higher than those at 50 nL/h. This is because there
are more oxygen molecules that are available to diffuse into the deoxygenated water
stream which results in a higher net mass transfer.

On the other hand, in Table 1.6, where water flow rate is set constant to 5 nL/h
and air flow rate is varied, the outlet concentration of oxygen of the 5 sets data are
approximately the same and the values are much lower compared to Table 1.2 where
the air flow rate is constant. This may due to the oxygen concentration in the water
has reached saturation as the water flow rate is constant while the air flow rate
continues to increase. Despite the concentration of oxygen in the air is increasing, the
net mass transfer is zero because gas phase and liquid phase has reached an
equilibrium state. The concentration gradient slowly decreases and approach zero.
Thus, the net mass transfer is zero.
Furthermore, based on the trend of the results, the outlet temperatures of water
are higher than the inlet temperatures of water. This is because the surrounding air
that is directed into absorption column C1 is at a room temperature of around 25oC as
air conditioning is turned on in the lab. This effectively cools the water as it flows
through the column passing by the water at the same time mass transfer took place.
Therefore, this resulted in a lower temperature of water when it exits the column.

In fluid flow, Sherwood number, Sh is the dimensionless group for convective


mass transfer. It represents the ratio between mass transfer by convection and mass
transfer by diffusion. On the other hand, Reynolds number, Re is a dimensionless
number that gives a measure of the ratio of inertial forces to viscous forces
(Subramanian, 2014). The values of Sherwood number and Reynolds number are
calculated for the varied water flow rate when the air flow rates are constant. By using
the natural logarithm of these two quantities, a graph of ln Sh against ln Re is plotted
as in Figure 1.1. The equation ln Sh = n ln Re + ln k is compared with the equation of
best-fit line obtained from the graph. By comparison, the gradient, n is found to be
very close to 1. Therefore, it can be deduced that the logarithmic of Sherwood number
is almost directly proportional to the logarithmic of Reynolds number.

When ln Re approaches zero (Re =1), the value 4.1686 is the y-intercept which is
also representing ln k. In other words, when Reynolds number equals to 1, the
Sherwood number equals to 64.625. Further investigating, it was found that the ratio
of Reynolds number to Sherwood number is around the average of 1 : 64 in this
experiment, which also means that
𝐾𝐿 𝐿 4𝑤/𝑊
= 64 ( )
𝐷 𝜇𝐿

However, as length of absorption column, L, mass diffusivity of oxygen, D, wetted

perimeter, W and water viscosity, μL are all constants, the equation above reduces to

𝐾𝐿 = 256 𝑤
So, it can be deduced that the overall mass transfer coefficient is proportional to the
water mass flow rate. As the mass flow rate of water increases, the mass transfer
coefficient will increase by a factor of around 256.

Precautionary Steps and Improvements

There are several precautions need to be concerned while doing the experiment.
First of all, the apparatus like tank and valves were checked for any leakages so that
the value obtained is accurate. Leakage can cause a pressure drop and will affect the
water and gas flow rates. In addition, the equipment has to be used in a sufficiently
ventilated environment and at atmospheric temperature. Lastly, the valve V3 has to be
controlled manually by observing and maintaining the water level in the
deoxygenated column C2. If insufficient water is allowed into column C2, the mass
transfer will not be efficient, whereas if excessive water flows into the column, it will
overflow and cause damage to the apparatus. One of the improvement method to
increase the efficiency of oxygen diffusion in water is by having a larger wetted
surface in the column. This can be achieved by having layers of plates in the
absorption column.

Applications in Industry

Moving on to the uses of gas absorption in industry, there are two categories of
absorption process – physical absorption and chemical absorption. Physical
absorption depends on the phase of matter. It can happen between liquid with gas and
liquid with solid. For chemical absorption, it depends on the stoichiometry of the
reaction and concentration of reactants (Jewell, n.d.). For gas absorption, it has the
application of gas purification. It removes carbon dioxide gas in the production of
ethylene oxide production. In addition, synthesis of chemical is one of the
applications of gas absorption. This reaction can produce compounds like nitric acid,
sulphuric acid and formaldehyde solution. Next, feedstock preparation also can be
done by gas absorption. One of the feedstock which is amine solution treating with
synthesis gas. Another example for chemical feedstock is coal gasification. In
addition, desulphurisation can be carried out with the flue gas and this is a common
application because it consists of economical requirements. Other industries
applicable with gas absorption are petroleum industry and coke extraction industry
(Thiele and Loning, 2006).

CONCLUSION

The overall mass transfer coefficient, KL of oxygen through a wetted wall


absorption column increases as the deoxygenated water flow rate increases whilst the
air flow rate is kept constant. Therefore, the rate of mass transfer also increases. From
the findings, the ratio of Reynolds number to Sherwood number is about 1:64, thus
further analysis discovered the relationship of KL = 256 w, showing that the overall
mass transfer coefficient increases by a factor of 256 with respect to the mass flow
rate of water.
REFERENCES

Green, D.W. and Perry R.H. (2008). Perry’s Chemical Engineers Handbook. (8th ed.).
New York: McGraw Hill.

Jewell, P.J. (n.d.). Cryogenic materials. The risks posed by using them. [online]
Available at:
<https://web.archive.org/web/20070812043328/http://www.bath.ac.uk/internal/
bio-sci/bbsafe/asphyx.htm#contacteff> [Accessed 6 March 2016].

Seader, J.D., Henley, E.J. and Roper, D.K. (2010). Separation process principles.
(3rd ed.). New Jersey: John Wiley & Sons.

Subramaniam, R.S. (2014). Convective mass transfer. [online] Available at:


<http://web2.clarkson.edu/projects/subramanian/ch330/notes/Convective%20M
ass%20Transfer.pdf> [Accessed 7 March 2016].

Thiele, R & Loning, J (2006). Industrial absorption current status and future aspects.
[online] Available at:
<http://www.nt.ntnu.no/users/skoge/prost/proceedings/distillation06/CD-procee
dings/paper004.pdf> [Accessed 6 March 2016].

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