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Experiment 7 - 3D

This document describes an experiment conducted by a group of chemical engineering students to determine the gas diffusion coefficient of acetone using the Stefan-Winkelmann method. The experiment involves measuring the descent of the liquid surface of acetone in a glass capillary tube over time as vapor diffuses into an air stream. The students recorded the height of the acetone column and calculated values needed to plot t/(L0-L) against (L0-L) from which the gas diffusion coefficient could be determined from the slope. The objectives were to determine the gas diffusion coefficient of acetone and the diffusivity of its vapor using this established method.

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Poh Ching Hong
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0% found this document useful (0 votes)
102 views15 pages

Experiment 7 - 3D

This document describes an experiment conducted by a group of chemical engineering students to determine the gas diffusion coefficient of acetone using the Stefan-Winkelmann method. The experiment involves measuring the descent of the liquid surface of acetone in a glass capillary tube over time as vapor diffuses into an air stream. The students recorded the height of the acetone column and calculated values needed to plot t/(L0-L) against (L0-L) from which the gas diffusion coefficient could be determined from the slope. The objectives were to determine the gas diffusion coefficient of acetone and the diffusivity of its vapor using this established method.

Uploaded by

Poh Ching Hong
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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CEB 2072 CHEMICAL ENGINEERING LABORATORY II

May 2022 Semester


5th July 2022

Chemical Engineering Department

EXP 7: Gas Diffusion Coefficient

GROUP 3D

NO. NAME STUDENT ID

1. Poh Ching Hong 19001325

2. Sashivarma A/L Saravanan 19001215

3. Mohamad Hafiz Fahmi bin Ahmad Shafie 19001324

4. Nur Athirah Munirah binti Mohd Fakhrurrozie 19001337

5. Wan Nur Alya binti Wan Abdul Manan 19001320

Page | 1
TABLE OF CONTENT

1.0 INTRODUCTION .................................................................................................................... 3

2.0 OBJECTIVES ........................................................................................................................... 4

3.0 METHODOLOGY ................................................................................................................... 5

4.0 RESULTS ................................................................................................................................. 8

5.0 DISCUSSION ......................................................................................................................... 12

6.0 CONCLUSION ....................................................................................................................... 14

7.0 REFERENCES ....................................................................................................................... 15

Page | 2
1.0 INTRODUCTION

Diffusion is a mass transfer phenomenon that happens when a component migrates within
the same phase or between phases as a result of the concentration difference between two points.
When a fluid has two or more components and there is a concentration gradient within the fluid,
one of the components will often flow in a certain direction to lessen the concentration gradient.
This process occurs in either the liquid or gas phases, or both at once. One common illustration of
diffusion occurs when liquid in an open water container evaporates into the air due to the disparity
in water vapour concentration between the surface of the water and the surrounding air.

There are two categories of diffusion which are diffusion in a uniform gradient of
concentration and diffusion in a non-uniform concentration. According to Fick's first law, which
states that diffusivity is dependent on concentration, diffusion occurs in a uniform concentration
gradient. As contrast to this, the diffusion in a gradient of non-uniform concentration follows Fick's
second law, where the diffusivity is unaffected by concentration.

In this experiment, the main aim is to study the diffusivity of vapor of a volatile liquid is
studied. The gas diffusivity coefficient of the volatile liquid is determined by using Stefan-
Winklemann’s method. This method, which is frequently used to determine a volatile liquid's
diffusivity, considers the volatile liquid's rate of evaporation, which is then followed by the rate of
descent of the liquid surface in a glass tube or diffusion cell (Coca et al., 1980). A liquid was kept
at a constant temperature inside a tube with a limited diameter and was circulated through the top
of the tube using air. All of this is done to make sure that the vapour partial pressure is transferred
from the surface of the liquid to the air.

For the apparatus, a glass capillary tube is placed in a transparent-sided temperature-


controlled water bath. A horizontal glass tube is fastened to the upper end of the capillary tube,
and a small air pump included in the device blows air through it. This configuration enables the
capillary tube to maintain a partial pressure difference between the evaporating liquid surface and
the flowing air stream. A liquid is enclosed in a limited diameter vertical tube that is kept at a
constant temperature and has an airstream passing through the top. The purpose of these is to
guarantee that molecular diffusion managed to transfer the vapour partial pressure from the liquid
surface to the air stream.

Page | 3
2.0 OBJECTIVES

The objectives of conducting this experiment are:

1. To determine the gas diffusion coefficient of acetone using the established Winkelmann’s
method.
2. To determine the diffusivity of the vapor of a volatile liquid which is acetone

Page | 4
3.0 METHODOLOGY

Start-up Procedure

1. The water bath was filled with clean water to approximately 15 mm from the top.

Figure 3.1: Clean water was filled into the water bath for about 15 mm from the top

2. The mains cable was plugged to the electrical supply. The voltage of the supply was ensured
to be correct to suit the equipment.
3. The main power on the control panel was switched on.
4. The set-point value on the temperature controller was adjusted to 55°C.
5. The heater was switched on. The water temperature was observed until it heated up to 55°C
and remained constant.
6. The air pump was switched on. The needle valve was adjusted so that a steady low velocity
of air stream would be detected at the end of flexible tubing.
7. The equipment was now ready for the experiment.

Page | 5
Figure 3.2: Start-Up Procedure

Priming Procedure for the Capillary Tube

1. The inside of the tube was cleaned.


2. A weak solution of detergent was prepared.
3. A Hirschmann pipette was used to fill the tube solution.
4. The tube was turned upside-down and shook.
5. The tube was emptied.
6. Steps 2 to 3 were repeated by using acetone.
7. The tube was now ready for the experiment.

Shut –down Procedure

1. The heater and air pump were switched off.


2. The set-point value of the temperature controller was adjusted to approximately 5°C below
the room temperature.
3. The water was allowed to cool down first until it was safe to touch. The drain valve and
the water tank were opened.
4. The flexible tubing was detached, and the capillary tube was cleaned for next use
5. The main power was switched off.

Page | 6
Experiment Procedure: Determination of the gas diffusion coefficient of acetone using the
established Winkelmann’s method.

1. The start-up procedure was performed.


2. The air pump was switched off initially.
3. The capillary tube was filled partially with acetone to a depth of about 30 mm. The two
capillary tube ends were closed with the cap provided.
4. The capillary tube was inserted through the fitting on top of the water bath cover. The
fitting was ensured to be not over-tightened.
5. The initial height of acetone filled was recorded as (L0) at time, t=0.
6. Both caps were removed and the flexible tubing from the air pump line was connected to
one end of the capillary tube. The air pump was switched on.
7. The height of acetone filled (L) was recorded for every 15 minutes interval.
8. Graph t/(L0 – L) against (L0 – L) was plotted and the value of gas diffusivity, D was
determined from the obtained slope, s.
9. The experiment value was compared with the theoretical value that can be predicted from
empirical equations (e.g., Modified Maxwell’s equation by Gililand).

Page | 7
4.0 RESULTS

Table 4.1: The experiment data for acetone height

Liquid Fall, t/ (L0-L)


Time, t (ks) L0 (mm) L (mm)
L0-L (mm) (ks/mm)
0 30 30 0 -
0.015 30 30 0 -
0.030 30 28 2 0.01500
0.045 30 27 3 0.01500
0.060 30 25 5 0.01200
0.075 30 24 6 0.01250
0.090 30 22 8 0.01125
0.105 30 21 9 0.01167
0.120 30 19 11 0.01091
0.135 30 18 12 0.01125

t/ (L0-L) vs Liquid Fall, L0-L (mm)


0.01800

0.01600

0.01400
y = -0.0004x + 0.0153
R² = 0.7813
0.01200
t/ L0-L (ks/mm)

0.01000

0.00800

0.00600

0.00400

0.00200

0.00000
0 2 4 6 8 10 12 14
Liquid Fall, L0-L (mm)

Figure 4.2: Graph of t/(L0-L) vs /(L0-L)

Page | 8
The constant temperature of the experiment = 55 °C

From the Figure 4.2, the gradient obtains is −0.0004 ks/𝑚𝑚2 which is the value for the s.
𝜌 𝐶
𝐿
𝑠 = (2𝑀𝐷 ) (𝐶 𝐵𝑀 ) = −0.0004 ks/𝑚𝑚2 = −4 × 105 s/𝑚2
𝐶
𝐴 𝑇

The molecular weight of the acetone


MWacetone = 58.08 kg/kmol = 58.08 g/mol

After that, the total molar concentration was calculated.


1 273
𝐶𝑇 = ( 3
)( )
22.4 𝑚 /𝑘𝑚𝑜𝑙 273 + 55

= 0.03716 𝑘𝑚𝑜𝑙 /𝑚3

Vapor pressure of the acetone was measured by using Antoine Equation:


For acetone: A = 14.3145, B = 2756.22 and C = 228.06
𝐵
ln 𝑃𝑉 = 𝐴 −
𝑇+𝐶
𝐵
𝑃𝑉 = exp( 𝐴 − )
𝑇+𝐶
2756.22
𝑃𝑉 = exp( 14.3145 − )
55 + 228.06
𝑃𝑉 = 97.2487 𝑘𝑃𝑎

After that, the saturation concentration at interface was calculated, CA:


𝑃𝑉
𝐶𝐴 = ( )𝐶
𝑃𝑎𝑡𝑚 𝑇
97.2487
= × 0.03716
101.325
= 0.03567 𝑘𝑚𝑜𝑙 / 𝑚3

Page | 9
Next, logarithmic mean molecular concentration of vapor, CBm (kmol/m3)

𝐶𝐵1 = 𝐶𝑇 = 0.03716 𝑘𝑚𝑜𝑙 / 𝑚3

𝑃𝑎𝑡𝑚 − 𝑃𝑉
𝐶 𝐵2 = ( ) 𝐶𝑇
𝑃𝑎𝑡𝑚
101.325 − 97.2487
𝐶 𝐵2 = ( ) (0.03716)
101.325
𝐶 𝐵2 = 0.001495 𝑘𝑚𝑜𝑙 / 𝑚3

𝐶𝐵1 − 𝐶𝐵2
𝐶𝐵𝑀 =
𝐶
ln (𝐶𝐵1 )
𝐵2

0.03716 − 0.001495
𝐶𝐵𝑀 =
0.03716
ln ( )
0.001495
𝐶𝐵𝑀 = 0.01110 𝑘𝑚𝑜𝑙 / 𝑚3

Diffusivity, D was calculated:


𝜌𝐿 𝐶𝐵𝑀
𝐷=
𝑠 (2𝑀𝐶𝐴 𝐶𝑇 )
785.7 𝑘𝑔/𝑚3 × 0.01110 𝑘𝑚𝑜𝑙/𝑚3
=
−4 × 105 s/𝑚2 (2 × 58.08 g/mol × 0.03567 𝑘𝑚𝑜𝑙/𝑚3 × 0.03716 𝑘𝑚𝑜𝑙/𝑚3 )

= −1.416 × 10−4 𝑚2 /𝑠

Lastly, percentage error was calculated.

𝑚2
According to the Youney et al. (2017): 𝐷𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 = 1.215 𝑥 10−5 𝑠

Page | 10
|𝑒𝑥𝑝𝑒𝑟𝑖𝑚𝑒𝑛𝑡 − 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙|
𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑒𝑟𝑟𝑜𝑟 = × 100%
𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙
(−1.416𝑥 10−4 ) − (1.215 𝑥 10−5 )
=
(1.215 𝑥 10−5

= 1265.4321%

Page | 11
5.0 DISCUSSION

Gaseous diffusion coefficient of air-acetone mixture at the condition of atmospheric


pressure and 55 °C (328 K) has been determined by the Winkelmann evaporation tube method. In
this experiment, a capillary tube containing volatile acetone liquid, component A was immersed
in a water bath with a constant temperature of 55 °C. A stream of air, component B was allowed
to flow over the opening end of the capillary tube so that the gaseous phase at that point is
essentially air while the gaseous phase at the liquid interface is pure acetone.

Due to the difference of the partial pressure of the acetone between both regions, acetone
liquid evaporated and travelled to the end of the capillary by the mechanism of diffusion. This
phenomenon can be explained by the random molecular movement of acetone down the
concentration gradient (Atkins, de Paula, & Keeler, 2018). Since a large volume of air is passing
by the end of capillary tube, the concentration of acetone at that point was assumed to be negligible.
Besides, the boundary at the liquid surface is impermeable to air as air is insoluble in acetone
liquid. Hence, air cannot diffuse into or away from the liquid surface. This was a case of the
diffusion of acetone through stagnant or non-diffusing air (Geankoplis, Hersel, & Lepek, 2018).

Throughout the experiment, the height of the acetone level in the capillary tube was
measured using ruler for every 15 minutes interval. All data was then tabulated in Table 4.1 to
determine the falling rate of the liquid level in the capillary tube over time, which was used as an
indicator of the evaporation rate of acetone or the diffusion rate of acetone through the air. By
plotting t/(L0 – L) against (L0 – L), a graph with a slope, s of −0.0004 ks/𝑚𝑚2 , as illustrated in
Figure 4.1, was obtained for diffusion coefficient calculation. It was determined that the gas
diffusion coefficient or diffusivity of acetone in air was determined to be −1.416 × 10−4 𝑚2 /𝑠.

To determine the validity of the result, the experimental value of diffusivity was compared
with the theoretical value, 1.215 × 10−5 𝑚2 /𝑠 that was predicted from Modified Maxwell’s
equation by Gililand (Youney et al.,2017). It was found that the percentage error of experimental
result was 1265.4321% which is considered high. The deviation might be due to the certain errors
made during conducting the experiment.

Page | 12
Errors and Modifications
It is believed that some errors had taken place during the experiment as there is some
deviation between the experimental value and the theoretical value. There are two types of errors
that commonly occur in experiments which are random errors and systematic errors. Random
errors cause readings to differ from one another, affecting measurement precision. Hence, the
results may fluctuate slightly from the precise reading. The source of this inaccuracy could be that
the observer's eyes are not aligned with conventional ruler when measure the acetone level in the
capillary tube. To prevent inaccuracy in measurements caused by this error, the observer should
use a cathetometer to measure the falling rate of the acetone level instead of ruler. According to
Hasan (2022), a cathetometer is a device that can accurately and precisely measure minute
variations in the levels of liquid surface such as the distance between the levels of acetone in the
capillary tube. On top of that, to prevent random error or particularly called as parallax error, the
observer can take several measurements to obtain average value. By taking the average reading, it
will minimize the chances of error.

Besides, other possible errors that might happen include air bubbles that escaped into the
capillary tube when filling up the acetone. Hence, when filling the capillary tube with acetone, no
air bubble should be allowed to escape into the capillary tube in order to minimize the error that
might affect the accuracy of data collected. Other than that, during the experiment, it was found
that the cartridge heater fractured and covered in deposits of mineral. This will lead to an uneven
distribution of heat in the water bath and prevented the acetone from diffusing at a set temperature.
Therefore, in order to collect the data with high accuracy, a new cartridge heater should be installed
before conducting the experiment. Lastly, other possible errors that might occur is when the
acetone-filled capillary tube was frequently taken out in order to measure the height or level of
acetone filled (L) for every 15 minutes. As a result, the acetone will immediately be exposed to
the surrounding temperature, which could affect the rate of diffusion. To acquire accurate results,
it is necessary to limit the action of repeatedly removing the capillary tube using the appropriate
measuring equipment. At the end of experiment, this can reduce the error and provide a result with
more accurate data.

Page | 13
6.0 CONCLUSION

In conclusion, the experiment was done to determine the gaseous diffusion coefficient of
air-acetone mixture at the condition of atmospheric pressure and 55 °C (328 K) by the Winkelmann
evaporation tube method. This method, which is frequently used to determine a volatile liquid's
diffusivity, considers the volatile liquid's rate of evaporation, which is then followed by the rate of
descent of the liquid surface in a glass tube or diffusion cell (Coca et al., 1980). From this
experiment, the team members were able to apply the knowledge that has been learned in the Mass
Transfer Principles chapter of the Separation Process I course. Throughout the experiment, the
height of the acetone level in the capillary tube was measured using ruler for every 15 minutes
interval. Based on the findings, the gas diffusion coefficient or diffusivity of acetone in air using
Winkelmann method showed a large deviation from theoretical value, with a 1265.4321% percent
error. This deviation might be due to the certain errors made during conducting the experiment.
For example, parallax error can occur when determining the acetone level in the capillary tube.
Therefore, some precaution measures should be taken into consideration when conducting the
experiment in order to minimize the chances of error. To avoid parallax error, several
measurements should be taken to obtain the average value and use a cathetometer to measure the
falling rate of the acetone level instead of a ruler. To conclude, Winkelmann method is a reliable
approach to determine the gaseous diffusion coefficient of air-acetone mixture.

In short, all objectives of this experiment are successfully achieved and the theories in this
experiment have been proven appropriately.

Page | 14
7.0 REFERENCES

Atkins, P., de Paula, J., & Keeler, J. (2018). Physical Chemistry (11th ed.). Oxford University
Press.

Coca, J., Bueno, J. L., & Alvarez, R. (1980). Gaseous Diffusion Coefficients by the Stefan-
Winkelmann Method Using a Polymer-Solvent Mixture as Evaporation Source. Industrial
& Engineering Chemistry Fundamentals, 19(2), 219–221.
https://doi.org/10.1021/i160074a016

Geankoplis, C. J., Hersel, A. A., & Lepek, D. H. (2018). Transport Processes and Separation
Process Principles (5th ed.). Pearson Education.

Hasan, M. M. (2022, January 1). What is a Cathetometer? How does it Works? Engineers Dream.
https://www.engineers-dream.com/2022/01/what-is-cathetometer.html

Huey, J. (2017, March 30). Vapour diffusion coefficient of acetone in air KEK 150085 sin jia huey.
Academia.edu. Retrieved July 10, 2022, from
https://www.academia.edu/32148628/Vapour_Diffusion_Coefficient_of_Acetone_in_Air_
KEK_150085_Sin_Jia_Huey

Youney, M. Y., Al-haji, H., Mohammad Al-Bajhan, Ahmed Al-Saif, & Al-Abdulaziz, A. (n.d.).
ISSN: 2000-000X vol. 1 issue 10, December 2017, pages: 9-12 integration ... Integration a
Design of Experiment in the Mass Transfer Laboratory to Investigate the Effect of
Temperature Change on Diffusion Coefficient of Acetone in Air. Retrieved December 10,
2017, from http://ijeais.org/wp-content/uploads/2017/12/IJEAIS171202.pdf

Page | 15

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