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1.

0 ABSTRACT:
Gas diffusion occurred when diffusion of vapor takes place from volatile liquid
(organic solvent) into another gas (air). This process used same concept as mass transfer
where one constituent is transported from region of higher concentration to that of a lower
concentration. In this experiment, acetone is used as the organic solvent. The objective of the
experiment is to find out the gas diffusion coefficient, D of acetone in the air by using
Winklemanns method. This experiment is conducted at temperature of 50C and atmospheric
pressure. The level of acetone, L is determined every 10 minutes by using a microscope with
mounted sliding vernier scale alongside the thermostatic tank. Before the reading was taken,
the vertical height of the microscope was adjusted until it was visible that the meniscus of the
capillary tube was set at the origin. A horizontal glass tube is fixed to the upper end of
capillary tube and air is drawn through this by small air pump included within the unit. This
arrangement allows maintenance of partial pressure difference within capillary tube between
evaporating liquid surface and flowing air stream. With the level of acetone being
determined, a graph of t/L-L0 (ks/mm) against L-L0 (mm) is plotted and the gradient, s of the
experiment can be calculated by applying some mathematical derivation. Antoine equation is
used to determine the partial pressure of acetone. From the result value of diffusion
coefficient, D is calculated to be 1.3791 x 10-4 m2/s. Several errors are made in this
experiment which causes the value of diffusion coefficient to deviate which will be discussed.

2.0 INTRODUCTION
Gas diffusion occurred when diffusion of vapour takes place from volatile liquid
(organic solvent) into another gas (air). This process used same concept as mass transfer
where one constituent is transported from region of higher concentration to that of a lower
concentration. In this experiment, acetone is used as the organic solvent. Unit operation that
used during experiment is the Gas Diffusion Coefficient Apparatus (Model: BP 10).The
objective of experiment is to find out the gas diffusion coefficient, D of acetone in the air by
using Winkle mans method. This Gas and liquid molecular diffusion coefficients between
two or more species are measured to understand mass transfer phenomena occurring in a
system. An important consideration when determining molecular diffusion coefficients is to
minimize any form of disturbances on the surface of the system or along the diffusion paths.
The Arm field gas apparatus measures the height level of acetone using a vernier height
gauge as air travels on the surface, while the Arm field liquid apparatus measures
conductivity of dissolved 1 M, 0.1 M, and 0.01 M sodium chloride solution dissolved in
water versus time.
All gas diffusion methods are based on interfacing the donor stream containing the
analyse, with an acceptor stream containing a reagent. The porous hydrophobic membrane
serves as a barrier that allows only the gaseous species passed through. This makes the gas
diffusion methods very selective, since the non-volatile species will not reach the detector.
When two phases of different concentrations, originally at equilibrium with their
surroundings, are contacted, a concentration gradient is created and mass transfer starts until
a new equilibrium is reached. In case of no motion or convection, species move through the
interphase by diffusion from high to low concentration regions until new and homogeneous
solutions result.
One experimental method of measuring the gaseous diffusion coefficient, DAB, in
binary gas systems is by diffusion of vapour A from a volatile liquid into another gas B in an
arrangement of Stefan tube, as shown in Figure 1. The experimental method due to Winkle
Mann has the liquid contained in a narrow diameter vertical tube, maintained at a constant
temperature, and a gas stream is passed over the top of the tube to ensure that the partial
pressure of the vapor is transferred from the surface of the liquid to the air stream by
molecular diffusion. The volatile liquid A is conveniently selected from among organic
solvents, such as ethanol, methanol, or acetone, or water may also be studied.

Figure 2(a): Evaporation of acetone inside the capillary tube with air flow
The process is clearly an unsteady-state situation. The rate of evaporation and hence the
change in liquid level by time is so slow, however, approximation of a quasi-steady-state
process brings in negligible error and steady-state mass flux expressions can be utilized.
Steady-state diffusion of only one of the two species in binary mixtures of ideal gases
(diffusion of A through stagnant B) starts with the Ficks law.

3.0 OBJECTIVE
The experiment is conducted to determine the gas diffusion coefficient of acetone
using established Winkelmanns method. Then, to investigate the relationship between time
interval and the level of the acetone. Besides that, determine the mass transfer equation using
a Ficks Law with a bulk flow. Lastly, to calculate the diffusion coefficient.

4.0 THEORY
Diffusion is the motion of chemical species in a fluid mixture caused by random
molecular mixing process being the consequence of thermally induced agitation which finally
leads to complete homogenization of the mixture. The diffusivity coefficient

D AB

of pure

acetone in air is determined by using Winklemanns method. This method examines the
height changes of liquid acetone contained within a narrow vertical tube by using a Vernier
height gauge. Mass transfer take place in either a gas phase or a liquid phase or in both
simultaneously.
In order to understand the phenomena of mass transfer, it is important to have a clear
understanding of the basics described by Ficks first law. In this experiment more specifically,
the diffusion of acetone in air is analysed. Ficks first law shows how in a mixture of two
gases, both gases would move with respect to each other in opposite directions from their
high concentration areas to their lower concentration areas.

One experimental method of measuring the gaseous diffusion coefficient, DAB, in


binary gas systems is by diffusion of vapour A from a volatile liquid into another gas B in an
arrangement of Stefan tube. The experimental method has the liquid contained in a narrow
diameter vertical tube, maintained at a constant temperature, and a gas stream is passed over
the top of the tube to ensure that the partial pressure of the vapour is transferred from the
surface of the liquid to the air stream by molecular diffusion. The volatile liquid that had been
use and selected among organic solvent is acetone.
For this experiment however, air cant actually move physically past the layer of
liquid acetone. This is because air is soluble in liquid. So it is important for the reader to note
that the flux described in Ficks first law is actually with respect with an average velocity of
the mixture and not to a fixed point such as a coordinate in the T-shape tube where the liquid
acetone is being evaporated.
The process is clearly an unsteady-state situation. The rate of evaporation and hence
the change in liquid level by time is so slow, however, approximation of a quasi-steady-state
process brings in negligible error and steady-state mass flux expressions can be utilized.
Ficks first law stated that:

J =D AB

C
(eqn1)
x

Where,
J: Diffusion flux in x direction, kmole/m2.sec
C: Concentration, kmole/m3
X: Distance through which diffusion occurs, m
D AB : Diffusion coefficient (diffusivity), m2/s
And becomes
N A ( 1 y A )=D AB

dCA
P d yA
= D AB T
(eqn 2)
dx
RT dx

Where,
N A = Molar diffusion flux, kmole/m2.s
y A = Mole fraction of species A, dimensionless
PT = Total pressure, Pa
R = Gas constant, m3.Pa/kmole.K
T = Temperature of the environment, K

This equation can be integrated over x for the diffusion distance L, and after changing mole
fractions to partial pressures and rearranging, to give

D AB
N A=

PT
( P A 1 P A 2 )
RTL
(eqn 3)
PBM

Where,
P A 1P A 2 = P A

= Partial pressure difference of A, Pa

PBM = Logarithmic mean of the partial pressures pB1, pB2, of B, Pa


The rate of mass transfer due to evaporation by time can be written as

( LM ) dxdt (eqn 4 )

N A=

Where,
L = Liquid density of A, kg/m3
M = Molecular weight of A
The approximation of quasi steady-state operation allows to equate the equations 3 and 4,
where for simplicity the variable distance x is changed to L

D AB
N A=

PT
( P A 1 P A 2 )
RTL
L dL
=
(eqn5)
PBM
M dt

( )

Integration from time t=0 to t=t for L=L0 to L=L yields,

t=

RT PBM L
2
2
L L0 ) ( eqn 6 )
(
2 D AB PT M P A

The change in diffusion distance is very small to measure correctly unless too long times are
allowed. It is however possible to rearrange the Equation 5 into a linear form of the type
Y = AX +B

Where,

Y = t / ( LL0 )

A=

RT P BM L
2 D AB PT M P A

X=

LL
0

RT P BM L

(
B = 2 D AB PT M P A ) L0

5.0 APPARATUS
1. TR 14 membrane test unit apparatus
2. 500 mL beakers
3. Electronic balance
4. Gloves
5. Ruler
6. Acetone
7. Sodium chloride
8. Water

Figure 5(a): The set up apparatus of gas diffusion unit.

6.0 PROCEDURE
1

The capillary tube is partially filled with acetone to a depth of approximation


33.03mm. The top nuts was removed from metal fitting.

Carefully, capillary tube was inserted through the rubber ring inside the metal nut until
the top of the tubes rest on the top of the nuts.

Gently the assembly is screwed onto the top plate with the T piece normal to the
microscope. The flexible air was connected to the end of the T piece. The object lens is
adjusted to within 20-32mm from the tank.

The vertical height of microscope was adjusted until the capillary tube is visible. When
the meniscus has been determined, the Vernier scale should be aligned with a suitable
graduation on the fixed scale.

Then, the air pump was switched on.

The level inside the capillary tube was recorded.

The temperature controlled water bath was switched on and a steady temperature was
obtained.

The reading was taken every 5 minutes to 10 times. The experiment was done at the
temperature 45oc and repeater the step by using temperature 45 and repeat step by
using temperature at 55oc and initial length acetone 38.04.

7.0 RESULTS
Initial length, Lo = 33.03 mm
Temperature = 50 oC

t/((L-LO)) Vs (L-LO)
3
2.5
2

t/((L-LO)) (ks/mm)

1.5

f(x) = 1.63x - 0.24


R = 0.9

t/((L-LO)) (ks/mm)
Linear ( t/((L-LO)) (ks/mm))

1
0.5
0
0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

LIQUID LEVEL (L-LO) (mm)

TIME (ks)
0.000
0.600
1.200
1.800
2.400
3.000
3.600

READING OF

LIQUID LEVEL (L-

VERNIER (mm)
33.03
33.83
34.88
36.06
37.26
38.63
40.08

LO) (mm)
0.00
0.80
1.05
1.18
1.26
1.37
1.45

Density of acetone, = 790 kg/m3

Gas constant, R =8.314 J/mol.K

Molecular weight of acetone = 58.08 kg/mol

Vapor pressure, Pv =56 kN/m3

Slope, s= 1.6288 ks/mm2 = 1.6288 x 106 s/m2

Density of acetone, = 790 kg/m3


Gas constant, R =8.314 J/mol.K
Molecular weight of acetone = 58.08 kg/mol
Vapor pressure, Pv =56 kN/m3
Slope, s= 1.6288 ks/mm2 = 1.6288 x 106 s/m2

t
( LLO )
0.00
0.75
1.14
1.53
1.90
2.19
2.40

(ks/mm)

8.0 CALCULATION

Assume standard conditions ( P=101.32kN/m2 , V= 22.4 m3, T=273 K)

Temperature, Ta =50 oC = 323 K

To find CT:
CT = (1/V)(T/Ta)
= (1/22.4)(273/323)
= 0.0377 kmol/m3

To find CB1:
CB1 = CT= 0.0377 kmol/m3

To find CB2:
CB2 = (Pa-Pv/Pa)CT
= (101.32-56/101.32)(0.0377)
= 0.0169 kmol/m3

To find CBM:
CBM = (CB1-CB2)/In(CB1/CB2)
= (0.0377-0.0169)/In(0.0377/0.0169)
= 0.0259

To find Ca:
Ca = (Pv/Pa)CT
= (56/101.32)(0.0377)
= 0.0208 kmol/m3

To find diffusivity, D :
D = (L x CBM)/(Ca x CT x 2sM)
D = (790 x 0.0259)/(0.0208 x 0.0377 x 2(1.6288 x 106)(58.08))
D = 1.3791 x 10-4 m2/s

9.0 DISCUSSION:
This experiment was conducted to obtain the gas diffusion coefficient of acetone
using the Winkelmanns method. In this experiment, the volatile liquid is heated until it
evaporated into free air stream. The rate of diffusion can be observed by the rate of
decreasing of acetone level in the tube by using a telescope. Diffusion is the movement of
molecules from area of high concentration to area of lower concentration and this is increased
with increasing temperature which means when the temperature increase the diffusion will
also rising up. In the other word, when temperature is higher, then the rate of diffusion would
probably increase caused by increasing kinetic activity of the solution.
Based on the result, the level of acetone was decreased when the time was increased
caused by diffusion. Diffusion is process where involving the movement of component or
molecules from one location to another location due to exist of concentration gradient.
Normally, the movement of molecule is from high concentration part to more less
concentration gradient.
In the experiment, the diffusion concept can be observed by the decreasing of acetone
level in the capillary tube. The boiling process of water generated heat and the heat was
transferred to the acetone. This process was increased the movement of molecules in the
acetone until it creates body that has high concentration compare to surrounding.
Furthermore, due to some driving forces and existing of concentration gradient, the molecule
was move from inside the capillary tube to the surrounding air that has less concentration.
Based on the graph that has been plotted, the x-axis of the graph is the differences
between final level of acetone and the initial level of acetone. Meanwhile, the y-axis of the
graph is the time taken divide by the difference between the levels of acetone. In addition, the
trend of the graph is increased proportionally. The increasing the difference between the
levels of acetone, the increasing the time divide by the difference between the levels of the
acetone. From the calculation and the data from the table, the value of diffusivity was
determined which is 1.3791 x 10-4 m2/s.
Moreover, the temperature controller was set up at 50C through along the experiment
and it not been set beyond 70C. It is because the boiling point of the acetone is at 56C
where the process where the phase of acetone change from liquid to vapor. When the
temperature exceeds 70C, the rate of evaporation is faster compare to temperature at the
boiling point. This situation can cause the problem to the experimenter to collect the data or

difference of acetone level. Finally, the discrepancy from the experimental data is the value of
the time divide by difference between levels of acetone between intervals is not increased
constantly due to some errors such as parallax error and the initial value of the acetone in the
capillary tube was not read accurately.

10.0 CONCLUSION
As the conclusion, the result for diffusivity coefficient at 50 C is 1.3791 x 10 -4 m2/s.
Based on the result, the level of acetone decreased as the time increased caused by diffusion.
From the graph plotted, it can be also conclude that the flowing air significantly increases the
diffusion coefficient thus increasing the mass transfer. During the experiment, there are some
errors occur. To get accurate values of diffusivity, a few of recommendations step should be
taken.

11.0 RECOMMENDATION
There are some recommendations for future used firstly, every experimenter must
make sure to avoid parallax error while taken the readings of level of acetone from the
Vernier scale because it will deviate the data and results calculated at the end of experiment.
Secondly, the amount of acetone used should be pipette and closed from surrounding before it
is drop into the capillary tube so that it will not alter the accuracy of the results. Other than
that, at the time interval where the readings of acetone is being recorded, experimenter must
use the cap provided instead of fingers to close the end of capillary tube and the flexible
tubing. For future experiments, some form of air flow regulation should be investigated.
Something as simple as a room fan could be placed next to the scale to ensure a more
constant air flow.

Another increase in accuracy could be achieved by regulating the

temperature with more consistency. If the experiment could be performed in a large insulated
room, the temperature may not vary as much.

12.0 REFERENCES / APPENDICES


1. Yu. I. Zhavrin, N. D. Kosov, S. M. Belov and S. B. Tarasov, (1984) Effect of
pressure on Diffusion Stability in Some Three-Component Gas Mixtures, Zhurnal
Tekhnicheskoi Fiziziki.
2. J. O. Hirschfelder, Ch. F. Curtiss and R. Bird (1954) Molecular Theory of Gases and
Liquids, John Willey & Sons, Inc., New York.
3. Sherwood, T.K., Pigford, R.L., Wilke, C.R,(1975) Mass Transfer, McGraw Hill
Kogakusha.
4. Bird, R.B., Stewart, W.E., Lightfoot, E.N., (2007) Transport Phenomena, Wiley,
2nd Edition.
5. Ulrich Kunz and Thomas Turek. (2009). Beilstein Journal of Organic Chemistry. Flow
through reactors for organic chemistry directly electrically heated tubular mini
reactors as an enabling technology for organic synthesis. Germany.
6. Fogler, H. S., Elements of Chemical Reaction Engineering, 2nd edition, Chapter 10.
Prentice Hall, 1992, New Jersey.
7. Perry, R. H., D. Green, Perrys Chemical Engineers Handbook, 6th edition,
McGraw-Hill, 1988.
8. Seager, S. L., Geertson, L. R., & Giddings, J. C. (1963). Temperature Dependence of
Gas and Vapor Diffusion Coefficients. Journal of Chemical & Engineering Data J.
Chem. Eng. Data, 8(2), 168-169. Retrieved March 25, 2016.
9. Katsanos, N., & Karaiskakis, G. (1983). Temperature variation of gas diffusion
coefficients measured by the reversed-flow sampling technique. Journal of
Chromatography A, 254, 15-25.
10. Christie John Geankoplis (University of Minnesota), Transport Processes and
Separation Process Principles (Includes Unit Operations) fourth edition, Pearson
Education International.
11. The Kinetic Theory of Gases, Leonard B. Loeb, (2004)
12. Diffusion and Mass Transfer, James S. Vrentas, Christine M. Vrentas, (2013)
13. The Properties of Gases and Liquids, Bruce Poling, John Prausnitz, John O Connell,
(2000)
14. Diffusion: Mass Transfer in Fluid Systems, E. L Cussler, (2009)

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