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EXPERIMENT # 09

OBJECT:
To study the effect of temperature on the vapor diffusion of a volatile liquid in air using
Winklemann Method.
APPARATUS:
1. Edibon, QDTG (Gaseous Mass Transfer and Diffusion Coefficient) Unit
2. Beaker, 250 ml
3. Measuring Cylinder, 25 ml

Fig.#1: Edibon, QDTG (Gaseous Mass Transfer and Diffusion Coefficient) Unit

Fig.#2: Process Diagram and Unit Elements Allocation

PARTS OF EQUIPMENT:
1. Air pump with air regulator. Range: 0-7 l/min.
2. Travelling optic system with accurate focus adjustment and mounted for vertical axis movement
against a Vernier scale (Vernier
3. range: 0-300 mm).
4. A thermostatically controlled water transparent - sided Bath. Capacity: 36 litres.
5. Heating resistance: 500 W. (Max. temperature 60ºC).
6. 2 Temperature sensors, “J” type.
7. Level switch.

CHEMICALS:
1. Acetone (>99%, ACS Reagent)

EQUIPMENT DESCRIPTION:
The QDTG is a teaching unit that allows to students familiarize with the notions of mass transfer
theory, specifically about the diffusion of a volatile liquid into an inert gas, obtaining experimental
data and results which are very useful for a correct practice understanding of the process and,
consequently, for the technical teaching of the students.
The experimental determination of the diffusion coefficient, DAB for a binary mixture, can be done
with a device such as a test tube with such dimensions that the effects in the limits of the system can
be ignored. Suppose, thus, that a pure liquid A evaporates slowly and constantly inside it, and that its
vapours are diffused through an inert and quiet gas B. During the experiment, temperature and
pressure will be constant. On the other hand, it will only be considered diffusion in the direction of
'z' axis.
These assumptions are obtained if a glass capillary tube is used instead of a test tube. This capillary
tube will have a volatile solvent (pure liquid A) and a gas (air, in this case) which will flow
horizontally in laminar regime.
In order to vary the temperature of the volatile solvent there is a thermostatic bath, which will
operate by the method colloquially called “bainmarie”.
The experiment will consist on measuring the heights difference in a time interval using a calibrated
device that allows measuring distances.

THEORY:
For the determination of diffusivity of acetone (or a similar Volatile material) in air, the volatile
liquid will be contained in a capillary tube.
The capillary tube will be contained in a test tube immersed in a constant temperature, water bath. A
stream of air, at the same water bath temperature, will pass over the end of the capillary tube in an
attempt to reduce the concentration of volatile material, at that point to zero. The experimental
procedure is to measure the rate of drop of the liquid level in the capillary with time.
The units in the International System for the diffusivity are m2/sec but often expressed in cm2/sec.
The experiment consists in measuring the height difference of the liquid in the measuring cylinder, z,
regarding the time t. To be able to determine the diffusivity, the equation of straight line will be
deduced from which DAB can be calculated.
The experiment to determine the diffusivity of gaseous is based on the Winkelmann’s method. In
this method, the volatile liquid is allowed to evaporate in a vertical glass tube over the top of which a
stream of vapour-free gas is passed. A water bath is provided for maintaining a steady temperature
so that there is no eddy current in the vertical tube and mass transfer takes place from the surface by
molecular diffusion alone. By monitoring the evaporation rate, which is the rate of fall of liquid
surface, and with the knowledge of concentration gradient, the diffusivity can be calculated

The rate of mass transfer is given by:

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 C  C 
N A  D A  T  (1)
 L  C Bm 

Where, D = diffusivity [m2/s]


CA = saturation concentration at interface [kmol/m3]
L = effective distance of mass transfer [m]
CT = total molar concentration [kmol/m3]
CBm = logarithmic mean value of CB [kmol/m3]

Considering the evaporation of the liquid:

  dL
NA   L  (2)
M  dt

Where, ρL = density of liquid [kg/m3]


M = molecular weight [kg/kmol]

From Equation (1) and (2), the diffusivity of acetone, D can be calculated as:

 L C Bm
D
2MC ACT s

t
Where, s is the slope of the plot against ( L  Lo )
L  Lo

  L CBm 
s   
 2MDC ACT 

PROCEDURE:
 Fill the water bath with distilled water until the float switch is dipped.
 Fill up the tube with the highest mark with acetone. Take note of the acetone height.
 Set the temperature to plus 5 oC of the room temperature.
 Start the experiment and note the decrease in height of acetone after every 5 minutes, till
forty minutes.
 Repeat the above steps for three more increment of 5 oC.

OBSERVATIONS:
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Room Temperature + 5 = 34 oC
S. TIME LEVEL LEVEL t/(zₒ-z)
No (t) DIFFERENCE
minutes z (mm) zₒ-z (mm) sec/mm
1 0 84 ----- -----
2 1 80 4 15
3 2 78 6 20
4 3 76 8 22.5
5 4 74 10 24
6 5 72 12 25
7 6 70 14 25.71
8 7 68 16 26.25
9 8 66 18 26.7
10 9 66 18 30
11 10 64 20 30
12 15 60 24 37.5
13 20 56 28 42.9
14 25 52 32 46.875
15 30 50 34 52.94
16 35 48 36 58.33
17 40 46 38 63.2

70

60
y = 1.2823x + 8.6961
50
t/(Zo - Z) sec/mm

40

30

20

10

0
0 5 10 15 20 25 30 35 40
Zo - Z (mm)

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Room Temperature + 10 = 39 oC
S. TIME LEVEL LEVEL t/(zₒ-z)
No (t) DIFFERENCE
minutes z (mm) zₒ-z (mm) sec/mm
1 0 84 ----- -----
2 1 80 4 15
3 2 78 6 20
4 3 76 8 22.5
5 4 74 10 24
6 5 72 12 25
7 6 70 14 25.71
8 7 68 16 26.25
9 8 66 18 26.7
10 9 64 20 27
11 10 64 20 30
12 15 56 28 32.143
13 20 50 32 37.5
14 25 46 36 41.7
15 30 44 38 47.4
16 35 42 40 52.5
17 40 40 42 57.143

70

60

50 y = 0.9079x + 12.389
t/(Zo -Z) sec/mm

40

30

20

10

0
0 5 10 15 20 25 30 35 40 45
Zo - Z (mm)

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Room Temperature + 15 = 44 oC
S. TIME LEVEL LEVEL t/(zₒ-z)
No (t) DIFFERENCE
minutes z (mm) zₒ-z (mm) sec/mm
1 0 84 ----- -----
2 1 80 4 15
3 2 76 8 15
4 3 72 12 15
5 4 70 14 17.143
6 5 68 16 18.75
7 6 66 18 20
8 7 62 22 19.09
9 8 60 24 20
10 9 60 24 22.5
11 10 58 26 23.08
12 15 52 32 28.125
13 20 46 38 31.6
14 25 44 40 37.5
15 30 38 46 39.13
16 35 36 48 43.75
17 40 34 50 48

60

50
y=x

40
t/(Zo - Z)sec/mm

30

20

10

0
0 10 20 30 40 50 60
Zo - Z (mm)

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CALCULATIONS :
Diffusivity of acetone ‘D’ can be calculated as :
𝜌𝐿 𝐶𝐵𝑀
𝐷=
2𝑀𝐶𝐴 𝐶𝑇 𝑆
For total Molar concenteration ‘𝐶𝑇 ′ :
1 𝑇𝑎𝑏𝑠
𝐶𝑇 = ×
22.4 𝑇𝑜
At 307K,
1 273
𝐶𝑇 = 22.4 × 307
𝑘𝑚𝑜𝑙
𝐶𝑇 = 0.0397
𝑚3
At 312K,
1 273
𝐶𝑇 = ×
22.4 312
𝑘𝑚𝑜𝑙
𝐶𝑇 = 0.039 𝑚3
At 317K,
1 273
𝐶𝑇 = 22.4 × 317
𝑘𝑚𝑜𝑙
𝐶𝑇 = 0.03845
𝑚3

Saturation concenteration at interface :


𝑃𝑉
𝐶𝐴 = × 𝐶𝑇
𝑃𝑇
By using Antonie equation ,
𝐵
ln𝑃∗ = 𝐴 − 𝑇+𝐶
At 307K
2940.46
ln𝑃∗ = 16.6513 − 307−35.93
𝑃𝑉 = 331.522 𝑚𝑚𝐻𝑔
Then ,
331.522
𝐶𝐴 = × 0.0415
760
𝐶𝐴 = 0.018𝑘𝑚𝑜𝑙/𝑚3
At 312K,
2940.46
ln𝑃∗ = 16.6513 − 312−35.93
𝑃𝑉 = 403.5 𝑚𝑚𝐻𝑔
Then ,
403.5
𝐶𝐴 = × 0.0415
760
𝐶𝐴 = 0.022𝑘𝑚𝑜𝑙/𝑚3
At 317K,

2940.46
ln𝑃∗ = 16.6513 − 317−35.93
𝑃𝑉 = 487.7 𝑚𝑚𝐻𝑔
Then ,
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487.7
𝐶𝐴 = × 0.0415
760
𝐶𝐴 = 0.027𝑘𝑚𝑜𝑙/𝑚3

Log mean concenteration :


𝐶𝐵1 − 𝐶𝐵2
𝐶𝐵𝑀 =
𝐶
𝑙𝑛 𝐶𝐵2
𝐵1
For 𝐶𝐵1 :
𝑃𝑇 − 𝑃𝑉
𝐶𝐵1 = × 𝐶𝑇
𝑃𝑇
At 307K,
760 − 331.522
𝐶𝐵1 = × 0.0415
760
𝐶𝐵1 = 0.0234 𝑘𝑚𝑜𝑙/𝑚3
Since ,
𝐶𝐵2 = 𝐶𝑇
Now ,
0.0415 − 0.0234
𝐶𝐵𝑀 =
0.0415
𝑙𝑛 0.0234
𝐶𝐵𝑀 = 0.0316 𝑘𝑚𝑜𝑙/𝑚3

At 312K,
760 − 403.5
𝐶𝐵1 = × 0.0415
760
𝐶𝐵1 = 0.0195 𝑘𝑚𝑜𝑙/𝑚3

0.0415 − 0.0195
𝐶𝐵𝑀 =
0.0415
𝑙𝑛
0.0195
𝐶𝐵𝑀 = 0.029 𝑘𝑚𝑜𝑙/𝑚3

At 317K,
760 − 487.7
𝐶𝐵1 = × 0.0415
760
𝐶𝐵1 = 0.015 𝑘𝑚𝑜𝑙/𝑚3

0.0415 − 0.015
𝐶𝐵𝑀 =
0.0415
𝑙𝑛
0.015
𝐶𝐵𝑀 = 0.026 𝑘𝑚𝑜𝑙/𝑚3

Finally ,
At 307 K,
784.6×0.0316
D=
2×58.08×0.018×0.0397×1.2823×106
𝑫 = 𝟐. 𝟑𝟑 × 𝟏𝟎−𝟒 𝒎𝟐 /𝒔𝒆𝒄

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At 312 K,
784.6×0.029
D=
2×58.08×0.022×0.039×0.9079×106
𝑫 = 𝟐. 𝟓𝟏𝟓 × 𝟏𝟎−𝟒 𝒎𝟐 /𝒔𝒆𝒄
At 317 K,
784.6×0.026
D=
2×58.08×0.027×0.03845×1×106
𝑫 = 𝟏. 𝟕 × 𝟏𝟎−𝟒 𝒎𝟐 /𝒔𝒆𝒄

RESULT AND DISCUSSION:


Discuss all your results. The questions below only serve as a guideline. Your discussion should not
only be limited to these questions.
t
1. Plot against ( L  Lo ) . Determine gas diffusivity, from the obtained slope, s.
L  Lo

2. Discuss the factors that affect the diffusion of acetone from the graph that have been plotted.

3. What will be the diffusivity if you increase the heating temperature? Explain.

4. Plot a graph showing the effect of temperature on diffusivity.

5. Based on objective of the experiment and the theory in gas diffusion makes a conclusion from your
finding.

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