No
Section
Page
1.0
Abstract
2.0
Objective
3.0
Introduction
4.0
Literature Review/Theory
5.0
Methodology
6.0
Results
7.0
Discussion
14
8.0
Conclusion
16
9.0
References
16
10.0
Appendix
17
ABSTRACT
Separation Laboratory 1 | 3 SKB
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1.0 OBJECTIVE
Separation Laboratory 1 | 3 SKB
Page 2
2.0 INTRODUCTION
Distillation is a separation method in which mixture components in a liquid mixture are
separated based on their relative volatilities. The distillation column provides an environment
where the liquid and vapour phases can approach equilibrium within a column. The existence in gas
phase is due to the vaporization process at the boiling point of the component. When the mixture is
heat up, the component that has higher volatility will evaporate first. Besides that, the components
that want to be separated via distillation should have different composition in vapor and liquid
where it is equilibrium at the boiling point of the liquid. In fact, most solutions used in distillation
process are highly volatile such as ammonia-water solution and ethanol-water solution. Separations
of components are easier to happen if the relative volatile mixture is high.
Separation is achieved by condensed vapor flowing as a liquid down the column theoretically
achieving equilibrium with the vapor flowing up the column. The distribution of components
differs in each phase and results in the separation. In the case of a binary mixture in batch
distillation under total reflux, the vapor condensing at the top of the distillation column will be rich
in one of the components. Liquid leaving the reboiler at the base of the column rich in the other
component. As the system reaches equilibrium the separation process reaches steady state for that
apparatus and set of operating conditions. This experiment is designed to study the distillation of a
binary mixture of Ethanol Water in a tray distillation column.
As other processes, there will be a few factors that affect the system such as temperature and
time that may affect the composition of the distillate. Therefore, the objective of this experiment is
to determine the effects of the operation time with the composition and distillation volume beside
to determine the relation between distillation volume and distillation composition. This experiment
was started with the preparation of 32 liter of ethanol-water mixture solution with composition of
ethanol (30%) and water (70%). The feed was allowed to be heated for a while. Ethanol which has
a higher volatility or a lower boiling point compared to water will evaporate first when heated. The
ethanol vapor will enter the bubble cap distillation column. Condenser will condense the ethanol
Separation Laboratory 1 | 3 SKB
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9. The distillate collected was measured. Sample composition was analyzed using refractometer to
get the refractive index.
10. Step 9 and 10 were repeated for every 5 minutes. The result was recorded as Table 4.1.
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5
79.0
78.3
76.0
10
78.9
79.3
76.0
15
79.1
79.0
76.0
20
78.8
78.9
76.0
25
78.7
78.8
76.0
30
78.9
79.0
76.0
35
78.8
78.8
76.0
40
78.8
79.4
76.0
45
78.7
78.8
76.0
50
78.7
78.8
76.0
55
78.6
78.7
76.0
60
78.6
78.7
76.0
79.5
78.5
79.4
79.4
79.3
79.4
79.3
79.3
79.2
79.2
79.0
79.2
79.2
79.2
80.1
79.5
78.8
79.0
78.9
78.9
78.8
79.0
78.8
78.8
79.0
79.0
79.0
79.0
79.0
79.0
79.0
79.0
79.0
79.0
79.0
79.5
75.0
76.0
76.0
76.0
77.0
77.0
77.0
77.0
77.0
77.0
77.0
77.0
76.0
76.0
77.0
77.0
78.0
78.0
78.0
79.0
79.0
79.0
79.0
79.0
76.0
77.0
77.0
77.0
78.0
78.0
79.0
79.0
79.0
79.0
79.0
79.0
78.0
78.0
79.0
79.0
79.0
80.0
80.0
80.0
80.0
80.0
80.0
80.0
TI 4
TI 5
24.0
24.5
24.5
25.0
26.0
26.0
28.5
27.0
27.0
27.5
28.0
28.0
TI 6
28.0
29.0
29.5
31.0
32.0
32.5
32.5
32.5
32.5
34.0
34.5
35.0
5.2
2.0
5.4
2.0
5.8
2.0
5.8
2.0
5.4
2.0
5.0
2.0
5.6
2.0
5.6
2.0
5.4
2.0
5.2
2.0
5.6
2.0
5.4
2.0
195
1.363
0
220
1.36
35
220
1.36
30
225
1.36
30
220
1.36
30
225
1.36
30
220
1.36
30
225
1.36
30
TI 1
TI 1A
TI 1B
TI 2
Temperature in plate
5.1
TI 2A
TI 2B
TI 2C
TI 2D
TI 2E
TI 2F
TI 3
Initial
temperat
u-re
Temperat
-ure of
cooling
water
RI 1A
RI 1B
Ratio of Reflux
Distillate volume
Reflux
Reflexion index
Voltage
Current
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225 225
1.36 1.36
30
30
24
170
230
180
1.36 1.363
30
0
10
15
18
20
Water (ml)
20
18
15
10
Mole of Ethanol
0.000
0.034
0.086
0.171
0.257
0.308
0.343
1.110
0.999
0.833
0.555
0.278
0.111
0.000
0.00
3.29
9.36
23.55
48.04
73.51
100.00
1.3350
1.3370
1.3410
1.3470
1.3525
1.3530
1.3600
Volume of
(mole)
Mole of Water
(mole)
% Mole of
Ethanol (%)
Refraction
Index
= 0.789
SG water = 1.000
For 2 ml of methanol and 18 ml of water:
Mole of ethanol
2 x 0.789
= 0.034 gmol
46.07
Mole of water
18 x 1.000
0.999 gmol
18.016
% mole of ethanol
0.034 x 100%
0.034 + 0.999
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3.29 %
20
40
60
80
100
120
% mole of ethanol
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Refraction Index
1.3630
1.3635
1.3630
1.3630
1.3630
1.3630
1.3630
1.3630
1.3630
1.3630
1.3630
1.3630
Volume of
(%)
Distillate (mL)
76.94
195
77.59
220
76.94
220
76.94
225
76.94
220
76.94
225
76.94
225
76.94
225
76.94
220
76.94
225
76.94
230
76.94
180
Table 4.2.2: The % mole of ethanol at different time
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Time (minutes)
5
10
15
20
25
30
35
40
45
50
55
60
10
20
30
40
50
60
70
time (minutes)
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100
50
0
0 10 20 30 40 50 60 70
time (minute)
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4. Dirty glass condition at refractometer may affect the value of refraction index.
5. There is probability that the volume of distillate may be lower than it really is as the result of
vaporization of ethanol to the surrounding. This happens when taking it out from the valve V4 i.e.
the ethanol temperature is greater than the surrounding temperature.
6. Unwanted particle in the column and instrument may affect the result of the experiment.
Precaution
Separation Laboratory 1 | 3 SKB
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