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Experimental Procedure

Experiment A: Determining column pressure drop


1. All of the valves on the equipment were closed except valve V10 on the reflux pipe.
2. Then, the filter cap on the top of the reboiler was replaced and the power to the control
panel was turned on. The temperature selector switch was set to T9 which represents the
temperature in the reboiler. At the same time, valve V5 was opened, allowing the cooling
water to flow into the condenser at a flow rate on F11 of approximately 3 litres/min.
3. Next, the power on the control panel for the reboiler heating element was fully turned
anticlockwise and was switched on. Red light would illuminate indicating that the heating
element was on.
4. The power controller was turned until a reading of approximately 0.50 kW appears on the
digital wattmeter. The contents in the reboiler were warmed up and the temperature
readout meter was observed.
5. Valve V6 and V7 which connect base and top of the distillation column respectively to
the manometer was opened.
6. The boil up rate could be measured by operating valve V3, so that all the condensate was
diverted into a measuring cylinder and the time to collect a set quantity was observed.
7. Valve V3 was partially opened and the condensate was drained when taking a sample
from the reflux system until a steady flow was obtained. The liquid was ensured to
remain in the flexible connecting tube to prevent vapour from escaping.
8. The distillation process was allowed to run for 5 to 10 minutes. Right after that, the
sample collection was started and the timing was immediately set at the same time. A
sizeable amount was collected approximately 90 mL in 100 mL measuring cylinder. The
first non-representative collected amount was poured in a bottle labeled recyclable
MHC/toluene.
9. The readings of the pressure drops over both the rectifying (top) and the stripping
(bottom) sections were taken by opening the valves V6 and V7 on the manometer.

10. The experiment was repeated by increasing the power to 0.75 kW, 1.00 kW, 1.25 kW and
1.50 kW.
11. Graph of pressure drop versus boil up rate was plotted based on the result.
Experiment B: Determining the mixture compositions
1. The equipment was set up to determine the refractive index of pure methylcyclohexane,
MCH and pure toluene.
2. The small quantities of methylcyclohexane, MCH approximately 25 mol%, 50 mol% and
75 mol% were used up and the refractive index for each quantity was measured.
3. The volume of constituents (MCH and toluene) used could be calculated by using the
following formula:

For 25 mol% MCH and 75 mol% toluene,


Vol

Vol

( MCH )
( Toluene)
+(Vol Toluene )
MW MCH
MW Toluene

( MCH )(100)
( MCH)
MW MCH

25=

( MCH)

Results

Experiment
A: Determining column pressure drop
Given:
Power (kW)

Boil up rate
(L/hr)

0.50
0.75

3.60
10.80

Pressure drop
(mm

H2O
70
82

Degree of

Refractive index

foaming on trays
Gentle localized
Violent localized

1.43875
1.44357

1.00

14.72

130

Foaming gently

1.44442

1.25

22.34

145

over whole tray


Foaming

1.45484

violently over
1.50

33.51

whole tray
Liquid flooding

145

1.46090

in column

Experiment B: Determining mixture compositions


Concentration
25 %
50 %
75 %

Refractive Index
1.47536
1.46132
1.47996

Graph of pressure drop against boil up rate


200
150

Pressure drop mm HO

130

100

145

82

70

50

145

0
0

10

15

20

25

Boil up rate ( L/hr )

30

35

40

Calculations
Here are the calculations to determine the volume of constituents needed to fulfill the following
requirements:

For 25 mol% MCH and 75 mol% toluene,


Vol

Vol

( MCH )
( Toluene)
+(Vol Toluene )
MW MCH
MW Toluene

( MCH )(100)
( MCH)
MW MCH

25=

( MCH )

25=

100
Vol
MW MCH Toluene
1+ Toluene +
+
Vol MCH MW Toluene MCH

Vol Toluene
MW Toluene MCH
=3

Vol MCH
MW MCH Toluene
Vol Toluene
92.15 0.774
=3

Vol MCH
98.19 0.867
Vol Toluene
=2.513 4
Vol MCH
1Vol Toluene :2.5134 Vol MCH
Thus, for 100 mL of mixture, quantities required would be as follow since the total volume is
3.5134 mL,
Volume of toluene

Volume of MCH

3.5134 mL :100 m L

3.5134 mL :100 mL

1Vol Toluene : x Vol Toluene @ 100

2.5134 Vol MCH : x Vol MCH @100

mLmixture

100 mL
Volmol%
Toluene@MCH
100 = and 50 mol% toluene,
Forx50
3.5134 mL
mLmixture

mLmixture

x Vol MCH @100 =


mLmixture

( 100 mL ) ( 2.51 34 )
3.5134 mL

Vol

Vol

( MCH )
( Toluene)
+(Vol Toluene )
MW MCH
MW Toluene

( MCH )(100)
( MCH)
MW MCH

50=

( MCH )

50=

100
Vol Toluene MW MCH Toluene
1+
+
+
Vol MCH MW Toluene MCH

Vol Toluene
MW Toluene MCH
=1

Vol MCH
MW MCH Toluene
Vol Toluene
92.15 0.774
=1

Vol MCH
98.19 0.867
Vol Toluene
=0.8378
Vol MCH
1Vol Toluene :0.8378 Vol MCH
Thus, for 100 mL of mixture, quantities required would be as follow since the total volume is
1.8378 mL,
Volume of toluene

Volume of MCH

1.8378 mL:100 m L

1.8378 mL :100 mL

1Vol Toluene : x Vol Toluene @ 100

0.8378 Vol MCH : x Vol MCH @ 100

mLmixture

x Vol Toluene @ 100 =


mLmixture

100 mL
1.8378 mL

mLmixture

x Vol MCH @100 =


mLmixture

( 100 mL ) ( 0.8378 )
1.8378 mL

For 75 mol% MCH and 25 mol% toluene,


Vol

Vol

( MCH )
( Toluene)
+(Vol Toluene )
MW MCH
MW Toluene

( MCH )(100)
( MCH)
MW MCH

75=

( MCH )

75=

100
Vol
MW MCH Toluene
1+ Toluene +
+
Vol MCH MW Toluene MCH

Vol Toluene
MW Toluene MCH
=0.333

Vol MCH
MW MCH Toluene

Vol Toluene
92.15 0.774
=0.333

Vol MCH
98.19 0.867
Vol Toluene
=0.2790
Vol MCH
1Vol Toluene :0.2790 Vol MCH
Thus, for 100 mL of mixture, quantities required would be as follow since the total volume is
1.2790 mL,
Volume of toluene

Volume of MCH

1.2790 mL:100 m L

1.2790 mL :100 mL

1Vol Toluene : x Vol Toluene @ 100

0.2790 Vol MCH : x Vol MCH @ 100

mLmixture

x Vol Toluene @ 100 =


mLmixture

100 mL
1.2790 mL

mLmixture

x Vol MCH @100 =


mLmixture

( 100 mL ) ( 0.2790 )
1.2790 mL