1.

APPARATUS AND MATERIALS

1) Methanol.
2) Distilled water.
3) SOLTEQ Vapour Liquid Equilibrium Unit.
4) Refractometer.
5) Sample collectors.
6) Dropper.
7) 500mL, 1000 mL and 2000 mL beakers.
8) 50 mL and 500 mL measuring cylinders.

2. PROCEDURE
6.1 General start up procedures.
1. A calibration curve of refractive index vs. composition plot for the binary system was
prepared.
2. The evaporator and condenser were checked to make sure the units are empty of liquid.
3. All valves were initially closed and the heater power switch was turned off.
4. The main power on the control panel was switched on. All sensors and indicators were
checked to ensure functioning properly.
6.2 General experiment procedures.
1. The general start-up as described was performed.
2. About 12-L methanol and 5-L deionized water were prepared.
3. Valve V8 was opened.
4. 0.1-L methanol and 3-L water were poured into the evaporator through valve V1.Then,
valve V1 was closed.
5. Valves V13 and valve V14 were opened at the level sight tube. It was ensured that the
liquid level was above the safety line on the level sight tube. Then, valves V13 and V14 were
closed.
6. Valve V10 was opened and adjusted to allow about 5 L/min of cooling water to flow
through the condenser.
7. The temperature controller TIC-01 was set to about 100C.The heater was switched on.
8. The temperature rise in TIC-01 was observed. The liquid in the evaporator had started to
boil when the temperature at TIC-02 started to increase sharply. The pressure at P1-01 was
observed. All temperatures and pressure were let to stabilize at a steady state value.
9. The evaporator pressure and liquid and vapour temperatures were recorded.

10. Liquid and vapour sample were collected from the unit according to the sampling
procedure. The samples were analysed to determine their compositions.
11. The heater was switched off and valve V11 was opened to allow cooling water to flow
through the cooling coil in the evaporator.
12. The temperature at T1-02 was let to drop significantly to signify that the boiling had
stopped. Valve V11 was closed.
13. An additional 0.2-L methanol was poured into the evaporator through valve V1.Then,
valve V1 was closed. There was about 0.3-L methanol and 3-L water in the evaporator. Steps
5 to 12 above were repeated.
14. An additional 0.2-L methanol was poured again into the evaporator through valve
V1.Then valve V1 was closed. There was about 0.5-L methanol and 3-L water in the
evaporator. Steps 5 to 12 were repeated again.
15. An additional 0.5-L methanol was poured into the evaporator through valve V1.Then
valve V1 was closed. There was about 1-L methanol and 3-L water in the evaporator. Steps 5
to 12 were repeated again.
16. An additional 1-L methanol was poured into the evaporator through valve V1.Then valve
V1 was closed. There was about 2-L methanol and 3-L water in the evaporator. Steps 5 to 12
were repeated again.
17. An additional 1-L methanol was poured into the evaporator through valve V1.Then valve
V1 was closed. There was about 3-L methanol and 3-L water in the evaporator. Steps 5 to 12
were repeated again.
18. Valve V2 and V3 were opened to drain all liquid from the evaporator.
19. 2-L methanol and 1-L water were poured into the evaporator through valve V1.Then
valve V1 was closed. Steps 5 to 12 were repeated.
20. An additional 1-L methanol was poured into the evaporator through valve V1.Then valve
V1 was closed. There was about 3-L methanol and 1-L water in the evaporator. Steps 5 to 12
were repeated.

21. An additional 2-L methanol was poured into the evaporator through valve V1.Then valve
V1 was closed. There was about 5-L methanol and 5-L water in the evaporator. Steps 5 to 12
were repeated.
22. The general shut-down procedures were performed.
6.3 General shut-down procedures.
1. The heater was switched off.
2. Valve V10 was opened to increase cooling water flow rate through the condenser.
3. Valve V11 was opened to allow cooling water to flow through the cooling coil in the
evaporator.
4. Valve V8 was opened slowly to depressurize the unit.
5. Wait for the temperature of the unit to drop below 50C.
6. Valves V2 and V3 were opened to drain all liquid from the evaporator.
7. Valves V5 and V7 were opened to drain all liquid accumulated at the condenser.
8. All valves were closed and the main power of the control panel was switched off.

3.RESULTS
a) Vapour liquid equilibrium Table
Pressure

Vol of

Vol of

temperature

RI

(bar)

Methanol(L)

Water(L)

liquid

vapour

liquid

vapour

0.1

95.9

68.6

1.33342

1.34014

0.3

92.3

71.7

1.33409

1.33947

0.5

89.9

84.0

1.33494

1.34223

1.0

84.8

80.4

1.33706

1.34238

2.0

79.1

73.5

1.33913

1.34140

3.0

76.5

74.2

1.34209

1.33893

2.0

72.2

71.3

1.33891

1.34090

3.0

70.5

70.0

1.34233

1.33683

5.0

68.4

68.1

1.34050

1.33670

Graph of RI vs Mol Fraction

1.344

Refractive Index

1.342
1.34
1.338
1.336
1.334
1.332
0

0.2

0.4

0.6
Mol Fraction

0.8

1.2

b) Calibration Table
Water
(ml)

Methanol
(ml)

Mol
Water

Mol
Methanol

Mol
Total

Methanol
Mol
Fraction

Methanol
wt%

Refractive
Index

10

0.556

0.556

1.33300

0.444

0.0494

0.4934

0.1001

16.49

1.33692

0.333

0.0986

0.4316

0.2285

34.50

1.34167

0.222

0.1481

0.3701

0.4002

54.23

1.34226

0.111

0.1975

0.3085

0.6409

75.96

1.33660

10

0.2466

0.2466

1.0000

100.00

1.33299

X-Y Equilibrium Diagram

VAPOR MOL FRACTION (X)

0.03
0.025
0.02
0.015
0.01
0.005
0
0

0.005

0.01

0.015

0.02

LIQUID MOL FRACTION (Y)

0.025

0.03

0.035

T- xy Graph of Methanol-Water System

120

Temperature (C)

100
80
60
40
20
0
0

0.005

0.01

0.015

0.02

Vapor/Liquid mol fraction

Vapor
Liquid

0.025

0.03

0.035

4. CALCULATIONS
8.1 Example calculation of methanol mol fraction from calibration table.

Water

: 4mL

Methanol : 6mL

Mole of water :

Mole of methanol :

Therefore,

0.4002
*Note that the vapor pressure of methanol is 97.658 mmHg.

From Antoines Law: PA

From Raolts Law: PA

. P A

where x (vapours mol fraction)

can be

Written as y (liquid mol fraction)

Therefore,

Antoines Constant:

Temperature
(C)

Reference

5.20409

1581.341

-33.50

Ambrose and
Sprake, 1970

15.1-103.83

8.2 Calculation of methanol mol fraction in vapour state.

When T = 68.6C (341.6 K)

0.0121

When T = 71.7C (344.7 K)

0.0135

When T = 84.0C (357.0 K)

0.0212

When T = 80.4.0C (353.4 K)

0.0187

When T = 73.5C (346.5 K)

0.0145

When T = 74.2C (347.2K)

0.0149

When T = 71.3C (344.3 K)

0.0134

When T = 70C (343 K)

0.0127

When T = 68.1C (341.1 K)

0.0119

8.3 Calculation of methanol mol fraction in liquid state.

When T = 95.9C (368.9 K)

0.0316

When T = 92.3C (365.3 K)

0.0286

When T = 89.9C (362.9 K)

0.0259

When T = 84.8C (357.8K)

0.0218

When T = 79.1C (352.1 K)

0.0178
When T = 76.5C (349.5 K)

0.0162

When T = 72.2C (345.2K)

0.0166

When T = 70.5C (343.5 K)

0.013

When T = 68.4C (341.4K)

0.012