RESULTS

Calibration data
Calibration table for methanol-water
Volume of
Methanol(mL)
0
1
2
3
4
5
6
7
8
9
10

Volume of
Water(mL)
10
9
8
7
6
5
4
3
2
1
0

Mol fraction
0.0000
0.0470
0.0999
0.1598
0.2283
0.3074
0.3997
0.5087
0.6397
0.7998
1.0000

wt%

Refractive Index

0.00
8.07
16.49
25.29
34.50
44.13
54.23
64.83
75.96
87.67
100.00

1.3345
1.3369
1.3379
1.3414
1.3428
1.3437
1.3434
1.3425
1.3405
1.3363
1.3329

RI vs Composition Methanol-Water Mixture

RI

0.1

0.2

0.3

0.4

0.5

0.6

0.7

Composition (Mol Fraction)

0.8

0.9

1.1

Pressure

Vol
Methanol

Vol
Water

0.1
0.3
0.5
1
2
3
2
3
5

3
3
3
3
3
3
1
1
1

1 atm

Temperature (
)
Liquid
98.3
95.6
93.7
87.3
83.8
78.9
72.7
71.5
68.3

Vapour
91.5
88.4
87.1
82.8
78.1
77.2
74.9
72.3
70.2

Composition literature
Liquid
0.010
0.036
0.054
0.120
0.170
0.300
0.480
0.560
0.650

Vapour
0.025
0.370
0.420
0.530
0.610
0.670
0.790
0.830
0.880

RI

Liquid
1.3334
1.3338
1.3348
1.3382
1.3396
1.3402
1.3422
1.3403
1.3365

% Error
Liquid
50.0
72.2
72.2
33.3
30.6
54.3
-10.4
-12.9
-24.6

Vapour
40.0
69.2
58.3
17.0
-13.1
-13.4
-5.1
-10.8
-11.5

Vapour
1.3345
1.3397
1.3415
1.3429
1.3392
1.3375
1.3360
1.3342
1.3331

Composition
experiment
Liquid
0.005
0.010
0.015
0.080
0.118
0.137
0.530
0.632
0.810

Vapour
0.015
0.114
0.175
0.440
0.690
0.760
0.830
0.920
0.981

T-xy Diagram
95
85

Liquid

Temperature (C)

Vapour

75
65
0

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

Liquid/Vapour Mol Fraction

X-Y Equilibrium Diagram

Vapor mol fraction

1.1
1
0.9
0.8
0.7
0.6
0.5
0.4
0.3
0.2
0.1
0
0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

Liquid mol fraction

0.8

0.9

1.1

PROCEDURE
General start-up procedures
1. The equilibrium data for the binary system were obtained to studied from lecture.
2. A calibration curve of refractive index vs. composition plot was prepared for the particular
binary system.
3. The evaporator and condenser were checked to ensure it empty with liquid.
4. All the valves were ensuring initially closed and the heater power was switched off.
5. The main power at the control panel was switched on. All sensors and indicators were
checked to make sure it well functioning.

General Shut-Down Procedures

1. The heater was switched off.
2. The valve V10 was opened to allow cooling water flow rate through the condenser.
3. The valve V11 was opened to allow cooling water to flow through the cooling coil in the
evaporator.
4. When the unit has been pressurized, valve V8 was slowly opened to depressurize the unit.
5. Temperature was waited at the unit until it drops to below 50C.
6. Valves V2 and V3 opened to drain all liquid from the evaporator.
7. Valves V5 and V7 opened to drain all liquid accumulated at the condenser.
8. All valves were closed and the main power at the control panel was switched off.

Sampling Procedures
Both vapor and liquid samples can be taken from the unit for analysis.
1. Vapor sampling from the condenser.
i. The vent valve V6 was ensured opened and drain valve V7 was closed.
ii. Valve V5 was slowly opened to allow some condensed vapor from the condenser to flow
into the top sample collector. Valve V5 closed.
iii. Valve V7 was opened to collect the sample in a sampling vial.
iv. The cap on the vial was immediately closed and was immersed in cold water.

2. Liquid sampling from the evaporator

i. Vent valve V4 was ensure that it opened and drain valve V3 was closed.
ii. Valve V12 was opened to allow cooling water to flow through the bottom sample collector.
iii. Then, valve V2 was slowly opened to allow some liquid from the evaporator to flow into
the sample collector. Valve V2 closed.
iv. Valve V3 was opened to collect the sample in a sampling vial.
v. The cap on the vial was immediately closed and was immersed in the cold water.

Experiment 1: Equilibrium Curve at Atmospheric Pressure

Objective: To construct an equilibrium curve for the methanol-water system at atmospheric
pressure.
1. The general start-up procedures were performing.
2.12-L of pure methanol and 5-L of 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, V1
was closed.
5. Valves V13 and V14 were opened at the level sight tube. The liquid level was ensuring it
was above the safety line on the level sight tube.V13 and V14 were closed back.
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-01was set to about 100C.The heater was switched on.
8. The temperature rose in TIC-01 was observed. When the temperature at TI-02 starts to
increase sharply, the liquid in the evaporator has begun to boil. The pressure at PI-01 was
observed. Wait until temperatures and pressure stabilized at a steady state value.
9. The evaporator pressure and the liquid, vapor temperatures value were recorded.
10. A liquid and vapour sample were collected from the unit as described in section 6.4.The
samples were analyzed to determine their compositions.
11. The heater was switched off and valve V11 opened to allow cooling water to flow through
the cooling coil in the evaporator.
12. The temperature at TI-02 was waited to drop significantly to signify that boiling has
stopped. Valve V11 closed.
13. Additional 0.2-L methanol was poured into the evaporator through V1.Valve V1 closed.
There was now about 0.3-L methanol and 3-L water in the evaporator. Steps 5 to 12 were
above repeated.
14. An additional 0.2-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 0.5-L methanol and 3-L water in the evaporator .Steps 5 to
12 above were repeated.

15. An additional 0.5-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 1-L methanol and 3-L water in the evaporator .Steps 5 to 12
above were repeated.
16. An additional 1-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 2-L methanol and 3-L water in the evaporator .Steps 5 to 12
above were repeated.
17. An additional 1-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 3-L methanol and 3-L water in the evaporator .Steps 5 to 12
above were repeated.
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 V1.Valve V1 was
closed. Steps 5 to 12 above were repeated.
20. An additional 1-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 5-L methanol and 1-L water in the evaporator .Steps 5 to 12
above were repeated.
21. An additional 2-L methanol was poured into the evaporator through valve V1.Valve V1
was closed. There was now about 5-L methanol and 1-L water in the evaporator .Steps 5 to 12
above were repeated.
22. The general shut-down procedures were performed.

CALCULATION
Density of water = 1 g/ml
Density of methanol = 0.79 g/ml
Molecular weight of water = 18 g/mol
Molecular weight of methanol = 32.04 g/mol
Moles =

Density
X Volume
MW

Calculation for 1 ml of methanol and 9 ml of water

Moles methanol =

0.79 g /ml
x 1ml
32.04 g /mol

= 0.0247
Moles water =

1 g/ml
x 9 ml
18 g/mol

= 0.5000
Moles Fraction of Methanol =

Mole Methanol
Mole Methanol + Mole Water
0.0247
0.0247+0.500

= 0.0470
Calculation for 2 ml of methanol and 8 ml of water
Moles methanol =

0.79 g /ml
x 2 ml
32.04 g /mol

= 0.049
Moles water =

1 g/ml
x 8 ml
18 g/mol

= 0.444

Moles Fraction of Methanol =

Mole Methanol
Mole Methanol + Mole Water
0.049
0.049+ 0.444

= 0.0999

Calculation for 3 ml of methanol and 7 ml of water

Moles methanol =

0.79 g /ml
x 3 ml
32.04 g /mol

= 0.0739
Moles water =

1 g/ml
x 7 ml
18 g/mol

= 0.3889
Moles Fraction of Methanol =

Mole Methanol
Mole Methanol + Mole Water
0.07390
0.0739+ 0.3889

= 0.1598
Calculation for 4 ml of methanol and 6 ml of water
Moles methanol =

0.79 g /ml
x 4 ml
32.04 g /mol

= 0.0982
Moles water =

1 g/ml
x 6 ml
18 g/mol

= 0.3333
Moles Fraction of Methanol =

Mole Methanol
Mole Methanol + Mole Water
0.0982
0.0982+ 0.3333

= 0.2283

Calculation for 5 ml of methanol and 5 ml of water

Moles methanol =

0.79 g /ml
x 5 ml
32.04 g /mol

= 0.1233
Moles water =

1 g/ml
x 5 ml
18 g/mol

= 0.2777
Moles Fraction of Methanol =

Mole Methanol
Mole Methanol + Mole Water
0.1233
0.1233+ 0.2777

= 0.3074