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TABLE OF CONTENTS
CONTENT PAGE
Abstract / summary 2
Introduction 3
Aims / objectives 4
Theory 5-8
Apparatus 9-11
Experimental procedure 12-16
Result 17-19
Sample calculation 20-26
Discussion 27-28
Conclusion 29
References 30
Recommendation 31
Appendix 32-34
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1.0 ABSTRACT:
Vapor-Liquid Equilibrium (VLE) unit can be used to study about the binary system. The main
purpose of this experiment is to determine the composition of methanol in the vapor phase and liquid
phase. In this experiment, a mixture of methanol and water is initially fed into the evaporator. The
quantity of methanol is added until the volume of methanol added is equal to the volume of water which
is 3.0 litres. The mixture was heated until boiled. The mixture vapor will rise up and will be cooled down
by the condenser at the top of the evaporator. As the vapor starts to condense, the liquid falls back into
the evaporator. When temperature remains constant, the system will stabilize and reached an equilibrium
state. Finally, the samples of vapor and liquid were taken to determine their compositions by using a
digital refractometer.
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2.0 INTRODUCTION:
One of the most common chemical engineering operations is the separation of two or more
compounds based on the differences of the boiling point. Therefore, this operation is applied in the vapor-
liquid equilibrium (VLE) experiment. In this experiment, vapor-liquid equilibrium unit is suitable for
investigating the relationship between the vapor and liquid at equilibrium state at 1 atm (at atmospheric
pressure) and at high pressure up to 2 bars. The purpose of the experiment using vapor-liquid equilibrium
unit is to construct an equilibrium curve for the methanol and water system at the atmospheric pressure.
The vapor-liquid equilibrium unit actually can be used to study any binary system as well as the
multi component system. For example, in this experiment, the mixture of methanol and water with
unknown composition is fed into an evaporator. When the heater is switched on, the mixture started to
boil. The vapor will rise up and cooled down by the condenser at the top of the evaporator. As the vapor
starts to condense, the liquid will fall back into the evaporator. So, the system will stabilize and finally
reached at equilibrium state when the temperature is constant. Then, the samples of the vapor and liquid
are taken to determine their compositions by using a refractometer to know the refractive index.
This unit must be operated under the supervision of authorized personnel who has been properly
trained to handle this unit. Before attempting to start the experiment and run the unit, make sure that all
operating instructions supplied with this unit carefully and have already been read. Moreover, while
conducting the experiment, the students should always check and identify any leak or make sure that the
level of water is enough to submerge the heater and temperature sensor. All the safety and precautions
should be taken while conducting this experiment. Besides that, the students must be careful while
handling the liquid at high temperature and before draining the samples, the heater must be switched off
in order to cool the liquid in the evaporator.
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3.0 OBJECTIVES:
The objective of this experiment is:
To construct an equilibrium curve for the methanol-water system at atmospheric pressure.
The Vapor-Liquid Equilibrium Unit is a bench top unit designed to investigate the
relationship between vapor and liquid at equilibrium for any binary system as well as for
multi component system. The system may run the unit an elevated pressure.
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4.0 Theory
Vapor liquid equilibrium obeys Roult’s Law which give a definition law that relates the vapor
pressure of an solution was dependent on the mole fraction of a solute added to solution. Roult’s Law
only works for ideal mixture and was commonly used for predicting the vapor-liquid equilibrium for an
ideal solution in equilibrium with an ideal gas mixture from the pure component vapor-pressure data. The
partial vapor pressure of a component in a mixture was equal to the vapor pressure of the pure component
at that temperature multiplied by its mole fraction in the mixture(Clark,2005).Roult’s Law can be
expressed by:
Figure 4.1.1: Schematic diagram of VLE setup
Psolution = XsolventP°solvent (Equation 4.1)
Where
Psolution=vapor pressure of the solution
Xsolvent=mole fraction of the solvent
P°solvent=vapor pressure of the pure solvent
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In order to reduce VLE calculations by Roult’s Law were the vapor phase was an ideal gas and the
liquid phase was an ideal gas solution.
Y i P = X i P i sat (eq 4.2) ∑
P =∑ (eq 4.3)
P= (eq 4.4)∑
P =
∑
(Equation 4.5)
When we discussed the phase behavior of pure fluids, we found that the temperature and pressure
were constant when the two phases were in equilibrium. Thus, the saturated liquid and vapor points were
both at the same temperature. When the liquid is heated it will boil at the same temperature as that at
which the vapor will condense when it is cooled. Another way of saying the same thing is that the bubble
point (boiling point) and dew point are the same for a pure fluid.
When we have two components in both the vapor and liquid phases, the bubble point and dew points no
longer coincide. There is a difference in composition between the liquid and vapor phases that are in
equilibrium at the same T and P .It means that when you raise the temperature of a mixture until it boils,
more of the more-volatile component ends up in the vapor phase. The liquid phase is left enriched in the
less-volatile component. Thus, you can achieve a partial separation in the mixture. This is the principle
behind distillation that accounts for most of the separation done in the chemical industry(Rowley,Vapor
Liquid Equilibrium).By using the partial pressure calculation of Roult’s Law,value of compositions vapor
and liquid can be findalso its boiling point.The graph from figure 4.1.1 below can be plotted when all the
values were get while figure 4.1.2 was for composition of two different component when its equilibrium
state achieved.
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Figure 4.1.2 : Boiling Point Diagram
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Figure 4.1.3: Equilibrium Diagram
In other hand,Vapor Liquid Equilibrium also can be determine by other law which was Dalton’s
Law.Dalton’s Law states that the total pressure exerted by the mixture of non -reactive gases is equal to
the sum of the partial pressure of gases itself(Dalton’s Law,2013).Mathematically,the pressure of a
mixture of gases can be defined as the summation,
∑ (Equation 4.6)
Or
Ptotal=p1+p2+ p3+...+pn
Where pn is partial pressure for each component.
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5.0 Apparatus
Vapor Liquid Equilibrium Unit
Refractometer
Distilled water
Measurement cylinder
Dropper
Power supply
Suck pump
Mask
Gloves
Methanol Beaker
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5.0 Apparatus
Figure 5.19:V9
Figure 5.6:V3
Figure 5.7:Heater
Figure 5.8:
Eva orator
Figure 5.12: V4
Figure 5.13:V5
Figure 5.14: V1
Figure 5.16: TI 02
Figure 5.21: Pressure
Gau e
Figure 5.20: Safety
Valve
Figure 5.15: Control
Panel
Figure 5.11:V6
Figure 5.10 Cooling
Water
Figure 5.9: V10
Figure 5.5: V7
Figure 5.1:V2
Figure 5.2: V13
Figure 5.18:V8 Figure 5.17: V14
Figure 5.4:V12 Figure 5.3: V11
Figure 5.0 :- Model BP16 Vapor Liquid Equilibrium Unit
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Figure 5.22 :- REFRACTOMETER
Figure 5.23 :- Control Panel of Model BP16 VLE
Figure 5.28:PT 1
Figure 5.27:
MAIN SWITCH
Figure 5.26:
SUIZ HEATER
Figure 5.25:TI 02
Figure 5.24: TIC
01
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6.0 Procedures
6.1 General start-up procedures
1. The equilibrium data for the binary system were obtain 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.
6.2 General Experiment Procedures
1. The liquid mixture of 3 to 6L at the desired composition were prepared and was poured into the
evaporator through valve 1 and closed it.
2. The valve V13 and V14 were opened at the level sight tube. The liquid level has been sure that
it above the safety line on the level sight tube. The valves V13 and V14 were closed back.
3. The valve V8 was opened for operation at atmospheric pressure.
4. Turn on the compressed air supply and set the desired pressure at the regulator for operation at
elevated pressure. The valve V9 was opened to start pressurizing the unit, Then the valve V9 was
closed when the pressure has been reached.
5. The valve V10 was opened and adjusted to allow about 5 to 10 L/min of cooling water to flow
through the condenser.
6. The temperature controller TIC-01 was set to slightly above the expected boiling point of theliquid mixture.
7. The heater was switched on.
8. The temperature rise in TCI-01 was observed. When the temperature at TCI-02 started to
increased sharply, the liquid in the evaporator has begun to boil. The pressure at PI-01.All the
temperature and pressure were waited to stabilize at a steady state value.
9.The evaporator pressure and the liquid, vapor temperatures recorded.
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10.A vapor and liquid sample were collected from the unit as described in section 3.4.
6.3 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 50°C.
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.
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6.4 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.
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6.5 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 as described in section 6.1 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 100°C.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. Waited 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 vapor 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.
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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 wasclosed. 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 as described in section 6.3 were performed.
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7.0 RESULT
Vapor liquid equilibrium data
Water (L) Methanol
(L)
Temperature (oC) Refractive Index (nD)
Vapor Liquid Vapor Liquid
3.0 0.1 93.0 89.3 1.34074 1.33367
3.0 0.3 89.3 86.6 1.33895 1.33385
3.0 0.5 87.5 83.6 1.33899 1.33384
3.0 1.0 83.3 81.5 1.33832 1.33384
3.0 2.0 79.9 76.5 1.33830 1.33394
3.0 3.0 77.8 73.6 1.33798 1.34040
Table 7.1
Water (L) Methanol
(L)
Temperature (oC) Refractive Index (nD)
Vapor Liquid Vapor Liquid
1.0 2.0 72.7 71.6 1.34187 1.34246
1.0 3.0 71.0 70.1 1.33969 1.34230
1.0 5.0 70.1 68.6 1.33812 1.34162
Table 7.2
Methanol Water
Density (g/m ) 0.79 1
Molecular weight (g/ mol) 32.04 18
Table 7.3
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Temperature and mole fraction of Methanol ()
Mole fraction
Y
(Vapor)
X
(Liquid)
Y
(Vapor)
X
(Liquid)
93.0 89.3 0.01341 0.01333
89.3 86.6 0.05356 0.05335
87.5 83.6 0.09373 0.09337
83.3 81.5 0.1740 0.1734
79.9 76.5 0.3078 0.3068
77.8 73.6 0.4148 0.4155
72.7 71.6 0.6307 0.6340
71.0 70.1 0.7770 0.7785
70.1 68.6 0.9233 0.9257
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0
10
20
30
40
50
60
70
80
90
100
0 0.2 0.4 0.6 0.8 1
t e m p e r a t u r e ( ° C )
Vapor/Liquid Mole Fraction (x/y)
T-xy diagram for methanol-water system
Temperature Vapor (C)
Temperature Liquid (C)
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1
V a p o r m o l f r a c t i o n
Liquid mol fraction
X-Y Equilibrium Graph
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8.0 CALCULATIONS
i) Number of moles of
VOLUME OF WATER (L) MOLES OF WATER (MOL)
3 166.667
1 55.556
Volume
Volume
Density of water
Density of methanol (79
Molecular weight Molecular weight 2
ℎ
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Volume
79
99
99 2
Volume
79
79
79 2
Volume 2
79
2
2
Volume
79
27
27 2
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Volume 2
79
2
2
Volume
79
27
27 2
Volume
79 99
99 2
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Mole fraction of Methanol ().
Table 8.2
Volume used (L) Volume used (L) Mole
(mol)
Mole
(mol)
(
)
Mole fraction
(
)
Mole fraction
3.0 0.1 7 2.4744 169.1414 0.99 0.01
3.0 0.3 7 7.4231 174.0901 0.96 0.04
3.0 0.5 7 12.3719 179.0389 0.93 0.07
3.0 1.0 7 24.7438 191.4108 0.87 0.13
3.0 2.0 7 49.4875 216.1545 0.77 0.23
3.0 3.0 7 74.2313 240.8983 0.69 0.31
1.0 2.0 97 105.0435 0.53 0.47
1.0 3.0 72 129.7873 0.42 0.58
1.0 5.0 27 179.2748 0.31 0.69
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Composition of Methanol () in mole fraction
Mole fraction Refractive Index, RI Mole fraction
Vapor Vapor
( )
(
)
Vapor Liquid
(vapor)
Y
(liquid)
X
93.0 89.3 0.99 0.01 1.34074 1.33367 0.01341 0.01333
89.3 86.6 0.96 0.04 1.33895 1.33385 0.05356 0.05335
87.5 83.6 0.93 0.07 1.33899 1.33384 0.09373 0.09337
83.3 81.5 0.87 0.13 1.33832 1.33384 0.1740 0.1734
79.9 76.5 0.77 0.23 1.33830 1.33394 0.3078 0.3068
77.8 73.6 0.69 0.31 1.33798 1.34040 0.4148 0.4155
72.7 71.6 0.53 0.47 1.34187 1.34246 0.6307 0.6340
71.0 70.1 0.42 0.58 1.33969 1.34230 0.7770 0.7785
70.1 68.6 0.31 0.69 1.33812 1.34162 0.9233 0.9257
Table 8.3
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Temperature and mole fraction of Methanol ()
Mole fraction
Y
(Vapor)
X
(Liquid)
Y
(Vapor)
X
(Liquid)
93.0 89.3 0.01341 0.01333
89.3 86.6 0.05356 0.0533587.5 83.6 0.09373 0.09337
83.3 81.5 0.1740 0.1734
79.9 76.5 0.3078 0.3068
77.8 73.6 0.4148 0.4155
72.7 71.6 0.6307 0.6340
71.0 70.1 0.7770 0.7785
70.1 68.6 0.9233 0.9257
Table 8.4
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1.34246 to 1.34162. The refractive index for vapor methanol is also decrease from 1.34187 to
1.33812. The mole fraction of the liquid methanol is increase from 0.6340 to 0.9257. The
mole fraction of the vapor methanol is also increase from 0.6307 to 0.9233.
Through the X-Y equilibrium graph, when the mole fraction of liquid methanol
increase the mole fraction of vapor methanol is also increase. The mole fraction that had been
used in the graph is calculated using the mole fraction formula.
Methanol is a volatile liquid. During the experiment, putting the methanol in the
beaker without closing the beaker can cause the half of the methanol is vaporize slowly. The
methanol is added before the temperature heater is lower than 50°C. All this action can cause
the error for this experiment and it can give not accurate reading. The eyes are not
perpendicular when the reading of methanol in the cylinder is recorded.
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10.0 CONCLUSION
As the conclusion, this experiment was successful carried out. The relationship between the
vapor and liquid at the normal pressure was successfully determined. The maximum mole
fraction of methanol is 1. The objective of this experiment is to construct an equilibrium
curve for the methanol-water system at atmospheric pressure. From the data of this
experiment, the composition of methanol in vapor is higher than the liquid. The composition
of methanol in vapor and liquid is increase when the volume of methanol is also increase.
When the objective of this experiment was achieved, it can be concluded that this experiment
is successfully done.
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11.0 RECOMMENDATION
Make sure that the evaporator, condenser and tubing’s are cleaned properly. Flush the
system with the de-ionized water.
Always make sure that there is enough liquid all the time to fully submerged the
heater and temperature sensor.
Be extremely careful when handling the liquid at high temperature.
Always switch of the heater and allow the liquid to cool before draining.
Make sure that the eyes is perpendicular during the reading the methanol in the
cylinder is recorded.
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12.0 Reference
1. http://www.fpharm.uniba.sk/fileadmin/user_upload/english/Physical_Chemistry/3-
Liquid-vapour_equilibrium.pdf , Retrieved 25 November 2013
2. http://www.chemguide.co.uk/physical/phaseeqia/idealpd.html Retrieved 25
November 2013
3. http://chemed.chem.wisc.edu/chempaths/GenChem-Textbook/Vapor-Liquid-
Equilibrium-843.html Retrieved 25 November 2013
4. Manual Lab Report CPE 451
5. http://lorien.ncl.ac.uk/ming/distil/distilvle.htm Retrieved 25 November 2013
6. http://chemed.chem.wisc.edu/chempaths/GenChem-Textbook/Vapor-Liquid-
Equilibrium-843.html Retrieved 25 November 2013
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13.0 Appendix
Figure 13.1 :-Distilled Water Figure 13.2 :-Measurement Cylinder
Figure 13.3 :-Dropper Figure 13.4 :-Power Supply
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Figure 13.9 :- Model BP16 Vapor Liquid Equilibrium Unit