M1 - VLE Lab Manual

VAPOUR LIQUID EQUILIBRIUM UNIT
1.0 INTRODUCTION
This Vapour Liquid Equilibrium Unit has been designed for teaching, training and research
purposes on vapour liquid equilibrium. The unit is suitable for investigating the relationship
between vapour and liquid at equilibrium for different mixtures. It can be operated at
atmospheric pressure as well as elevated pressures of up to 4bar(g). It mainly consists of
an evaporator, immersion heater, condenser and product coolers. Instruments are provided
for the measurement of the evaporator’s pressure and temperature while provisions are
also given for both liquid and vapour sampling.
Among the special features of the unit are:

 All components are made of stainless steel to withstand corrosion and most chemicals
used during experiments.
 Insulation of evaporator to prevent heat loss to the surroundings.
 Digital instrumentations allow more accurate measurements of pressure and
temperature.
 Level sight tube at evaporator for observation of liquid level.
 Top and bottom sample collectors to ensure depressurization and cooling of samples
before collection.
1
2.0 GENERAL DESCRIPTION
The Vapour Liquid Equilibrium Unit can be used to study any binary system as well as multi
component systems. For example, a liquid mixture of methanol-water with a known
composition is initially fed into the evaporator. When the heater is switched on, the mixture
will heat up and start to boil. The heater has a temperature controller which will switch off
the heater if the evaporator’s temperature exceeded the setpoint value. As the liquid boils,
vapour will rise from the evaporator into the condenser. The vapour starts to condense,
and the liquid will flow back into the evaporator. The process continues until an equilibrium
state is reached between the vapour and liquid phases. This is when the temperature
remains constant. Samples of vapour and liquid can then be taken to determine their
compositions.
2
2.1 Unit Assembly
1
7
2
9
10
5
1
Figure 1: Unit Construction for Vapour Liquid Equilibrium Unit (Model:BP16)
1. Condenser 6. Pressure Relief Valve
2. Evaporator 7. Control Panel
3. Bottom Sample Collector 8. Top Sample Collector
4. Cooling Water Supply 9. Rotameter
5. Cooling Water Drain 10. Heater
3
Figure 2: Process flow diagram for the Vapor-Liquid Equilibrium Unit
4
2.2 Experiment Capabilities
The unit is capable of performing the following experiments:

 Determine the vapour liquid relationship at equilibrium for binary and multi-
component systems at atmospheric and elevated pressures.
 Study the effect of initial mixture composition upon the boiling temperature and
vapour liquid phase compositions.
 Determine the minimum boiling point of a binary mixture.
2.3 Specifications
a. Evaporator
Cylindrical vessel made of stainless steel.
Volume: 6-L
Diameter: 150 mm
Height: 350 mm
Fitted with a level sight tube, feed port, sampling/drain port, temperature &
pressure sensors, heater and cooling coil.
Heater power: 2 kW
Cooling coil heat exchange area: 0.15 m 2
b. Condenser
Coil type condenser made of stainless steel.
Heat exchange area: 0.30 m2
Cooling water flow range: 0 to 10 L/min
Fitted with inlet/outlet cooling water connections, vent and sampling ports.
c. Bottom sample collector

Cylindrical vessel with cooling coil made of stainless steel.
Volume: 250 mL
Heat exchange area: 0.01 m2
Fitted with inlet/outlet cooling water connections, vent and drain ports.
d. Top sample collector

Cylindrical vessel made of stainless steel.
Volume: 1-L
Fitted with vent and drain ports.
e. Control panel
Consists of the main switch, heater power switch and digital displays for
evaporator temperature controller, pressure and vapour temperature sensors.
5
2.4 Technical Specifications

Operating limits:
Temperature: 0 to 200°C
Pressure: 0 to 10 bar(g)
Max. cooling water pressure: 2 bar(g)
2.5 Overall Dimensions

Height: 2.00 m
Width: 1.27 m
Depth: 0.63 m
2.6 Utilities Requirement

Electrical supply: 240 VAC / 50 Hz (1-phase)
Cooling water: laboratory tap water, 10 LPM @ 2 m head
Drainage point
Refractometer
2.7 Valves List
Tag Type Function

V1 Ball Charging of feed into the evaporator
V2 Globe Bottom sampling flow control
V3 Ball Sampling or drainage of evaporator
V4 Ball Venting of bottom sample collector
V5 Globe Top sampling flow control
V6 Ball Venting of top sample collector
V7 Ball Sampling or drainage of top sample collector
V8 Globe Venting of condenser
V9 Ball Isolation of compressed air line
V10 Globe Cooling water flow control to condenser
V11 Ball Cooling water flow to evaporator
V12 Ball Cooling water flow to bottom sample collector
V13 Ball Isolation of level sight tube
V14 Ball Isolation of level sight tube
6
2.8 Instrumentation and Control
Tag Description Range

Evaporator temperature controller,
TIC-01 0–200.0°C
Liquid temperature sensor
TI-02 Vapour temperature sensor 0–200.0°C
PI-01 Evaporator pressure sensor 0–10 bar(g)
PI-02 Condenser pressure gauge 0–10 bar(g)
FI-01 Cooling water flow rotameter 0–10 L/min
– Pressure relief valve at condenser 0–10 bar(g)
7
3.0 INSTALLATION AND COMMISIONING
3.1 General Installation Procedures

The unit must be placed at a rigid and level floor that has adequate strength to
support its complete weight.
Connect the electrical socket to 240-VAC/50Hz/1 phase power supply.
Connect the water inlet nozzle and the drain nozzles with proper size water hose.
3.2 Cooling Water Supply

The Vapour Liquid Equilibrium Unit requires a source of clean and constant
temperature (cold) laboratory tap water with flow approximately 10 liters per minute
at 2m head. The Vapour Liquid Equilibrium Unit comes with a control valve
installed on the unit to control the water flow rate.
Connect the water supply to the cold water inlet using the hose provided.
3.3 Cooling Water Drain

The Vapour Liquid Equilibrium Unit comes with a water outlet nozzle to drain the
cooling water supply. The cooling water outlet line should be allowed to flow
directly into the drain.
Connect the hose provided to drain the cooling water supply.
3.4 Drainage Point

The Vapour Liquid Equilibrium Unit comes with a drainage point to drain the liquid
be used in the experiment.
Connect properly the hose provided to drain the liquid mixture from the evaporator.
3.5 Commissioning Procedures

Push the reset button of the Earth Leakage Circuit Breaker (ELCB) inside the
control panel after the main power supply is switched on. The ELCB should be
kicked off, indicating that the ELCB is functioning properly. If not, have a trained
wireman to inspect the trainer for any electrical leakage. The ELCB should be
tested at least once a month.
Switch on the main switch and the recorder power switch. The Loop Controller and
the Recorder should lit-up.
Make sure that all valves are initially closed.
Initiate the start-up procedures.
The unit is now ready to use.
8
4.0 SUMMARY OF THEORY
4.1 Introduction of Vapor-Liquid Equilibrium
Let us consider the meaning of an equilibrium state as applied to a multi component,

multiphase system comprised of non-reacting substances. As an example, suppose we
introduce liquid water and liquid methanol into a vessel equipped with means of measuring
pressure and temperature and of withdrawing samples of liquid and vapour for analysis.
We now place the vessel in a bath maintained at a specific temperature. Within the vessel
water and methanol will begin to distribute themselves between liquid and vapour phases.
This distribution process involves vaporization and diffusion. Eventually, the system will be
in an equilibrium state, which can be verified when successive reading of the temperature,
pressure, liquid mol fractions and vapor mol fractions are identical. This equilibrium state is
reproducible and according to the phase rule,the condition is unique for a two-component,
two-phase system when any two of its intensive properties are specified, although the
quantities of the phases, and thus the extensive properties, may differ. In applying
thermodynamics to phase equilibrium, we are mainly interested in intensive properties and
the relationships between them; therefore the phase rule specifies the condition necessary
to determine the equilibrium state.
As we have already seen, the successful application of the methods of thermodynamics

requires an empirical understanding of the system under study. To assist in cultivating this
understanding, we first consider various ways in which vapor-liquid equilibrium data may
be presented and thereby seek to develop a physical appreciation of the variables of phase
equilibrium and how they are interrelated. Often, however, the concept of phase equilibrium
and the variables expressing it do not acquire physical meaning until one considers the
experiment determination.
4.2 Pxy and Txy Diagram
In studying vapor-liquid equilibrium in a binary system, there are four intensive variables
which will concern us; temperature, pressure, a single liquid mole fraction, and a single
vapor mole fraction. Only a single mol fraction is required to describe the composition of a
phase in a binary system because of the condition that mol fractions in a phase must sum
to unity. Application of the phase rule to a binary system shows that the maximum numbers
of intensive variables, which can be specified, are two - this occurs when only a simple
phase is present. Therefore, to graphically represent the phase behavior of a binary
system, a three-dimensional plot is necessary such as shown in Figure 3. It shows that
each phase is represented by a surface on PTxy coordinates. The upper surface
represents liquid phase, and the lower surface represents the vapor phase. Where there is
equilibrium between the two phases, we know that the temperatures and pressure must be
equal. Therefore, the compositions of the equilibrium phases are determined by the
intersection of a constant-temperature plane with a constant-pressure plane.
9
Figure 3: Ptxy diagram
In Figure 3 a constant-temperature plane is shown by the lens-shaped envelope AB which

lies in the vertical plane DAVaLaBE. This envelope is shown to intersect a constant-
pressure envelope KVaLaH that lies in the horizontal plane. The intersection of the
envelopes occurs in two places: on the liquid surface at the point L a and on the vapor
surface at point Va. These points represent values of x1 and y1 that are in equilibrium at the
temperature and pressure we have selected. Equilibrium liquid and vapor compositions are
shown as Lb and Vb where the isothermal plane 0CIVVbLbNP corresponding to Tb intersects
the isobaric pane MLVbLbC1 corresponding to Pb.
Because three variables are required to describe the state of a single phase, the
representation of phase behavior on a two-dimensional plot can be accomplished by
holding one variable constant; three such plots are possible. These types of plots
corresponding to the three-dimensional diagram in Figure 3 are shown on Figure 4, 5 and 6
unless we are concerned with the equilibrium near the critical region, we will have little use
for the PT plot and we will find that the envelopes on Txy and Txy diagrams will span the
entire range of fractions. Usually we are interested in systems at low to moderate pressure
where the constant-temperature envelope will resemble T a in Figure 5 and the constant-
pressure envelope will resemble Pa in Figure 4.
10
Figure 4: Pxy diagram
Figure 5: Txy diagram
Consider equilibrium at a constant temperature of Ta as requested on Figure 4. At

equilibrium the pressure must be equal for each phase and a horizontal line ties together
the saturated liquid and vapor curves. Such lines determine the equilibrium and vapor
compositions at a given pressure and are called tie lines. The phase rule requires
specification of two variables to determine the two-component, two-phase system. As we
have already specified Ta, only one other variable may be chosen. If we choose either x1
or y1, we have fixed a point on either saturated curve and tie line determines P and mole
fraction of the other phase. In Figure 5, a constant-pressure diagram; tie lines are
characterized by temperature.
4.3 Ideal System
In a homogeneous solution the number of molecules of any one component per unit area
of surface will be less than if that component exposed the same area of surface in the pure
liquid state. For this reason the rate of vaporization of a substance per unit area will
decrease with dilution. According to Raoult’s law the resulting partial pressure of
component A in the vapour phase is
p A=x A P A
(1)
where xA = the mole fraction of component A in the boiling liquid, and PA = saturation
pressure of pure component A at the temperature of the liquid mixture.
Dalton’s law states that the total pressure of an ideal gas mixture equals the sum of the
partial pressures
P=∑ pi
i
(2)
11
The partial pressure pi is by definition equal to the product of the gas-phase mole fraction
and the total pressure
pi≡ yi P
(3)
Equations (1) and (3) give the mole fraction of component A in the gas phase as
x P
y A= A A
P
(4)
Extend to a binary system, Raoult’s law and Dalton’s law (equations (1) and (2)) give
P= p A + p B=x A P A +( 1− x A )P B=x A ( P A −PB )+P B
or
P−P B
x A=
P A−P B
(5)
Equation (5) is used to find xA for ideal binary mixtures at selected temperatures between
the boiling temperatures of the two pure components at pressure P, and equation (4) gives
the corresponding value of yA.
The distribution coefficient, also called the vaporization equilibrium constant or just the K-
value for the component i, is defined by the equation
y A=K i x i
(6)
The relative volatility of component A relative to component B is defined as
K y /x
α AB= A = A A
K B yB / xB
(7)
or in combination with equation (5) for ideal mixtures,
α AB=P A /P B
(8)
Raoult’s and Dalton’s law give reasonable estimates for cognate molecules such as
benzene and toluene when distilled at normal or lower pressure. Pairs represent are
examples of ideal systems.
4.4 Non-Ideal Homogeneous Mixtures
In a close to ideal mixture, such as benzene and toluene, the intermolecular forces
between two benzene molecules are approximately the same as between a benzene and a
toluene molecule.
Deviations from Rauoult’s law are due to changes in the intermolecular forces, of which the
hydrogen bond plays an important role. The hydrogen bonds O→HO, N→HO, O→HN
are strong. In water the hydrogen bond is especially strong. A high fraction of a component
12
with fewer tendencies to form hydrogen bonds with water, will reduce the hydrogen bonds
in the water and increase its volatility. The increase in vapour pressure corresponds to a
positive deviation from Raoult’s law as shown in Figure 6 for the ethanol-water mixture at a
temperature of 60 C. The total pressure of this mixture goes through a maximum. A
composition giving maximum pressure when boiling at constant temperature, gives a
minimum boiling temperature when boiling at constant pressure. At this point the
composition of the vapour equals the composition of the liquid, and it is called an
azeotropic mixture. Figure 7 shows the mole fraction y of ethanol in the liquid as a
function of the mole fraction x of ethanol when an ethanol-water mixture boils at
atmospheric pressure. The mole fraction x = y = 0.894 or 96 percent by volume is the
azeotropic mixture of ethanol and water. The boiling-point of the azeotropic mixture is
78.15 C, which is below the boiling-points of the pure components. The mixture is called a
minimum azeotrope. At reduced pressures the azeotrope shifts towards higher alcohol
concentrations. It disappears at pressures below 0.08 bar absolute.
Figure 6: Vapor Pressure of ethanol ( PA) and water (PB) and total P = ( PA)+ (PB) of ethanol-water mixture.
X= mole fraction of ethanol in liquid. Dashed lines correspond to Raoult’s law
A mixture of acetone and chloroform shows a different type of deviation from Raoult’s law.
The pure components do not have hydrogen bonds. But chloroform has an active hydrogen
atom that acts as donor of an electron, thus forming a hydrogen bond between an acetone
and a chloroform molecule. This gives a negative deviation from Raoult’s law (Figure 8).
Figure 9 shows the mole fraction y of acetone in the vapour as a function of the mole
fraction x of acetone in the liquid when the mixture boils at atmospheric pressure. This
mixture has a maximum azeotrope, i.e. the boiling temperature of the azeotrope is above
the boiling-points of the pure components.
13
Figure 7: Mole Fraction y of ethanol in vapour as a fuction of mole fraction x of ethanol in liquid of
ethanol-water mixture boiling at atmospheric pressure.
Deviations from ideal behaviour in the liquid phase are taken into account by the liquid
phase activity coefficient γ, and equation (4) becomes
P
y A=x A γ A A
P
(9)
Equations (6) and (9) give
PA
K A =γ A
P
(10)
The activity coefficient is a function of temperature and composition of the liquid phase. An
appropriate models (Van Laar’s, Margules’, Wilson’s, UNIQUAC etc.) have been suggested
for calculation of the activity coefficient. Van Laar’s third-order equations for binary
mixtures of non-electrolytes are
2
A 12 x 2
ln γ 1 = 2
[ x 1 ( A12 / A21 )+ x 2 ]
(11)
14
Figure 8: Vapour pressure of acetone ( PA) and chloroform ( PB) and total pressure P = ( PA)+ (PB)
of acetone-chloroform mixture. X= mole fraction of acetone in liquid.
Dashed lines correspond to Raoult’s law
Figure 9: Mole Fraction y of acetone in vapour as a fuction of mole fraction x of acetone in liquid of
acetone-chloroform mixture boiling at atmospheric pressure.
15
4.5 PT Diagram
Figure 10: PT diagram
Figure 6 shows the curves formed by the intersection of the two constant-composition
planes, TSRVaCIII and VVVULaCII, with the liquid and vapor surfaces on Figure 3. Note that
it is possible for mixtures to have a critical temperature, C II and CIII, those above those of
either pure component. The intersection of the projections of the vapor portion of one curve
with the liquid portion of another locates an equilibrium point, L a, Va.
As temperature increases there is a narrowing of the range of composition over which a

liquid phase can exist. For example, from Figure 1 it is seen that for the isothermal plane
CIVVbLbNP corresponding to Tb component 2 is above critical temperature and therefore
cannot exist as a pure liquid – in fact, there is a maximum mol fraction component 2 above
which no liquid phase can form at this temperature. The composition range also narrows as
the pressure is increased. Figure 3 shows that the lens-shaped envelope formed by the
intersection of the constant-pressure plane, MLV bLb0CI at Pb with the liquid and vapor
surfaces does not with the liquid and vapor surfaces does not extend to x 1 = y1 = 1. This
limited composition range can also be discerned from figure 5 where it is observed that
pressure Pb lies above the vapor pressure curve for component 1. As the temperature or
pressure continues to increase, the composition range steadily diminishes. Often, a point is
reached where neither component can exist as pure conjugate liquid and vapor phases.
The preponderance of experimentally determined vapor-liquid equilibrium data is reported

at either constant temperature or pressure as either of these constraints can be easily
imposed on an experimental determination. Unless we are dealing with systems following
ideal solution behavior where the phase behavior may be calculated from pure component
properties, experimental data are needed to construct the phase diagrams.
16
5.0 GENERAL OPERATING PROCEDURES
5.1 General Operation
It is important that the user read and fully understand all the instructions and
precautions stated in the manufacturer's manuals supplied with the equipment
prior to operation. The following procedures will serve as a quick reference for
operating the equipment.
5.2. Evaporator temperature control

The evaporator temperature limit can be controlled by adjusting the setpoint of
TIC-01 on the control panel. The top value indicates the current bottom liquid
temperature, while the smaller bottom value indicates the setpoint temperature.
Simply use the arrow keys to adjust the temperature setpoint to the desired value,
usually slightly above the expected boiling point of the liquid mixture as follows :
Press lighty UP or DOWN arrow key to increase or decrease the value by one.
Press and hold UP or DOWN arrow key to increase or decrease the displayed
value at a rapid rate. New data will self-enter in five seconds, or can be entered by
pressing the adanced key.
5.3 Heater protection

The heater must be fully immersed in liquid when turned on to prevent heater burn-
out. Always fill the evaporator with at least 3-L of liquid before running any
experiments. The liquid level at the sight tube should be above the safety line
before the heater can be switched on.
5.4 Cooling water control

Use valve V10 which installed below the flowmeter FI-01 to adjust the cooling
water flow rate into the condenser. When running the unit, the exit cooling water
temperature from the condenser shall not exceed 40 °C. During shut-down, open
valve V11 to quickly cool down the liquid in the evaporator. Valve V12 is used to
cool the liquid sample in the bottom sample collector.
5.5 Pressure relief valve

The operating pressure limit is preset at the maximum of 10 bar(g). To reduce this
limit, pressurize the unit to the desired pressure using compressed air. Unscrew
the cap on the pressure relief valve and turn the nut counter-clockwise to reduce
the pressure limit until the valve starts to open. Screw the cap back onto the valve.
5.6 Venting and drainage

As a safety precaution, always cool down and depressurize the unit first before
opening any valves for draining. Follow the general shut-down procedures as
described in Section 6.3.
17
6.0 EXPERIMENT PROCEDURES
6.1 General Start-up Procedures
1. Obtain the equilibrium data for the binary system to be studied from literature.
2. Prepare a calibration curve of refractive index vs. composition plot for the
particular binary system. Refer to Appendix A.
3. Check that the evaporator and condenser is empty of liquid.
4. Ensure all valves are initially closed and the heater power switch is turned off.
5. Switch on the main power at the control panel. Check all sensors and
indicators are functioning properly.
6.2 General Experiment Procedures
1. Prepare about 3 to 6-L of liquid mixture at the desired composition and pour it
into the evaporator through valve V1. Close valve V1.
2. Open valves V13 and V14 at the level sight tube. Make sure that the liquid
level is above the safety line on the level sight tube. Close back valves V13
and V14.
3. For operation at atmospheric pressure, open valve V8.
4. For operation at elevated pressures, turn on the compressed air supply and
set the desired pressure at the regulator. Open valve V9 to start pressurizing
the unit, then close valve V9 when the pressure is reached.
5. Open and adjust valve V10 to allow about 5 to 10 L/min of cooling water to
flow through the condenser.
6. Set the temperature controller TIC-01 to slightly above the expected boiling
point of the liquid mixture.
7. Switch on the heater.
8. Observe the temperature rise in TIC-01. When the temperature at TI-02 starts
to increase sharply, the liquid in the evaporator has begun to boil. Observe the
pressure at PI-01. Wait for all temperatures and pressure to stabilize at a
steady state value.
9. Record the evaporator pressure and the liquid and vapour temperatures.
10. Collect a vapour and liquid sample from the unit as described in Section 3.4.
18
6.3 General Shut-down Procedures
1. Switch off the heater.

2. Open valve V10 to increase the cooling water flow rate through the condenser.
3. Open valve V11 to allow cooling water to flow through the cooling coil in the
evaporator.
4. If the unit is pressurized, slowly open valve V8 to depressurize the unit.
5. Wait for the temperature at the unit to drop to below 50°C.
6. Open valves V2 and V3 to drain all liquid from the evaporator.
7. Open valves V5 and V7 to drain all liquid accumulated at the condenser.
8. Close all valves and switch off the main power at the control panel.
6.4 Sampling Procedures
Both vapour and liquid samples can be taken from the unit for analysis.
Note: Sample volume to be taken should be as minimum (e.g less than 25ml) as
possible to avoid any effect on the volume remained in the evaporator.
1. Vapour sampling from the condenser

i) Ensure that vent valve V6 is opened and drain valve V7 is closed.
ii) Slowly open valve V5 to allow some condensed vapour from the
condenser to flow into the top sample collector. Close valve V5.
iii) Open valve V7 to collect the sample in a sampling vial.
iv) Immediately close the cap on the vial and immerse it in cold water.
2. Liquid sampling from the evaporator

i) Ensure that vent valve V4 is opened and drain valve V3 is closed.
ii) Open valve V12 to allow cooling water to flow through the bottom sample
collector.
iii) Then, slowly open valve V2 to allow some liquid from the evaporator to
flow into the sample collector. Close valve V2.
iv) Open valve V3 to collect the sample in a sampling vial.
v) Immediately close the cap on the vial and immerse it in cold water.
19
6.5 EXPERIMENT 1: Equilibrium Curve at Atmospheric Pressure
Objective:
To construct an equilibrium curve for the methanol-water system at atmospheric
pressure.
Procedures:
1. Perform the general start-up procedures as described in Section 6.1.
2. Open valve V8.
3. Pour 2-L methanol and 2.5-L water into the evaporator through valve V1.
Close valve V1.
4. Open valves V13 and V14 at the level sight tube. Make sure that the liquid
level is above the safety line on the level sight tube. Close back valves V13
and V14.
5. Open and adjust valve V10 to allow about 5 L/min of cooling water to flow
through the condenser.
6. Set the temperature controller TIC-01 to about 100°C.
7. Switch on the heater.
8. Observe the temperature rise in TIC-01. When the temperature at TI-02 starts
to increase sharply, the liquid in the evaporator has begun to boil. Wait for all
temperatures to stabilize at a steady state value.
9. Record the evaporator liquid and vapour temperatures.
10. Collect a liquid and vapour sample from the unit as described in Section 6.4.
11. Analyze the samples to determine their compositions.
12. Switch off the heater and open valve V11 to allow cooling water to flow
through the cooling coil in the evaporator.
13. Wait for the temperature at TI-02 to drop significantly (60°C) to signify that
boiling has stopped. Close valve V11.
14. Pour an additional 1-L methanol into the evaporator through valve V1. Close
valve V1. There is now about 3-L methanol and 2.5-L water in the evaporator.
15. Repeat steps 7 to 13 above.
16. Open valves V2 and V3 to drain all liquid from the evaporator.
20
17. Pour 4-L methanol and 0.5-L water into the evaporator through valve V1.
Close valve V1.
19. Pour an additional 1.5-L of methanol into the evaporator through valve V1.
Close valve V1. There is now about 5.5-L methanol and 0.5-L water in the
evaporator.
21. Perform the general shut-down procedures as described in Section 6.3.
Analysis & Discussions:
1. Record all experiment data in the sample table.

2. Plot the vapour and liquid compositions against the vapour temperature.
3. Construct the equilibrium curve by plotting the vapour composition against the
liquid composition.
4. Compare between the composition plot and equilibrium curve obtained from
the experiment to the literature data.
21
7.0 EQUIPMENT MAINTENANCE
1. After each experiment, drain off any liquids from the evaporator and condenser.
2. Make sure that the evaporator, condenser and tubings are cleaned properly. Flush the
system with de-ionized water.
3. Wipe off any spillage from the unit immediately.
8.0 SAFETY PRECAUTIONS
1. The unit must be operated under the supervision of an authorized staff who has been
properly trained to handle the unit.
2. All operating instructions supplied with the unit must be carefully read and understood
before attempting to operate the unit.
3. Always make sure that there is enough liquid all the time to fully submerge the heater
and temperature sensor.
4. Be extremely careful when handling liquid at high temperature.
5. Always switch off the heater and allow the liquid to cool down before draining.
6. Do not touch the hot components of the unit.
7. Feed stock which severely affect stainless steel 304 and polypropylene (PP) are not to
be used.
8. The system should not be subjected to shock, sudden impact, vibration, or additional
load.
9. Restore the system to operating conditions after any repair job.
10. Always check and rectify any leak.
11. Do not exceed the maximum cooling water pressure of 2 bar(g) for the condenser.
12. Be extremely careful when handling hazardous, flammable or polluting materials.
13. Do not stretch the Viton O-rings during servicing.
14. Make sure the system is sufficiently ventilated at all times during operation,
maintenance and storage.
15. Only properly trained staff shall be allowed to carry out any servicing or repair job.
Manufacturer's manual must always be observed.
22
Result Experiment
Composition Composition
Temperature (°C) RI % Error
Volume Volume experiment literature
Pressure methanol water
(L) (L)
Liquid Vapour Liquid Vapour Liquid Vapour Liquid Vapour Liquid Vapour
2.5
DRAIN ALL LIQUID FROM THE EVAPORATOR BY OPENING VALVE 2 AND VALVE 3
0.5
5.5
23
Density (p) Methanol,

= g/cm3
CH3OH
Density (p) Water, H2O = g/cm3
MW Methanol, CH3OH = g/mol

MW Water, H2O = g/mol
Vol Vol Mass Mass Mol Mol

Mol Fraction(Methanol)
Methanol Water Methanol Water Methanol Water
mL mL g g mol mol
2000
2500
3000
DRAIN ALL LIQUID FROM THE EVAPORATOR BY OPENING VALVE V2 AND V3
4000
500
5500
24
RI vs Composition for Methanol- Water Binary Mixture
1.346
1.344
1.342
1.34
1.338
RI
1.336
1.334
1.332
1.33
0 0.2 0.4 0.6 0.8 1
Composition ( Mol Fraction)
Figure 1: Graph of RI against Composition of Methanol – Water Binary Mixture
25
T-xy Diagram for Methanol-Water System at 1 atm
105
100
95
90
Temperature ('C)
85
80
75
70
65
60
0.0000 0.1000 0.2000 0.3000 0.4000 0.5000 0.6000 0.7000 0.8000 0.9000 1.0000
Liquid / vapor mol fraction
Figure 2: T-xy Diagram for Methanol-Water system at 1 atm
26
X-Y Equilibrium Diagram for Methanol-Water System at 1 atm
1.0000
0.9000
0.8000
0.7000
0.6000
Vapor mol fraction
0.5000
0.4000
0.3000
0.2000
0.1000
0.0000
0.0000 0.1000 0.2000 0.3000 0.4000 0.5000 0.6000 0.7000 0.8000 0.9000 1.0000
Liquid mol fraction
Figure 3: X-Y Diagram for Methanol-Water system at 1 atm
27

M1 - VLE Lab Manual

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

M1 - VLE Lab Manual

Uploaded by

Copyright:

Available Formats

VAPOUR LIQUID EQUILIBRIUM UNIT

Among the special features of the unit are:

2.0 GENERAL DESCRIPTION

2.1 Unit Assembly

Figure 1: Unit Construction for Vapour Liquid Equilibrium Unit (Model:BP16)

1. Condenser 6. Pressure Relief Valve

2. Evaporator 7. Control Panel

3. Bottom Sample Collector 8. Top Sample Collector

4. Cooling Water Supply 9. Rotameter

5. Cooling Water Drain 10. Heater

Figure 2: Process flow diagram for the Vapor-Liquid Equilibrium Unit

2.2 Experiment Capabilities

The unit is capable of performing the following experiments:

c. Bottom sample collector

d. Top sample collector

2.4 Technical Specifications

2.5 Overall Dimensions

2.6 Utilities Requirement

2.7 Valves List

Tag Type Function

2.8 Instrumentation and Control

Tag Description Range

3.0 INSTALLATION AND COMMISIONING

3.1 General Installation Procedures

3.2 Cooling Water Supply

3.3 Cooling Water Drain

3.4 Drainage Point

3.5 Commissioning Procedures

4.0 SUMMARY OF THEORY

4.1 Introduction of Vapor-Liquid Equilibrium

Let us consider the meaning of an equilibrium state as applied to a multi component,

As we have already seen, the successful application of the methods of thermodynamics

4.2 Pxy and Txy Diagram

Figure 3: Ptxy diagram

In Figure 3 a constant-temperature plane is shown by the lens-shaped envelope AB which

Figure 4: Pxy diagram

Figure 5: Txy diagram

Consider equilibrium at a constant temperature of Ta as requested on Figure 4. At

4.3 Ideal System

4.4 Non-Ideal Homogeneous Mixtures

Figure 10: PT diagram

As temperature increases there is a narrowing of the range of composition over which a

The preponderance of experimentally determined vapor-liquid equilibrium data is reported

5.0 GENERAL OPERATING PROCEDURES

5.1 General Operation

5.2. Evaporator temperature control

5.3 Heater protection

5.4 Cooling water control

5.5 Pressure relief valve

5.6 Venting and drainage

6.0 EXPERIMENT PROCEDURES

6.1 General Start-up Procedures

6.2 General Experiment Procedures

6.3 General Shut-down Procedures

1. Switch off the heater.

6.4 Sampling Procedures

1. Vapour sampling from the condenser

2. Liquid sampling from the evaporator

6.5 EXPERIMENT 1: Equilibrium Curve at Atmospheric Pressure

Analysis & Discussions:

1. Record all experiment data in the sample table.

7.0 EQUIPMENT MAINTENANCE

8.0 SAFETY PRECAUTIONS