LABORATORY MANUAL

SEPARATION TECHNOLOGY
(CKD 20102)

JANUARY
1
2020
 Experiment 1
Plate and Frame Filtration

1. Objective(s)
The students should be able to:

 Run the operation of Plate and Frame Filter for filtration of calcium carbonate slurry.
 Record the data of filtrate volume against time.
 Determine the density and viscosity of the filtrate at 20L and 50L volume.
 Determine filtration time to completion.
 Determine the lost quantity of calcium carbonate after filtration process.

2. Introduction

Filtration is the removal of solid particles from a fluid by passing the fluid through a filtering
medium on which the solids are deposited. Industrial filtrations range from sample straining to
highly complex separations. The fluid may be a liquid or a gas, the valuable stream from the filter
may be the fluid, solids or both. In industrial filtration, the solids content of the feed ranges from a
trace to a very high percentage. Fluid flows through a filter medium by a virtue of a pressure
differential across the medium. Filters are also classified into those that operate with pressure
above the atmospheric level on the upstream side of the filter medium and those that operate at
atmospheric pressure on the upstream side and a vacuum on the downstream side. Pressures
above the atmospheric level may be developed by a pump or blower. There are many industrial
filters, such as pressure filters, vacuum filters or centrifugal filters and separators. Filters are
divided into 3 types which are cake filters, clarifying filters and cross flow filters. Cake filters
separate relatively large amounts of solids as cake of crystal or sludge.

Filter presses are the pressure filters designed to de-water chemically conditioned sludge
on a batch basis using mechanically applied pressure to achieve high solid content sludge cakes.
The filter consists of a series of parallel plates; each dressed with a filter cloth and rigidly held
together in a structure frame. The filter plates are placed between the stationary and moving
platens. In operation, the hydraulic closing device compresses the plate pack. The recessed
chamber between the individual plates forms the cake space in which the suspended solids are
then retained. The slurry to be filtered is fed by slurry pump which pressure subjected to the
allowable pressure needed for filtration. During the filtration cycle, the filtrate passes through the

2
filter cloth and drains along a grooved rib of the plates while the solid is retained within the cake
chamber. Once the filtration pressure is reached and the filtrate discharge is reduced, the
compressed air is introduced to inflate the filter medium to speed up the filtration process. Once
the filtrate is reduced to droplets, the compressed air is released and releasing the hydraulic
pump which then opens up the press and shifting the filter plates either manually or mechanically
discharges the cake.

In industrial filtration, a common filter medium is canvas cloth. Synthetic fabrics such as
nylon, polypropylene and various polyesters are also highly resistant chemically. Filter aids are
used in the filtration of very fine solids or slimy to increase the porosity of the cake to permit the
passage of the liquor at a reasonable rate. Filter aids are diatomaceous silica, perlite or other
inert porous solids. The filter aids are pre-coated on the filter medium. Pre-coats prevent
gelatinous solids from plugging the filter medium as well as giving a clearer filtrate.

3. Chemicals and Ancillary Equipment

a) Chemicals required:
Calcium carbonate powder (commercial grade)
Water (in the tank 200 liters for making calcium carbonate slurry)

b) Ancillary equipment/apparatus required:

5000 mL beaker
Stop watch (for time recording)
Density meter and Viscosity meter

3
Figure 1: Diagram of Plate and Frame Filter

4
4. Operating Instruction

4.1 General Start-up Procedures

1. Dissolve 3.0 kg of calcium carbonate powder in a 5 liters beaker and transfer it to

the slurry tank. Different weight of calcium carbonate powder will be added in the water
to get the required slurry concentration.
2. In 100 liters of water, it will be 3 wt% calcium carbonate slurry. The slurry concentration
will be varied from 3 wt % to 5 wt %.
3. Switch on the main switch to check that the power supply is available to all the
equipment. The control power indicating lights for the incoming current supplies should
be lighted.
4. The pump must be checked for the correct rotation and it must not be run dry i.e. without
any liquid delivered.
5. Check the sealing of the pump for any leakage.
6. Check all filter plates are installed in the correct plate sequence and are packed together
with the plate handles resting neatly on the side bars.
7. Check filter cloths are properly arranged and tied. The cloth is to be free of creases on
the sealing face areas. Use only pre-shrunk, barrel neck clothes and ensure that it covers
congruently the eyes of the plate hang over the plate.
8. Check the filtrate outlet valves or spigots are fully opened.
9. Check that inlet feed pump maximum discharged pressure for filtering does not exceed
the maximum feed pressure stated in the specification. Recommended feed pressure is 5
kg/cm for most of the applications.
10. Check the electrical wiring for the motorized hydraulic pump if any.
11. Press the button to stop the process in case of emergency.
12. Ensure that the slurry tank have enough slurry before operating the pump. (Ask
technician for advice). Never run the pump in a dry condition even for a few
revolutions or the stator will be damaged.
13. Do not release the hydraulic pump pressure before operating the squeeze process. Also,
ensure that the feed process is completed. Do not inflate the rubber membrane when
there is no solids in the filter pack.
14. Do not release the hydraulic pump pressure until the compress air outlet valve is fully
opened.
15. Check and ensure that both the compressor and dryer are ON and the manual isolation
valve is OPEN to allow the compressed air supply to the filter press system.

5
6
4.2 Experimental Procedure

1. Open the air regulator outlet valve.

2. Check the pressure gauge setting.
3. Release the hydraulic pump air valve and operation valve (knob) anti- clockwise to
release the hydraulic pressure.
4. Pack the filter press by pushing it towards the stationary platen. At the same time, dress
up the filter cloths with creases.
5. Move the moving platen towards the filter plate pack.
6. Lower down the trust bar and alignment it in line with the hydraulic piston.
7. Move the hydraulic piston towards the trust bar by pumping the hydraulic pump using the
lever.
8. Check the filter pack alignment and the cloths to ensure no crease is formed. In order to
have a proper good sealed compression.
9. Pull the PVC drip tray towards the stationary platen at the bottom of the filter pack. This is
to contain any dripping during filtration process (if occur).
10. Start pumping the hydraulic ram until it reaches to the required working pressure. Then,
lock it by turning the operation valve (knob) clockwise.
Warning: Check to ensure that the slurry tank has enough slurry before operating the
pump. NEVER run the pump in a dry condition even for a few revolutions or the
stator will be damaged.
11. On the control panel, press the feed pump START button and the RUN light will be
ACTIVATED. This indicates that the process of feeding the slurry into the filter press has
started.
12. When the feeding of the slurry into the filter press had reached the pre-set timing or
pressure by the consolidation timer and feeding pressure gauge, which ever come first,
the pump will be stopped and the RUN light will be OFF.
CAUTION: Do not release the hydraulic pump pressure before operating the squeeze
process. Also, ensure that the feed process is already completed. Do not inflate
the rubber membrane when there is no solid in the filter pack.
13. Close the air regulator valve and SLOWLY open the Inlet valve. This will let the
compressed air in so as to inflate the rubber membrane SLOWLY. These processes will
squeeze the water out of the filtrate or cake.

7
4.3 Shut down Procedure

1. Upon completion, close the air regulator inlet valve and open the outlet valve slowly to
deflate the rubber membrane slowly.
2. Do not release the hydraulic pump pressure until the compress air outlet valve is fully
opened.
3. Shift the drip tray away from the bottom of the filter pack.
4. Release the hydraulic pump pressure by turning the operation valve (knob) anti-
clockwise. The hydraulic piston will retract back to the body.
5. Swing the trust bar back to the stopper and hold.
6. Push the moving platen back towards the hydraulic piston.
7. Move the end filter plate i.e. the one next to moving platen towards the hydraulic piston.
8 Let the solid cakes drop onto a receptacle at the bottom of the filter press. Subsequently,
unpack the rest of the filter plate one at a time.
9. Clean the residue from the filter cloth by mean of a plastic scrapper.
Warning: Do not use any sharp object to clean the filter cloth since this can damage the
filter cloth.
10. Ensure that all the sealing edges are clear of residues especially at the bottom area. This
is to prevent any improper sealing during the next filtration compression process.
11. Upon completion, for the next filtration process, subsequently repeat the operating
process.

8
5. Results & Discussion (Please attach this part in your report)
 The volume of filtrate, V in litres, is collected at different time intervals and must be recorded
in the data/result sheet (Table 1).
 Viscosity and density of filtrate must be checked and recorded for BOTH volume 20L and
50L (Table 2).
 Discuss all your results. Your discussion should covers, but not limited to, on the efficiency
of the process and relationship between viscosity and density of filtrate with volume. Do
some observation on the raw material, whether the raw material is too fine or otherwise.
 Please complete the following tables.

Table 1
Volume of Filtrate (L) Time (min)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100

Table 2
1. Initial Weight of Calcium Carbonate powder kg
2. Final Weight of Calcium Carbonate powder kg
3. Weight Loss of Calcium Carbonate power kg
4. Percentage of Weight Loss %
5. Total Filtration Time min
6. Total Volume of Filtrate L
7. Viscosity of Filtrate, µ At 20 L Pa.s
At 50 L Pa.s

9
8. Density of Filtrate, ρ At 20 L g/cm3
At 50 L g/cm3

10
 Experiment 2A
Bubble Cap Distillation

1. Objective(s)

The students should be able to:

 Operate vapour – liquid separation experiment using a Bubble Cap Distillation unit.
 Analyze the sample of top and bottom product by using Refractometer to obtain the
Refractive Index (RI) in order to determine their respective composition.
 Determine the volume of top product obtained for every experimental time interval.
 Determine the composition (mole fraction) of feed, final top and bottom products.

2. Introduction

Distillation is one of the important unit operations in many chemical industries and has been used
from the inception of chemical and process industry. Distillation is used for the separation of
components in a liquid mixture of volatile constituents. The distillation column is usually a vertical
column where the liquid and vapour phases of the mixture are made to mix and approach
equilibrium. The bubble cap distillation column provides distinct stages at which such equilibrium
can be approached.

Distillation is a process of separating the components of a solution by the application of

heat when the vapour produced by boiling the solution has a different composition to that of the
solution. If the vapour formed is condensed and subsequently reboiled it will produce, yet again, a
vapour of different composition. Repeated boiling of condensed vapours will ultimately produce a
product of desired quality rich in concentration of one of the components of the original solution.

Distillation takes place in a distillation column which, in essence, comprises a reboiler, a

column and a vapour condensed. The reboiler provides the heat for vapour generation; within the
column rising vapours continually mix with liquid flowing down the column, condense and are
reboiled until vapour of required composition leaves the column and condenses in the vapour
condenser to be removed as liquid product. A certain proportion of this condensate is returned to
the column, called reflux, the proportion being a major influence on the quality of the product
achieved.

11
 Since this experiment use batch distillation plant, therefore, it can be said that this is a
process whereby a specific quantity of a liquid mixture is separated into its components. The
technique is used extensively in laboratories and small scale production plants where the
equipment is often used for separating several different mixtures of where if only one mixture is
separated, the mixture is not produced continuously. The relatively high capital cost of continuous
distillation plants with their sophisticated control systems, often results in smaller companies
operating batch distillation plants. Batch Distillation is particularly useful for separating liquid
mixtures contaminated with solids which would otherwise foul a continuous plant.

The unit consists of distillation column filled with bubble cap trays with a vacuum jacket
and thermo-siphon reboiler, vapour condenser, infinitely variable reflux control, distillate cooler
and receiver, all manufactured in borosilicate glass. Vapour generated in the reboiler rises
through the column and is condensed in a vertical water-cooled condenser. The condensed
product leaves the column and passes into an infinitely variable reflux ratio controller
incorporating the variable area flow meters. Each column component has five bubble cap plates
with a temperature measurement nozzle on each plate. Vapour and liquid compositions
throughout are determined by respective temperatures. The unit is equipped with the facility for
liquid and gas sampling at the top and bottom of the column. A condenser consists of a coil type
heat exchanger. A reflux separator is provided at the top of the column. Reflux is returned to the
column and the product passes through a cooler and a graduated pipe section and can be
passed either to a receiving vessel, which allows product removal operating under vacuum or
back to the boiler.

3. Chemicals and Ancillary Equipment

a) Chemicals required:
Industrial grade Ethanol
Water

b) Ancillary equipment/apparatus required:

2000 mL beaker
50 mL beaker
100 mL measuring cylinder
Dropper (2 unit)
Glass rod
Pail
Refractometer (for measuring sample refractive index)

12
 Figure 1: The Bubble-Cap Distillation Unit

4. Operating Instruction

4.1 Safety Consideration

1. You must familiarize yourself with each item such as the Reboiler, Condenser, Distillation
Unit and the flow paths and apparatus before conducting of the experiment. This
distillation operation usually deals with very hot and highly flammable materials. Extreme
care must be taken when handling the apparatus, in taking readings and collecting
samples.

13
2. The flow meters should be operated smoothly in order to avoid pressure surges within
the equipment.
3. Inspect the equipment visually for any damaged components or glass breakage. If any
such defects are noticed, please report them to your instructor/technician.
4. Goggles must be worn at all times in the laboratory.
5. Appropriate rubber gloves must be worn when organic solvents are handled.
6. Avoid wearing clothes which can easily catch fire.
7. The flow rates of liquids should not exceed the maximum of the rates shown in the flow
meter.
8. The water supply pressure to the condenser and the coolers should not exceed 2 bar
gauge.
9. Inspect the equipment visually for glass breakage and leakage.
10. Do not allow the water pressure to exceed 2.0 bar maximum as indicated by PI.2.
11. Always maintain V8 in the open position during atmospheric operation (avoid
system pressurizing).
12. Don’t isolate cooling water until the heating has been shut down (at least 10 minutes).
13. Don’t switch on the immersion heater with the level in the reboiler below the heater
elements or when the reboiler is empty.
14. Don’t return the product distillate collected to the reboiler vessel when the equipment is in
operation.
15. Do not allow the liquid level to raise much above the top graduation on the tube before
the stop valves V2 and V3 are opened.
16. Don’t drain the liquid in reboiler vessel until its cold.
17. Do not touch the hot components of the unit.

4.2 General Start-up Procedure

1. Prepare 30 L of 10 % v/v (volume/volume) mixture of ethanol in water by mixing

appropriate quantities of the industrial grade of ethanol in distilled water.
2. By using Refractive Index (RI) method, check the RI of pure ethanol and pure water
and record as Standard Refractive Index (Table 1).
3. Refer to the diagram of the equipment in the lab for better/ accurate view.
4. Ensure valves V1, RCV1, V3, V4, V5, V6, V7, V9 and FCV2 are closed.
5. Ensure valves V2, V8 and V10 are open.
6. Open V6, start fill in the ethanol-water mixture up to the desired level (ask
lecturer/technician). Close back V6.
7. Slowly open the cooling water to the condenser and set the flow to about 6-8L/min
(max 2.0 bars).

14
8. Make sure water is indeed flowing through it.
9. Check water flows to the drain from the cooling water outlets.
10. Do not start the experiment until the cooling water flow is visible in the outlets to the
drain.
11. Ensure that the Bottom Product sampling valve V5 and Top Product sampling valve V4 is
closed.
12. Ensure that the Reboiler vessel is already charged with the ethanol-water mixture
through the charge port (refer to the diagram).
13. Check that the liquid level is satisfactory (refer to instructor/technician).
14. Otherwise top up with the ethanol-water mixture through the charge port (refer to
instructor/technician).
15. Ensure that the concentration of feed in the Reboiler vessel is correct and that the liquid
level is at the vessel equator (refer to lecturer/technician).
16. The Reboiler vessel should never be filled with liquid above the maximum level indicated.
17. The level should never recede below the minimum level while on operation.
18. Close the Reflux Adjustment Valve RCV1 and valve below Product Cooler V2.
19. Turn on the main power control switch.
20. Turn on the power switch of the heater.
21. Switch on electrical supply (green ‘heater on’ button).
22. Set heater controller HC.4 to maximum setting. (About 200 V).
23. Obtain a sample of ethanol-water mixture from the Reboiler through the Sampling
Port and test its composition using Refractometer. Record the reading at Time “0”
of “Bottom Product” in Table 2.
24. Allow a period of 15 minutes for the equipment to maintain thermal equilibrium with
surroundings.
25. Observe the temperature readings of all Temperature Indicator (TI). Record the
temperature reading every 5 minutes (from Time “0” onwards).
26. When distillate liquid is seen to flow through RI.1C, reduce the heat input and set HC.4 to
roughly 180V.
27. During this period observe HC.4.
28. The unit is now ready to be used for an experiment.

4.3 Experiment: Operation under Partial Reflux Condition (Reflux Ratio 1.0)

1. Ensure that the valve for Reflux Ratio RCV1 adjustment is opened.
2. Adjust both valve for Reflux Ratio RCV1 and valve below Product Cooler V2 so that both
readings on RI.1A and RI.1B provide a Reflux Ratio of 1.0 for the operation.

15
3. Wait for about 15 minutes until the flow rate shown by RI.1A and the temperature
readings at the top and bottom of the columns are steady. (Refer to instructor/technician).
4. Collect samples from the sampling valves, V4 and V5 for every 5 minutes. All
sample from V4 must be drawn and measure its volume. Record the volume in
Table 2.
5. Observe the temperature of the Reboiler TI4. If the temperature is already 90ºC, reduce
the current of the Reboiler to between 170V to 180V.
6. Observe the flow rate at RI.1A. Adjust the valve for Reflux Ratio RCV1 to ensure that
the Reflux Ratio is maintained at 1.0.
7. The concentration of the samples drawn is measured using the Refractive Index method.
8. Continue record the reading of temperatures for every 5 minutes.
9. Readings are recorded in the provided table of results.

4.4 General Shut-Down Procedures

1. Adjust heater controller HC.4 to minimum setting.

2. Switch off electrical supply (red ‘heater off’ button).
3. Turn off the power switch of the Reboiler.
4. Turn off the main power control switch.
5. Do not drain the hot liquid from the Reboiler. If necessary, the liquid within the system
could be drained only when the liquid is already cooled.
6. Allow the cooling water to run for some time (Ask lecturer/technician).

16
 5. Results (Please attach this part in your report)

 By using density and molecular weight information of ethanol and water, calculate the
composition of feed in mole.
 By using a graph paper, plot the graph of Refractive Index (RI) vs Mole Fraction of Ethanol
(Data provided in Appendix 1). From the graph, determine the final composition of top and
bottom products.
 Discuss all your results. Your discussion should covers, but not limited to, on the function of
refractive index in composition determination, importance of reflux ratio in distillation process
and the integration of all component in this plant (i.e cooling water, reboiler etc, condenser).
 Please complete the following tables.

Table 1
Ethanol industrial grade
Standard Refractive Index (RI)
Water

Table 2
Time Temperature Readings ( º C ) RI RI Volume of
(Min) TI 1 TI TI TI 2 TI TI TI 4 TI 5 TI 6 Top Bottom Top
Product
1A 1B 2A 2B Product Product (mL)
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100

17
 Appendix 1

Refractive Index (RI) Mole fraction of ethanol

1.332 0
1.334 0.02
1.335 0.03
1.337 0.07
1.339 0.09
1.341 0.11
1.344 0.13
1.346 0.16
1.347 0.17
1.348 0.20
1.348 0.23
1.349 0.27
1.349 0.32
1.350 0.36
1.352 0.42
1.354 0.48
1.356 0.55
1.358 0.64
1.359 0.74
1.361 0.85
1.362 1.00

18
 Experiment 2B
Packed Column Distillation

1. Objective(s)

The students should be able to:

 Operate vapour – liquid separation experiment using a Packed Column Distillation unit.
 Analyze the sample of top and bottom product by using Refractometer to obtain the
Refractive Index (RI) in order to determine their respective composition.
 Determine the volume of top product obtained for every experimental time interval.
 Determine the composition (mole fraction) of feed, final top and bottom products.

2. Introduction

Distillation is one of the important unit operations in many chemical industries and has been used
from the inception of chemical and process industry. Distillation is used for the separation of
components in a liquid mixture of volatile constituents. The Distillation column is usually a vertical
column where the liquid and vapour phases of the mixture are made to mix and approach
equilibrium. Packed Bed Distillation Columns are sometimes used to carry out the Distillation in
the industry.

Distillation is a process of separating the components of a solution by the application of

heat when the vapour produced by boiling the solution has a different composition to that of the
solution. If the vapour formed is condensed and subsequently reboiled it will produce, yet again, a
vapour of different composition. Repeated boiling of condensed vapours will ultimately produce a
product of desired quality rich in concentration of one of the components of the original solution.

Distillation takes place in a distillation column which, in essence, comprises a boiler, a

column and a vapour condenser. The boiler provides the heat for vapour generation; within the
column rising vapours continually mix with liquid flowing down the column, condense and are
reboiled until vapour of required composition leaves the column and condenses in the vapour
condenser to be removed as liquid product. A certain proportion of this condensate is returned to
the column, called Reflux, the proportion being a major influence on the quality of the product
achieved.

19
 Since this experiment use Batch Distillation plant, therefore, it can be said that this is a
process whereby a specific quantity of a liquid mixture is separated into its components. The
technique is used extensively in laboratories and small scale production plants where the
equipment is often used for separating several different mixtures of where if only one mixture is
separated, the mixture is not produced continuously. The relatively high capital cost of continuous
distillation plants with their sophisticated control systems, often results in smaller companies
operating batch distillation plants. Batch distillation is particularly useful for separating liquid
mixtures contaminated with solids which would otherwise foul a continuous plant.

This unit comprises of a reboiler operating on the thermosyphon principle heated by

either steam or electrically. Process vapours enter at the base of the column which contains a
packed column containing 10 mm Raschig Rings, (the vapour temperatures entering and leaving
the column are measured by temperature indicators TI 3 and TI1 respectively as shown in Figure
1) and are condensed at the top of the column in a condenser. The distillate is separated into
reflux, which is passed back to the column and product, which passes through a product cooler
and then through a graduated pipe section. The product may then be collected or returned back
to the reboiler. Vapours leaving at the top of the column are totally condensed to liquid distillation
in the overhead condenser and pass to the Reflux Control Flow Meters, RI 1A and RI 1B. RI 1A
indicates the quantity of distillate returned to the column via the three-way valve while RI 1B
indicates the quantity of distillate removed as product.

3. Chemicals and Ancillary Equipment

a) Chemicals required:
Industrial grade Ethanol
Water

b) Ancillary equipment/apparatus required:

2000 mL beaker
50 mL beaker
100 mL measuring cylinder
Dropper (2 unit)
Glass rod
Pail
Refractometer (for measuring sample refractive index)

20
 Figure 1: The Packed Column Distillation Unit

4. Operating Instruction

4.1 Safety Consideration

1. You must familiarize yourself with each item such as the Reboiler, Condenser, Distillation
Unit and the flow paths and apparatus before conducting of the experiment. This
distillation operation usually deals with very hot and highly flammable materials. Extreme
care must be taken when handling the apparatus, in taking readings and collecting
samples.
2. The flow meters should be operated smoothly in order to avoid pressure surges within
the equipment.

21
3. Inspect the equipment visually for any damaged components or glass breakage. If any
such defects are noticed, please report them to your instructor/technician.
4. Goggles must be worn at all times in the laboratory.
5. Appropriate rubber gloves must be worn when organic solvents are handled.
6. Avoid wearing clothes which can easily catch fire.
7. The flow rates of liquids should not exceed the maximum of the rates shown in the flow
meter.
8. The water supply pressure to the condenser and the coolers should not exceed 2 bar
gauge.
9. Inspect the equipment visually for glass breakage and leakage.
10. Do not allow the water pressure to exceed 2.0 bar maximum as indicated by PI.2.
11. Always maintain V8 in the open position during atmospheric operation (avoid
system pressurizing).
12. Don’t isolate cooling water until the heating has been shut down (at least 10 minutes).
13. Don’t switch on the immersion heater with the level in the reboiler below the heater
elements or when the reboiler is empty.
14. Don’t return the product distillate collected to the reboiler vessel when the equipment is in
operation.
15. Do not allow the liquid level to raise much above the top graduation on the tube before
the stop valves V2 and V3 are opened.
16. Don’t drain the liquid in reboiler vessel until its cold.
17. Do not touch the hot components of the unit.

4.2 General Start-up Procedure

1. Prepare 30 L of 10 % v/v (volume/volume) mixture of ethanol in water by mixing

appropriate quantities of the industrial grade of ethanol in distilled water.
2. By using Refractive Index (RI) method, check the RI of pure ethanol and pure water
and record as Standard Refractive Index (Table 1).
3. Refer to the diagram of the equipment in the lab for better/ accurate view.
4. Ensure valves V1, RCV1, V3, V4, V5, V6, V7, V9 and FCV2 are closed.
5. Ensure valves V2, V8 and V10 are open.
6. Open V6, start fill in the ethanol-water mixture up to the desired level (ask
lecturer/technician). Close back V6.
7. Slowly open the cooling water to the condenser and set the flow to about 6-8L/min
(max 2.0 bars).
8. Make sure water is indeed flowing through it.
9. Check water flows to the drain from the cooling water outlets.

22
10. Do not start the experiment until the cooling water flow is visible in the outlets to the
drain.
11. Ensure that the Bottom Product sampling valve V5 and Top Product sampling valve V4 is
closed.
12. Ensure that the Reboiler vessel is already charged with the ethanol-water mixture
through the charge port (refer to the diagram).
13. Check that the liquid level is satisfactory (refer to instructor/technician).
14. Otherwise top up with the ethanol-water mixture through the charge port (refer to
instructor/technician).
15. Ensure that the concentration of feed in the Reboiler vessel is correct and that the liquid
level is at the vessel equator (refer to lecturer/technician).
16. The Reboiler vessel should never be filled with liquid above the maximum level indicated.
17. The level should never recede below the minimum level while on operation.
18. Close the Reflux Adjustment Valve RCV1 and valve below Product Cooler V2.
19. Turn on the main power control switch.
20. Turn on the power switch of the heater.
21. Switch on electrical supply (green ‘heater on’ button).
22. Set heater controller HC.4 to maximum setting. (About 200 V).
23. Obtain a sample of ethanol-water mixture from the Reboiler through the Sampling
Port and test its composition using Refractometer. Record the reading at Time “0”
of “Bottom Product” in Table 2.
24. Allow a period of 15 minutes for the equipment to maintain thermal equilibrium with
surroundings.
25. Observe the temperature readings of all Temperature Indicator (TI). Record the
temperature reading every 5 minutes (from Time “0” onwards).
26. When distillate liquid is seen to flow through RI.1C, reduce the heat input and set HC.4 to
roughly 180V.
27. During this period observe HC.4.
28. The unit is now ready to be used for an experiment.

4.3 Experiment: Operation under Partial Reflux Condition (Reflux Ratio 1.0)

1. Ensure that the valve for Reflux Ratio RCV1 adjustment is opened.
2. Adjust both valve for Reflux Ratio RCV1 and valve below Product Cooler V2 so that both
readings on RI.1A and RI.1B provide a Reflux Ratio of 1.0 for the operation.
3. Wait for about 15 minutes until the flow rate shown by RI.1A and the temperature
readings at the top and bottom of the columns are steady. (Refer to instructor/technician).

23
4. Collect samples from the sampling valves, V4 and V5 for every 5 minutes. All
sample from V4 must be drawn and measure its volume. Record the volume in
Table 2.

24
5. Observe the temperature of the Reboiler TI4. If the temperature is already 90ºC, reduce
the current of the Reboiler to between 170V to 180V.
6. Observe the flow rate at RI.1A. Adjust the valve for Reflux Ratio RCV1 to ensure that
the Reflux Ratio is maintained at 1.0.
7. The concentration of the samples drawn is measured using the Refractive Index method.
8. Continue record the reading of temperatures for every 5 minutes.
9. Readings are recorded in the provided table of results.

4.4 General Shut-Down Procedures

1. Adjust heater controller HC.4 to minimum setting.

2. Switch off electrical supply (red ‘heater off’ button).
3. Turn off the power switch of the Reboiler.
4. Turn off the main power control switch.
5. Do not drain the hot liquid from the Reboiler. If necessary, the liquid within the system
could be drained only when the liquid is already cooled.
6. Allow the cooling water to run for some time (Ask lecturer/technician).

25
 5. Results (Please attach this part in your report)

 By using density and molecular weight information of ethanol and water, calculate the
composition of feed in mole.
 By using a graph paper, plot the graph of Refractive Index (RI) vs Mole Fraction of Ethanol
(Data provided in Appendix 1). From the graph, determine the final composition of top and
bottom products.
 Discuss all your results. Your discussion should covers, but not limited to, on the function of
refractive index in composition determination, importance of reflux ratio in distillation process
and the integration of all component in this plant (i.e cooling water, reboiler etc, condenser).
 Please complete the following tables.

Table 1
Ethanol industrial grade
Standard Refractive Index (RI)
Water

Table 2
Volume of
Top
Time Temperature Readings ( º C ) RI RI Product
(Min) TI 1 TI 2 TI 3 TI 4 TI 5 TI 6 Top Bottom
Product Product
0
5
10
15
20
25
30
35
40
45
50
55
60
65
70
75
80
85
90
95
100

26
27
 Appendix 1

Refractive Index (RI) Mole fraction of ethanol

1.332 0
1.334 0.02
1.335 0.03
1.337 0.07
1.339 0.09
1.341 0.11
1.344 0.13
1.346 0.16
1.347 0.17
1.348 0.20
1.348 0.23
1.349 0.27
1.349 0.32
1.350 0.36
1.352 0.42
1.354 0.48
1.356 0.55
1.358 0.64
1.359 0.74
1.361 0.85
1.362 1.00

28
 Experiment 3
Packed Column Gas Absorption

1. Objective(s)
The students should be able to:

 Operate vapour–liquid separation experiment using a Packed Column Gas Absorption

Process Unit.
 Analyze the sample using the method of direct titration in order to determine the amount of
NaOH reacted in the mixture with the sample.
 Calculate the concentration of CO2 being absorbed for every experimental time interval.

2. Introduction
Packed Beds are usually employed in Chemical and Process Industries for mass transfer
operations. Here, a gas stream is usually interacted with a liquid stream flowing counter currently
in order to affect the mass transfer. The flow rates of liquid and gas have to be carefully selected
in order to achieve effective mass transfer and in the meantime, to avoid undesirable phenomena
such as flooding of the column. It is anticipated that this experiment will impart to the students
with a good understanding of the concepts mentioned above.

For this particular equipment (Figure 1), there are three separated Packed Columns C1,
C2 and C3 of equal sizes are erected vertically. The Packed Columns are arranged to operate
individually. The bottom ends are connected to a line supplying air or a mixture of CO 2 in air
depending on the requirements of the experiment. Valves V1, V2 and V3 can separately control
the flow rates of the Compressed Air to each column. The Solute Gas whenever required is
supplied through flow control valves FCV1 and FCV2 and flow meters FI1 and FI2 respectively.
Gas outlet from the columns is vented to the atmosphere which is next to Packed Column C3.

Water is fed from the mains line or pumped to the top of each column. The water flow
rates can be controlled by using valves V4, V5 and V6. Provision is also available to supply water
to the top of the columns through a re-circulation pump which sucks water from a Recirculation
Tank which is close to Packed Column C1. The water flow rate is measured by means of a flow
meter FI3. Valves V8, V9 and V10 control the outlet flow rates for each column. Valves V11 and
V12 can be used to vent effluent gases and liquids and purge any liquids from the columns. By
means of a ‘Green Oil’ filled manometer and a multiport selection valve, Differential Pressure

29
across the column is determined. When column dynamics are being studied, water is
continuously circulated by means of the Recirculation Pump and Compressed Air is blown
through the column.

Plant operation is controlled from a free standing control panel fitted with a mimic
diagram housing flow controllers, pressure indicators and services controllers.

Figure 1: Packed Column Gas Absorption Process Unit

3. Chemicals and Ancillary Equipment

a) Chemicals required:
Hydrochloric acid (HCl)
Sodium hydroxide (NaOH)
Phenolphthalein Indicator

b) Ancillary equipment/apparatus required:

50 ml Burette and Retort Stand
10 ml Graduated Cylinder
50 ml Pipette

30
250 ml Conical Flask
Beakers

31
4. Operating Instruction

4.1 Safety Considerations

1. The flow meters should be operated smoothly in order to avoid pressure surges within
the equipment.
2. The flow rates of liquids and gases should not exceed the maximum of the flow meter.
3. The CO2 supply pressure to the column should not exceed approximately 2 bar.
4. The maximum flow rates should be controlled so that the pressure should be within the
manometer range particularly when the column is operated near flooding conditions as
shown by DP1 (Height of Indicator is about 5 cm).
5. Once adjustments are made on parameters such as flow rates etc., sufficient time should
be allowed for the process to attain steady state (Allow at least 15 minutes for this
operation).

4.2 General Start-up Procedure

4.21 Chemicals preparation:

0.01 M HCl Standard Solution 1 litre

1. Withdraw 10 ml solution of HCl 1 M from the container.
2. Pour 10 ml solution of HCl 1 M into 1000 ml volumetric flask.
3. Add distilled water up to marked level at volumetric flask.
4. Shake the solution for a while.

0.01 M NaOH Standard Solution 1 litre

1. Weigh 0.4 g of 40 M NaOH pellets.
2. Pour NaOH pellets into 100 ml beaker.
3. Add distilled water into the 100 ml beaker.
4. Use magnetic stirrer to stir the mixture.
5. Pour the mixture into 1000 ml volumetric flask.
6. Add distilled water up to marked level at volumetric flask.
7. Shake the solution for a while.

4.22 Pre-start up checks:

1. Inspect the equipment visually for any damaged components or glass breakage.
2. Ensure that the Cylindrical Re-circulation Vessel is charged with water and that the liquid
level is satisfactory (Refer to your lecturer or technician).

32
3. Ensure valves FCV1, FCV2, FCV3, FCV4, V7, V12 and V13 are closed.
4. Ensure valve V11 are open.
5. Choose the column to be operated (Ask lecturer/technician) and adjust the
following valves:

Valve Column 1 Column 2 Column 3

Open Closed Open Closed Open Closed
V1 X X X
V2 X X X
V3 X X X
V4 X X X
V5 X X X
V6 X X X
V8 X X X
V9 X X X
V10 X X X
SV1 X X X

6. Ensure the manometer is reading zero.

7. Switch the selector valve SV1 to connect to the column chosen.

4.23 Setting up of Liquid Flow:

1. Check valves V11, V12 and FCV3 is closed and open valve V7.
2. Turn on the power switch of recirculation pump.
3. Slowly open valve FCV4 to give the required flowrate of 0.5 L/min as indicated by FI3. 4.
Ensure that the liquid overflow from the unit is connected to a suitable drain.
5. Open valve V11 and V13 while close V7 when the water has entered the column and
when the flowrate has reached 1.5 L/min.
6. The unit is now ready to be used for experiment when the water has come down from the
column.

4.3 Experiment: Absorption of CO2 into water from Air-CO2 mixture

1. Open the water feed valve gradually until the desired flow rate 1.5 L/min is achieved as
indicated in FI3. Ensure that the water flow rate is allowed to stable for about 10 minutes
after each change until the desired value is reached.
2. Open the Compressed Air Valve and ensure that the pressure is 1.5 bar gauge.
3. Depending on the column to be operated, OPEN the valve V1, V2, or V3.
4. Gradually OPEN the feed valve FCV1 for Air flow until the desired flow rate about 60
L/min is indicated in the flow meter FI1. Allow flow rate of 40 L/min and increase to 60

33
 L/min after time elapse between 10 to 15 minutes. Ensure that you keep on monitoring
the Indicator from the manometer or DP1. Ensure that there is no ‘sudden jump’ of the
level. (Consult your lecturer or technician). Ensure that the water flow rate is allowed to
stable for about 10 minutes after each change until the desired value is reached.
5. After steady state conditions are reached, OPEN valve FCV2 GENTLY until CO 2 rate is 2
L/min is achieved.
6. Allow further period of 10 minutes for the Absorption process to attain steady state
(Consult your lecturer or technician).
7. Draw at least 30 ml sample from the outlet valve, V12 for every 10 minutes.

4.3.1 Direct Titration

1. Draw 10 ml of samples and pour into the 250 ml conical flask. Add in 30 ml (V1) of
prepared 0.01 M NaOH solution (Consult your lecturer or technician concerning how to
prepare this solution). The volume of NaOH is in excess to ensure that all CO 2 has
reacted with NaOH in the mixture.
2. Add a few drops of an indicator (Phenolphthalein) to the solution.
3. Pour in the already prepared 0.01 M HCl solution into the burette and do titrate it with the
mixture inside the conical flask.
4. Repeat the measurements every 10 minutes and carry out the titration with FRESH
samples until CONSTANT concentration of NaOH has been achieved.
5. Record your results in Table 1.

4.4 General Shut-Down Procedure

1. Slowly close CO2 supply valve.

2. Slowly close the compressed air flow at FCV1.
3. Open V7.
4. Turn off the power switch of recirculation pump.
5. Turn off the air supply and CO2 supply (green valve).
6. Open V11 and allow fresh water to enter the column for a few minutes to drain off the
water.

34
5. Results (Please attach this part in your report)

 Discuss all your results, elaborate more on the percentage of CO 2 being absorbed at each of
time interval. Your discussion should covers, but not limited to, efficiency and application of
all types of packings in each of column.
 By using the provided formula below, calculate the amount of CO 2 being absorbed by the
absorption column in this experiment.
Stoichiometry equation:

2 NaOH + CO2  Na2CO3 + H2O

Na2CO3 + HCl  CO2 + H2O+ NaCl

2 moles of NaOH results with 1 mole of CO2

Let,
x = moles of NaOH added = 0.01V1
y = moles of HCl used = 0.01V2
Then,
g moles of NaOH reacted = (x-y)
g moles of CO2 reacted = 0.5 (x-y)
Hence,
CO2 concentration = 0.5 (x-y)/ (VCO2 sample) = mol/Liter

 Please complete the following table.

Table 1
Time
Volume Of HCl Titrated, V2 (mL) CO2 concentration
(Minutes) (mol/Litre)
1 2 3 Average
0

10

20

30

40

50

60

35
 Experiment 4
Pulsed Column Liquid-liquid Extraction Process

1. Objective(s)

The students should be able to:

 Operate a Liquid – Liquid Extraction Experiment using a Pulsed Column Liquid – Liquid
Extraction Unit.
 To determine the height equivalent theoretical plates (HETP) for column by using
equilateral triangular diagram.
 To investigate the effect of the pulsation stroke on the HETP.

2. Introduction

Extraction is a unit operation used to separate components based on their Chemical Differences
instead of differences in Physical Properties. When separation of components of a Liquid Mixture
becomes ineffective or very difficult by means of Distillation, and then Liquid Extraction is one of
the main alternatives to consider.

Separation by liquid-liquid extraction can be defined as the selective removal of one or more
components either from a homogeneous liquid mixture or from a solution, using a second liquid or
solvent, which is partially or wholly immiscible with the first.

A widely used terminology describes the system in terms of :

o F : Feed.
o S : Solvent.
o R : Raffinate.
o E : Extract.

The equilateral-triangle diagram developed by Hunter and Nash is commonly used for multistage
extraction calculations involving ternary systems. In practice, toluene is used as solvent to
remove the solute, acetone, from water; the toluene-rich phase is called the extract, and the
water-rich phase the raffinate.

36
The following diagram indicates the Flow of Streams and Components In a Liquid – Liquid
Extraction System.

Components of Pulsed Column Liquid – Liquid Extraction Unit are as follows :

o Feed Vessels (B1 / B2) – Graduated Cylindrical Vessels with 25 L capacity.
o Column (K1) – a DN 80 Packed Column with 10 mm Ceramic Saddles. Effective Height
of column is 2.5 m.
o Dosing Pumps (P1 / P2) – 0.25 kW Piston Pumps with up to 42 L/h capacity.
o Pulsator (P3) – 0.25 kW Pulsator Pump with a 20 mm stroke and 50 Hz frequency.
o Receiving Vessels (B3 / B4) – Graduated Cylindrical Vessles with 25 L capacity.
o Pulsation Dampers (B5 / B6).

37
38
39
3. Chemicals and Ancillary Equipment

Chemicals Required:
 Acetone (Solute).
 Diionized-Water ( Diluent)
 Toluene (Solvent).

Ancillary Equipments Required:

 Two 2000ml Jug and two 25ml beakers.
 Refractometer index .

4. Operating Instruction

1. Prepare the following chemicals :

a) Feed (Heavy Phase): Mixture of Acetone – Water solution. Prepare 20 litres of
50wt % mixture of Acetone in Water by mixing appropriate quantities of the
Acetone in Distilled Water.
b) Prepare 20 litres of Solvent (Light Phase): Pure Toluene.
2. Ensure that all valves are closed.
3. Fill Feed Vessel B1 with the Acetone – Water solution and Feed Vessel B2 with the
Pure Toluene Solvent. Determine the composition of the feed (heavy phase) using
refractometer.
4. Turn on the power supply
5. Turn on the main power control switch.
6. Open valves V3. Switch on Feed Pump P1.
7. Allow the Acetone – Water Solution (Heavy Phase) to enter the column and fill to a
level of about 10 cm below the solvent inlet. Switch off Pump P1.
8. Open valve V4. Switch on Solvent Pump P2.
9. As the Solvent (Light Phase) enters the column, carefully watch the Interface Level which
forms between the Light and Heavy Phases. Maintain the interface level at 2-3 cm above
the solvent inlet.
10. The unit is now ready for experiment.

Experiment: Extraction of Acetone from Water Using Toluene.

In this experiment, there are two feeds to the Mixer and two outlet flows from the Settler.

40
 Feed Flows:
Solvent: Toluene (Light Phase).
Feed: Acetone – Water Mixture (Heavy Phase).
Outlet Flows:
Extract : Toluene Rich Phase.
Raffinate: Water Rich Phase.

PROCEDURES:
1. Check to ensure the liquid starts to overflow at the top of the column, stop Pump P2.
2. Turn on the both pumps P1 and P2 .
3. Turn on the Pulsator Pump P3 and set the Pulsation Stroke Length.
4. Let the experiment run for a while to attain steady state.
5. Allow both liquids to flow into the collection vessels B3 and B4 respectively. The bottom
product contains the Water Rich Phase (Raffinate ) while the top product contains the
Toluene Rich Phase ( Extract ).
6. Open valve V10 to withdraw a 10 ml sample of Raffinate and open valve V12 to collect a
10 ml sample of Extract .
Note: Take samples at suitable time intervals and measure their Refractive
Indices. When the readings are consistent over time, steady state has been
reached.
7. Record the Refractive Index of both samples and use the given Calibration Curves
(Appendix B) to determine the Acetone (Solute) composition in each phase.
8. Record all data in appendix B.
9. Repeat the experiment (steps 3 to 10) by turning on the pulsator pump P3 and changing
the pulsation stroke length. Fix the same flow rate and feed composition throughout the
whole experiment.

3.2 General Shut – Down Procedures.

1. Switch off pumps P1, P2 and P3.

2. Close valves V3 and V4.
3. Open valves V5, V6 and V9 to drain all liquid from the experiment.
4. Open valves V13 and V14 to drain all liquid from the Receiving Vessels B3 and B4.
5. Turn off the power for the control panel.

41
5. Results (Please attach this part in your report)

Discuss all your results. The questions below only serve as a guideline. Your discussion should
not only limit to these questions.

1. Plot the calibration curve for toluene rich phase and water rich phase (Refractive index vs
acetone weight percent) by refer data given in Appendix B.
2. Determine weight percent acetone of the raffinate and extract in Appendix A by refer to
calibration curve prepare in question 1.

3. Determine the required theoretical extraction stage from the pulsed column liquid-liquid
extraction experiment results by construct the graph using equilateral diagram given in
Appendix E. Refer to Appendix D for a step by step calculation guide.
4. Discuss the various factors that would help to increase the rate of transfer of solute to
solvent phase.
5. Explain how pulsation frequency increases the transfer rate in pulsed columns.

42
 APPENDIX A

Experiment: Extraction of Acetone from Water Using Toluene.

Results:

Feed RI
Feed Composition

Raffinate Extract
(water rich phase ) (Toluene rich phase)
Feed Solvent Solvent Pulsation
Time Refractive Solute Refractive Solute
flowrate flowrate to Feed stroke
(min) Index (Acetone) Index (Acetone)
(L/hr ) (L/hr ratio (mm)
Composition Composition
(wt %) (wt %)

APPENDIX B

43
 Data Calibration Curve for Toluene Rich Phase

No Volume (mL) Average Weight (g) Ave. % Weight Refractive

Index
(Ave)
Toluene Water Acetone Toluene Water Acetone Acetone Toluene
1 104.1 2.5 12.7 89.8 0.3 10.0 10.0 89.8 1.4753
2 91.8 3.0 25.2 79.1 1.1 19.8 19.8 79.1 1.4649
3 64.6 4.1 54.0 55.7 2.0 42.4 42.4 55.7 1.4304
4 50.0 5.4 67.4 43.1 4.0 52.9 52.9 43.1 1.4147
5 37.5 7.3 77.4 32.3 7.0 60.7 60.7 32.3 1.4006
6 16.3 23.0 81.6 14.0 22.0 64.0 64.0 14.0 1.3687

Data Calibration Curve for Water Rich Phase

No Volume (mL) Average Weight (g) Ave. % Weight Refractive

Index
(Ave)
Toluene Water Acetone Toluene Water Acetone Acetone Toluene
1 16.8 22.0 81.6 14.0 22.0 64.0 64.0 14.0 1.3681
2 13.9 25.1 80.1 12.2 25.0 62.8 62.8 12.2 1.3682
3 8.0 34.6 74.7 6.9 34.5 58.6 58.6 6.9 1.3661
4 3.6 46.1 65.0 3.0 46.0 51.0 51.0 3.0 1.3618
5 1.6 59.6 50.4 1.0 59.5 39.6 39.6 1.0 1.3556
6 1.4 80.2 25.5 0.2 79.9 20.0 20.0 0.2 1.3449

APPENDIX C

Equilibrium data Binodal/ Solubility Data for Acetone-Toluene-Water System

Toluene Rich phase Water Rich phase

Acetone Acetone
Water(wt%) Toluene(wt%) Water(wt%) Toluene(wt%)
(wt%) (wt%)
9.79 2.42 87.78 63.93 21.68 14.39
19.48 2.92 77.60 63.14 24.88 11.98
41.61 3.97 54.42 58.84 34.27 6.59
52.30 5.27 42.43 51.22 45.68 3.10
60.67 7.20 32.14 39.65 58.97 1.38
63.58 22.54 13.89 19.94 78.86 1.20

44
 Data for Solute Distribution (Tie lines)

No Volume (mL) Heavy Phase (Water Rich) Light Phase (Toluene Rich)

Toluene Water Acetone Refractive % Weight Refractive % Weight

Index (Acetone) Index (Acetone)
1 23.2 20.0 76.5 1.3621 51.7 1.3735 69.8
2 30.2 20.0 68.8 1.3574 40.8 1.3979 55.5
3 34.8 20.0 63.7 1.3544 32.7 1.3943 50.4
4 41.7 20.0 56.1 1.3531 30.1 1.4213 42.2
5 51.0 20.0 45.9 1.3494 21.4 1.4084 39.4
6 64.9 20.0 30.6 1.3443 9.6 1.4183 32.5

APPENDIX D

STEP BY STEP CALCULATION GUIDE

1. Obtain the equilibrium data from Appendix C. Draw the equilibrium data
binodal/solubility curve for toluene rich phase and water rich phase (Acetone fraction vs
Toluene fraction) on a triangular plot (Appendix E).
2. Plot the corresponding tie lines of acetone for toluene rich phase and water rich phase on
a triangular plot (refer to Appendix C).
3. Locate the each points for on a triangular plot based on:
Feed,F
Solvent ,S
Raffinate,R(refer to Table appendix A)
Extract ,E(refer to Table appendix A)
Feed and solvent mixture,M

45
4. Locate the point ΔR,where all operating lines should meet.

5. Draw a tie line from point E to its equilibrium point on the bimodal plot. Connect an
operating line from that equilibrium end of the tie line to point ΔR. Extend that operating
line so that it intersects with the bimodal plot at the other end. Draw another tie line from
that new intersection and continue until a tie line has passed the operating line connecting
R and S.

46
6. Count the number of tie lines contained inside the E-F-R-S quadrilateral(it may not be a
rounded number).That will be the number of required theoretical stage to achieve final
raffinate and extract compositions.

APPENDIX E

47
48