JULY 2017

Separation Technology CKD 20103 SA/July2017

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 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

1
Separation Technology CKD 20103 SA/July2017

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

Figure 1: Diagram of Plate and Frame Filter

2
Separation Technology CKD 20103 SA/July2017

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.

3
Separation Technology CKD 20103 SA/July2017

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.

4
Separation Technology CKD 20103 SA/July2017

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.

5
Separation Technology CKD 20103 SA/July2017

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, At 20 L Pa.s
At 50 L Pa.s
8. Density of Filtrate, At 20 L g/cm3
At 50 L g/cm3

6
Separation Technology CKD 20103 SA/July2017

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.

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

7
Separation Technology CKD 20103 SA/July2017

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)

8
Separation Technology CKD 20103 SA/July2017

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.
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.

9
Separation Technology CKD 20103 SA/July2017

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. Dont isolate cooling water until the heating has been shut down (at least 10 minutes).
13. Dont switch on the immersion heater with the level in the reboiler below the heater
elements or when the reboiler is empty.
14. Dont 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. Dont 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.
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.

10
Separation Technology CKD 20103 SA/July2017

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).
4. Collect samples from the sampling valves, V4 and V5 for every 5 minutes.
5. Observe the temperature of the Reboiler TI4. If the temperature is already 90C, 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.

11
Separation Technology CKD 20103 SA/July2017

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).

12
 Separation Technology CKD 20103 SA/July2017

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 ( 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

13
Separation Technology CKD 20103 SA/July2017

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

14
Separation Technology CKD 20103 SA/July2017

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.

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

15
Separation Technology CKD 20103 SA/July2017

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)

16
Separation Technology CKD 20103 SA/July2017

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.
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.

17
Separation Technology CKD 20103 SA/July2017

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. Dont isolate cooling water until the heating has been shut down (at least 10 minutes).
13. Dont switch on the immersion heater with the level in the reboiler below the heater
elements or when the reboiler is empty.
14. Dont 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. Dont 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.
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.

18
Separation Technology CKD 20103 SA/July2017

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).
4. Collect samples from the sampling valves, V4 and V5 for every 5 minutes.
5. Observe the temperature of the Reboiler TI4. If the temperature is already 90C, 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.

19
Separation Technology CKD 20103 SA/July2017

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).

20
 Separation Technology CKD 20103 SA/July2017

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

21
Separation Technology CKD 20103 SA/July2017

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

22
Separation Technology CKD 20103 SA/July2017

Experiment 3
Packed Column Gas Absorption

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

Operate vapourliquid 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 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.

23
Separation Technology CKD 20103 SA/July2017

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)
Soodium hydroxide (NaOH)
Phenolphthalein Indicator

b) Ancillary equipment/apparatus required:

50 ml Burette and Retort Stand
10 ml Graduated Cylinder
50 ml Pipette
250 ml Conical Flask
Beakers

24
Separation Technology CKD 20103 SA/July2017

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).
3. Ensure valves FCV1, FCV2, FCV3, FCV4, V7, V12 and V13 are closed.
4. Ensure valve V11 are open.

25
Separation Technology CKD 20103 SA/July2017

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
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.

26
Separation Technology CKD 20103 SA/July2017

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 15 minutes for the Absorption process to attain steady state
(Consult your lecturer or technician).
7. Draw 10 ml sample from the outlet valve, V12 for every 15 minutes.
8. Add 30 ml (V1) of prepared 0.01 M NaOH solution to the sample. (Consult your
lecturer or technician concerning how to prepare this solution). The volume of NaOH is
in excess to ensure that all CO2 has reacted with NaOH in the mixture.
9. Add a few drops of an indicator (Phenolphthalein) to the solution.
10. Titrate the mixture with already prepared 0.01 M HCl solution. (Consult your lecturer or
technician on how to prepare this solution).
11. Repeat the measurements every 10 minutes and carry out the titration with
FRESH samples until CONSTANT concentration of NaOH has been achieved.
12. 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.

27
Separation Technology CKD 20103 SA/July2017

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

Discuss all your results, elaborate more on the percentage of CO2 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 CO2 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

28
Separation Technology CKD 20103 SA/July2017

Experiment 4
Solid-Liquid Extraction (Leaching)

1. Objective(s)

The students should be able to:

Operate solid-liquid extraction experiment using Solid-Liquid Extraction Unit.

Analyze the sample by using density measurement to obtain gram of oil extracted from the
solid per gram of solvent.
Obtain the time when the solid-liquid extraction is nearly finish.

2. Introduction

Extraction is an important unit operation in many chemical industries. Extraction essentially is

a separation process where the raw materials undergo purification and isolation of a final useful
product. Without an efficient separation technology, raw materials would be in short supply,
more expensive and of a lower quality. In solid-liquid extraction process, one or more
components from a solid phase (or mixtures of phases) can be removed by using a liquid
(solvent) to selectively dissolve the required solute fraction.

Solid-liquid extraction can be defined as the removal of one or more components from
a solid phase (or a mixture of phases) by using a liquid to selectively dissolve the required
solute fraction. A complete extraction generally includes the following three steps:

Contact of solid with liquid and selective dissolution of one or more components of the
solid phases.
Separation of the resulting solution from the residual solid.
Separation of the solute from the solvent in the extracted solution.

Solid-liquid extraction can be used either when the extracted component is required or
to recover the solid residue. The former is generally described as Leaching while the latter is
more often associated with purification such as washing of filter cakes.

The solvent feed (solvent stream, extractant etc.) is allowed to come into intimate
contact with the solids feed (solid stream, charge etc.). The resulting solution (solute and
solvent) which leaves the plant, is described as the Overflow (effluent stream etc.) whilst the
residual solid (inerts etc.) together with entrained solution make up the Underflow.

29
Separation Technology CKD 20103 SA/July2017

Although the Overflow is generally less dense than the Underflow and so might
separate naturally in that order, this is not a pre-requisite of this description and the terms are
always applied in the sense given here, irrespective of practical aspects of the separation.

The Solid-Liquid Extraction unit (Model BP 04) is designed to operate as a fixed-bed

extractor either in a batch or continuous mode of operation. Pure solvent vapour generated in
the reboiler (B1) rises through a packed column (K1) and is condensed in a vertical water-
cooled condenser (W2) before being cooled down in a product cooler (W4). The liquid solvent
is then directed either to the collecting vessel (B3) or through the extraction vessel (B2). A pre-
heater (W3) is provided to allow for extraction processes at different solvent temperature.

Solid to be extracted is contained inside a glass container with porous bed support.
The container is then placed in the extraction vessel (B2). The solvent and extracted solute
(now in solution) from the extraction vessel may be turned to the reboiler where the solvent is
regenerated for further extraction.

The components of solid-liquid extraction unit are as shown below:

Reboiler (B1) 6 L spherical evaporator vessel made of borosilicate glass.
Electrically Safety Handling Mantel (W1), 1700W with
temperature control.
Column (K1) DN 50x1000 mm column made of borosilicate glass.
Packings: Glass Raschig rings (8 mm x 8mm).
Condenser (W2) Vertical coil heat exchanger DN50 made of borosilicate glass.
Heat transfer area: 0.3 m2
Product cooler (W4) Vertical coil heat exchanger made of borosilicate glass.
Heat transfer area: 0.03 m2
Receiver vessel (B3) 6 L spherical vessel made of borosilicate glass.
Extraction vessel (B2) 4 L cylindrical container made of borosilicate glass with porous
support for solid samples and quick closure unit.
Pre-heater (W3) 250 W cartridge heater with temperature control.

A process flow diagram for the Solid-Liquid Extraction unit is as shown in the next page.

30
Separation Technology CKD 20103 SA/July2017

Figure 1: The Solid-Liquid Extraction Unit (Model BP 04)

31
Separation Technology CKD 20103 SA/July2017

3. Chemicals and Ancillary Equipment

a) Chemicals required:
Industrial grade Ethanol (5 6 L)
Crushed raw soybean (500 g)

b) Ancillary equipment/apparatus required:

Density meter
Measuring cylinder (100 mL)
Beaker (50 mL)
Test Tube (11 test tube per group)
Dropper
Glass rod

4. Operating Instruction

4.1 Safety Consideration

1. Inspect the equipment for chemical leakages or glass breakages. Refer to
manufacturer for replacement of any defective parts.
2. The plant should be kept well ventilated while in operation in order to avoid organic
vapours and fumes.
3. Check whether the solvent in tank is appropriately filled before commencement of a
trial.
4. Sampling measurements ethanol need to be carried out quickly in order to avoid
solvent evaporation as ethanol is volatile.
5. Since flammable liquids are used, standard precautions to be taken in case of fire
should be studied before the experiment.
6. In case of any emergency, stop the ethanol flow pump and al the electrical switches.

4.2 General Start-up Procedure

1. Materials needed: Ethanol (solvent) and Crushed raw soybean (solids that containing
soybean oil as solute).
2. Ensure that all valves are initially closed. Open all vent valves V6, V7 and V9.
3. Charge the Reboiler B1 with ethanol as follows:
a) Measure and record the required amount of solvent in the reboiler.
b) Unscrew the charge port cap.
c) Carefully pour the solvent into the reboiler through the charge port.
d) Ensure the liquid level is above the vessel equator.
e) Screw back the charge port cap.

32
Separation Technology CKD 20103 SA/July2017

4. Ensure that all tubing are properly connected.

5. Run the cooling water through the Product Cooler W4 and Condenser W2.
Note : Open the Cooling Water valve V13 and keep it open throughout the experiment.
Open the valve slowly to prevent a pressure surge to the cooling system.
6. Switch on the heating system for the reboiler as follows:
a) Initially close valve V12 to allow for total reflux.
b) Switch on the main power supply on the control panel.
c) Adjust the Temperature Controller TIC-101 setpoint to a few degrees above
the boiling point of the solvent. In case of ethanol, adjust to 80oC.
d) Switch on the power to Heater W1.
e) Observe the temperature rise in the reboiler.
f) Allow the system to reach steady state at total reflux.
Note : If the column starts to flood and liquid begins to accumulate above the Reflux
Separator, temporarily switch off the Heater W1 until column conditions are back
to normal.
7. The equipment is now ready for experiment.

4.21 Charging of Fresh Solid

1. Weigh approximately 500g of the raw soybeans.

2. Charge the Extraction Vessel B2:
a) Ensure that the extraction vessel is drained of solvent.
b) Carefully remove the vessel cover and the solid container.
c) Discard any used solid in the container.
d) Fill in the container with the raw soybeans
e) Carefully place the container back into the extraction vessel.
f) Replace the extraction cover.
3. Check that the solvent feed line is properly connected to the extraction vessel.

4.22 Sampling Procedures

1. All samples should be collected in Sampling Vials with caps to avoid excessive
evaporation of solvent. The samples will be used for density measurement later.
2. Conduct effluent sampling as per following:
a) Place a sampling vial below valve V3.
b) Open valve V3 and collect approximately 50 mL of effluent in the sampling vial.
c) Close valve V3.
3. Conduct reboiler sampling as per following:
a) Place a sampling vial below valve V1.
b) Open valve V1 and collect approximately 50 mL of reboiler content in the
sampling vial. Quickly close valve V1.

33
Separation Technology CKD 20103 SA/July2017

c) Cool the sample by immersing the vial in cold water.

4. Conduct distillate sampling as per following:
a) Place a sampling vial below valve V11.
b) Open valve V11 and collect approximately 50 mL of distillate in the sampling
vial.
c) Close valve V11.

4.23 Solvent Refill in the Reboiler

1. When the solvent level in the reboiler is low, refill as necessary:

a) Switch off the Heater W1 power.
b) Allow the solvent temperature in the reboiler to drop below boiling point and
observe until the boiling has stopped.
c) Open the charge port cap and quickly refill the reboiler to minimize escape of
solvent vapour. Immediately screw back the cap.
d) Switch on the Heater W1 power.

4.3 Experiment: Batch Extraction of Soybean Oil from Raw Soybean using
Ethanol

1. Check that all valves are initially closed except vent valves V6, V7 and V9. Ensure that
the extraction vessel B2 is empty of solids.
2. Open valves V2, V5 and V12. Make sure valve V12 is fully open to obtain the maximum
solvent flow rate.
3. Allow the solvent to pass through the Product Cooler W4, Flow Indicator FI-301, Pre-
heater W3, Extraction Vessel B2 and back into Reboiler B1.
4. Monitor the solvent flow rate at the Flow Indicator FI-301. Once it is relatively constant,
close valve V12 to prevent any more solvent from entering the Extraction Vessel B2.
5. Charge fresh solid in the extraction vessel (see Section 4.2.1). Record the solids
weight.
6. Close valve V2, V5 and open valve V12. When the solvent starts to enter the extraction
vessel, immediately start the timer.
7. Allow the solvent to fill the vessel until all solids are fully immersed in the solvent. Keep
on monitoring in the solvent flow rate FI-301. Record the average flow rate value.
8. Close valve V12 to prevent more solvent from entering the extraction vessel B2. Stop
the timer and record the filling time to determine the volume of solvent in the vessel B2.
9. Reset the timer. Let the extraction process to take place for 30 minutes. In the
meantime, make sure that vessel B3 is empty by opening valve V10 and draining all
liquid. Close back valve V10.
10. Temporarily switch off the Heater W1 power to avoid flooding in the column.
11. Refill the reboiler with solvent if necessary (see Section 4.2.3).

34
Separation Technology CKD 20103 SA/July2017

12. After 30 minutes, open valves V4 and V5. Let all the effluent flow into vessel B3. Leave
for a few minutes to allow for the effluent to completely drain from the solids.
13. Measure the volume of effluent collected in the vessel B3 by using a measuring
cylinder.
14. Collect a 50 mL sample of the effluent for density measurement.
15. Record your data in the provided table.

4.31 Calibration Curve: Density of Solution vs Gram Soybean Oil/Gram

Ethanol

1. Obtain 11 test tubes; label the test tubes with A1 until A11. Total volume in each test
tube is 10 ml.
2. Prepare the mixture of pure soybean oil and ethanol to each test tube according to
volume indicated by Table 1 (see Results)
3. Stir the mixture of solution (A1 until A11) with glass rod.
4. Obtain density reading for solution in each tube using density meter.
5. Record the density reading for each tube tests at Table 1 (see Results).
6. Calculate weight/weight (w/w) soybean oil/ethanol and record at each of density
reading at Table 1 (see Results).
Note : Density of soybean oil @25oC is 0.917g/mL; density of ethanol @25oC is 0.789
g/mL.
7. By using a graph paper, plot the graph of Density of solution vs g soybean oil/g ethanol.

4.4 General Shut-Down Procedure

1. Open all vent valves V6, V7 and V9.

2. Place a container under valve V10. Open valves V4, V5, V8 and V10 to drain all liquid
from the equipment.
3. Shut-down the reboiler as follows:
a) Let the cooling water run. Switch off the Heater W1.
b) Close valve V12 for total reflux.
c) Allow the solvent in the reboiler to cool down to room temperature.
d) Empty the reboiler B1 by draining all liquid through valve V1.
4. Shut-down the cooling water flows as follows:
a) Let the cooling water run until the solvent in the reboiler has cooled down to
room temperature.
b) Close valve V13.
5. Clean the extraction vessel B2 as follows:
a) Ensure that the vessel is drained of solvent.
b) Carefully remove the vessel cover and the solids container.
c) Discard the used solid and clean the container.

35
Separation Technology CKD 20103 SA/July2017

d) Carefully place the container back into the extraction vessel.

e) Replace the extraction vessel cover.
Note : Always clean the solid container thoroughly especially the porous support, to
prevent molds from growing among the pores.

36
Separation Technology CKD 20103 SA/July2017

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

Discuss all your results. Your discussion should covers, but not limited to, on the factors
that affected efficiency of leaching process, the choice of solvent or others solvent
available and function and performance of contact time factors in this experiment.
By using provided formula, please complete the following table and construct a calibration
curve.

Table 1
Test Volume of Pure Volume of Ethanol Density g soybean oil/
tube Soybean Oil (mL) (mL) (g/mL) g ethanol
A1 0 10
A2 1 9
A3 2 8
A4 3 7
A5 4 6
A6 5 5
A7 6 4
A8 7 3
A9 8 2
A10 9 1
A11 10 0

By referring to a calibration curve, determine solute composition and amount of solute

(Table 2).
Table 2

Mass of soybean : ___________kg

Solvent Flow Rate : ___________mL/min
Solvent Feed Temperature : _________ oC

Solvent Effluent
Contact

Solute Amount of
Time

Filling

Density composition solute

(min)
Time

Volume
Volume (L) (g/mL) (g soybean oil/g (g)
(L)
ethanol)
30
min

37