Mass Transfer Operations Lab Manual PDF

MASS TRANSFER
OPERATIONS LAB
(ChE-306L)
Lab Incharge:
Ms. Kanwal Shabbir
Graduate Assistant:
Engr. Anees Ahmad
Department of Chemical Engineering

University of Engineering and Technology, Lahore
Contents
List of Possible Hazards in M.T.O. Lab ...............................................2

The COSHH Regulations ......................................................................3
Water-Borne Infections .........................................................................4
Use of Residual Current Device as an Electrical Safety Device ..........5
Lab Note Book Rubric ..........................................................................6
Experiment Performance Rubric ...........................................................7
Equipment Status in Mass Transfer Operations Lab ..........................10
List of Consumables for Mass Transfer Operations Lab ....................12
List of Glass Wares for Mass Transfer Operations Lab .....................14
Equipment Detail Manuals ..................................................................17
Lab Manuals (Experiments) ............................................................. 104
Lab Flexes ........................................................................................ 173
Material Safety Data Sheets for Chemicals ..................................... 187
Page - 1
List of Possible Hazards in M.T.O. Lab
Following are the potential hazards and their remedies:
S. No. Potential Hazard Mitigation

Circuit breakers are installed
1 Electrical Hazard with equipment to avoid any
personal or equipment damage.
Chemical Hazards 1. Latex gloves and lab coat is
1. Acid / Alkali solutions are strongly corrosive. recommended to avoid any
2 2. Acid may splash vigorously. contact with these chemicals.
3. Organic chemicals are volatile (form vapors 2. Slow addition of acid drops
fast). in water is recommended.
Biological Hazard
Retained water in tanks of equipment may Immediate draining of tanks is
3
allow the growth of legionella Pneumophila and recommended.
other water borne microbes.
First aid kit is recommended for
4 Injury from sharp glass objects. lab.
Fire:
Fire extinguisher is
5 1. Organic vapors can cause fire.
recommended.
2. Electrical short circuit can cause fire.
1. Immediate evacuation of lab
is recommended if release is
severe.
2. Acid / Alkali must be
6 Accidental Acid or Alkali release.
neutralized with its
counterpart.
3. Spillage must be confined in
affected area only.
1. Organic chemicals should
not be kept near fire or spark.
7 Accidental contact of non-compatible chemicals.
2. Acid should not come into
contact with pure metals.
Page - 2
The COSHH Regulations
The Control of Substances Hazardous to Health Regulations (1988)
The COSHH regulations impose a duty on employers to protect employees and others
from substances used to work which may be hazardous to health. The regulations require you
to make an assessment of all operations which are liable to expose any person to hazardous
solids, liquids, dusts, vapors, gases or micro-organisms. You are also required to introduce
suitable procedures for handling these substances and keep appropriate records.
Since the equipment supplied by Armfield Limited may involve the use of substances
which can be hazardous (for example, cleaning fluids used for maintenance or chemicals used
for particular demonstrations) it is essential that the laboratory supervisor or some other person
in authority is responsible for implementing the COSHH regulations.
Part of the above regulations are to ensure that the relevant Health and Safety Data
Sheets are available for all hazardous substances used in the laboratory. Any person using a
hazardous substance must be informed of the following:
Physical data about the substance

Any hazard from fire or explosion
Any hazard to health
Appropriate First Aid treatment.
Any hazard from reaction with other substances.
How to clean/dispose of spillage.
Appropriate protective measures.
Appropriate storage and handling.
Although these regulations may not be applicable in your country, it is strongly

recommended that a similar approach is adopted for the protection of the students operating
the equipment. Local regulations must be considered.
Page - 3
Water-Borne Infections
The equipment described in this instruction manual involves the use of water which
under certain conditions can create a health hazard due to infection by harmful micro-
organisms.
For example, the microscopic bacterium called Legionella pneumophila will feed on
any scale, rust, algae or sludge in water and will breed rapidly if the temperature of water is
between 20 and 45°C. Any water containing this bacterium which is sprayed or splashed
creating air borne droplets can produce a form of pneumonia called Legionaries Disease which
is potentially fatal.
Legionella is not the only harmful micro-organism which can infect water but it serves
as a useful example of the need for cleanliness. Under the COSHH regulations, the following
precautions must be observed. Any water contained within the product must not be allowed to
stagnate, i.e. the water must be changed regularly.
Any rust, sludge, scale or algae on which micro-organisms can feed must be removed
regularly, i.e. the equipment must be cleaned regularly.
Where practicable the water should be maintained at a temperature below 20°C or

above 45°C. If this is not practicable then the water should be disinfected if it is safe and
appropriate to do so. Note that other hazards may exist in the handling of biocides used to
disinfect the water.
A scheme should be prepared for preventing or controlling the risk incorporating all of
the actions listed above.
Further details on preventing infection are contained in the publication “The Control of
Legionellosis including Legionnaries Disease”- Health and Safety Series booklet HS (G) 70.
Page - 4
Use of Residual Current Device as an Electrical Safety Device
The equipment described in this instruction manual operates from a mains voltage
electrical supply. The equipment is designed and manufactured in accordance with appropriate
regulations relating to the use of electricity. Similarly, it is assumed that regulations applying
to the operation of electrical equipment are observed by the end user.
However, it is recommended that the RESIDUAL CURRENT DEVICE (RCD)

supplied (alternatively call an EARTH LEAKAGE CIRCUIT BREAKER -ELCB) be fitted to
this equipment. If through misuse or accident the equipment becomes electrically dangerous,
an RCD will switch off the electrical supply and reduce the severity of an electric shock
received by an operator to a level which, under normal circumstances, will not cause injury to
that person.
If the electrical supply to the laboratory already incorporated an RCD, then the device
supplied with the equipment need not be used. If the electrical supply does not incorporate such
protection, then the loose RCD supplied by Armfield Ltd. Should be fitted by a competent
electrician either in the supply to the laboratory or in the supply to the individual item of
equipment.
NOTE: If any doubt exists whether the electrical supply incorporates a device then RCD
supplied should be fitted.
At least once each month, check that the RCD is operating correctly by pressing the
TEST button. The circuit breaker MUST trip when the button is pressed. Failure to trip means
that the operator is not protected and the equipment must be checked and repaired by a
competent electrician before it is used.
Page - 5
Lab Note Book Rubric
Excellent (2) Satisfactory (1) Unsatisfactory (0) Score

1. All experiments are written
All experiments are
completely and results
written completely Experiments are
Completion interpreted.
and results incomplete.
2. Graphs, tables and
interpreted.
suggestions are mentioned.
Copy is submitted
Copy is submitted at least one at the end of the Submission do not
Timely
day before oral evaluation semester within comply with the
Response
(viva). given timeline given time domain.
from lab instructor.
All experiments are concluded At least all
with correct interpretation of experiments are Objective of
Comments / results and any discrepancy in concluded with performing
Suggestions procedure or equipment is correct experiment is not
pointed out and correction interpretation of clear.
proposed. results.
1. Sources of error are correctly
identified.
Errors are not
2. Proper tools e.g. regression At least procedural
Sources of identified and
analysis is used to quantify / equipment errors
Errors reasons are
the magnitudes of errors. are identified.
unknown.
3. Effect of errors on results is
correctly interpreted.
1. A standard format is
followed for writing all
experiments.
Haphazard
Organization 2. Index of performing all
presentation
/ experiments is available at Overall neat look is
lacking any co-
Presentation the start of the notebook maintained.
ordination between
of Contents along with the date of
contents.
performing the experiment.
3. Graphs, tables are captioned
properly and attached.
Total Scores
Page - 6
Experiment Performance Rubric
Below average Unsatisfactory

Excellent (4) Good (3) Satisfactory (2) Score
(1) (0)
1. 90% at least. 1. 80% at least. 1. 75% at least. 1. Below 75%.
2. In case of 2. In case of 2. In case of 2. In case of
Attendance 100 % leaves, lab leaves, lab leaves, lab leaves, lab
work is work is work is work is not
compensated. compensated. compensated. compensated.
Always on time in Always on time in Always on time in Always on time On time in less
Punctuality 95% labs at least. 90% labs at least. 80% labs at least. in 75% labs at than 75% labs at
least. least.
1. Calibration
checks of
equipment.
1. Calibration
2. Rinsing and
checks of
washing of 1. Rinsing and
equipment.
apparatus. washing of No
Pre- 2. Rinsing and Clear
3. Clear apparatus. understanding of
Experiment washing of procedural
procedural 2. Clear any experimental
Activities apparatus. understanding.
understanding. procedural activities.
3. Clear
4. Preparation of understanding.
procedural
solutions /
understanding.
chemicals /
accessories for
experiment.
Active
participation in: Active
participation in:
1. Keeping
Active
workplace 1. Keeping
participation in:
clean. workplace Active
2. Collection of clean. participation in: No active
1. Keeping
Participation data. 2. Collection of participation in
workplace
3. Proper data. 1. Collection lab activities.
clean.
handling of 3. Proper of data.
2. Collection of
equipment / handling of
data.
chemicals. equipment /
4. Cooperating chemicals.
with team
members.
1. Proper cleaning 1. Proper cleaning
/ washing of / washing of 1. Proper
items. items. cleaning / Proper cleaning No participation
Post 2. Safekeeping of 2. Safekeeping of washing of / washing of in post
Experiment items and items and items. items. experiment
Activities accessories. accessories. 2. Safekeeping
activities.
3. Proper waste 3. Proper waste of items and
disposal of disposal of accessories.
chemical. chemical.
Page - 7
4. Proper shut
down of
equipment.
1. All possible
hazards are
evaluated.
2. Proper
1. All possible
functioning of 1. All possible
hazards are
safety hazards are
evaluated.
parameters is evaluated. All possible
2. Proper
evaluated. 2. Proper hazards are No possible
functioning of
Safety 3. PPE’s are used functioning of evaluated hazard evaluation
safety
properly. safety is done.
interlocks is
4. MSDS are interlocks is
evaluated.
consulted and evaluated.
3. PPE’s are
Lab safety form
used.
is filled
countersigned
by lab
instructor.
Result 1. Proper data is
Calculation collected from 1. Proper data is
experiment. collected from
2. Erroneous experiment. 1. Erroneous
readings / 2. Erroneous readings /
trends in data readings / trends in data All results are No results
are identified. trends in data are identified. calculated. calculated.
3. All results are are identified. 2. All results are
calculated. 3. All results are calculated.
4. Unit calculated.
consistency is
maintained.
Discussion Results are: Results are:
Results are:
on Results 1. Accurate 1. Accurate No idea has been
1. Accurate Results are
2. Precise 2. Precise built from data
2. Precise accurate.
3. Reproducible 3. Reproducible and results.
4. Presentable
Data / Results are
Data / Results are
presented in:
presented in:
1. Graphical form. Data / Results are
1. Graphical
2. Statistically presented in:
form.
analyzed e.g. 1. Graphical
2. Statistically
Graph / trend lines form Data / Results No graphical /
analyzed e.g.
Statistical regression statistically are presented in statistical
trend lines
Analysis of coefficients analyzed e.g. graphical form. manipulation of
regression
Data added. trend lines data.
coefficients
3. Errors marked regression
added.
graphically. coefficients
3. Errors marked
4. Graphs added.
graphically.
properly
captioned.
1. Objectives of 1. Objectives of 1. Objectives of Objectives of
Analytical No idea is built
experiment are experiment are experiment are experiment are
Thinking from experiment.
fully grasped. fully grasped. fully grasped. fully grasped.
Page - 8
2. Idea from 2. Idea from 2. Idea from
experiment can experiment can experiment can
be applied to be applied to be applied to
other physical other physical other physical
situations. situations. situations.
3. Any betterment 3. Any betterment
to current to current
procedure is procedure is
proposed. proposed.
4. One has
developed
theoretical
understanding
of concept.
Total Scores
Page - 9
Equipment Status in Mass Transfer Operations Lab
Max.
S. Place of
Equipment Remarks Recommendations Expected
No. Availability
Price
1. Pump is defected. 1. Repair Pump. - Rs. 2000
2. Extensive Leakages in all 2. Use Epoxy (Resin + Brandth
Rs.100
Ion Joints. Hardener) Adhesive. Road LHR.
1 Exchange 3. Need to be replaced of
3. Plastic Pipes are causing Brandth
Apparatus whole unit. Due to very Rs. 965
leakages. Road LHR.
bad condition.
4. Clumps are not present with Brandth
4. Purchase Clumps In Search
tubing and causing leakages. Road LHR.
Gas 1. Capillary Tube is damaged Abkari
1. Purchase new. Rs. 100
Diffusion at entrance. Road LHR.
2
Coefficient 2. Use Epoxy (Resin + Brandth
2. Leakages in Water Tank. Rs. 100
Apparatus Hardener) Adhesive Road LHR.
1. Boiler heater is causing Need to be Need to be
noise formation above 1. Replace Boiler Heater. inspected inspected
Continuous 100oC. thoroughly. thoroughly.
3 Distillation 2. Boiler Level Sensor is
2. Replace Level Sensor. In Search In Search
Apparatus permanently damaged.
3. Thermocouples are 3. Replacement of
In Search In Search
problematic. Thermocouples.
Batch
1. Thermocouples are
4 Distillation 1. Re-Calibration is needed. - -
inaccurate.
Apparatus
From Any
1. Solvent Pump is 1. Repair Solvent Pump
Motor, Rs. 1000
Problematic. (Repairable)
Mechanic
2. Electrodes are not working. 2. Replace Electrodes In Search In Search
Liquid-
Shahalam
Liquid
5 3. Leakages in water tanks. 3. Replace Tanks. Market In Search
Extraction
LHR.
Apparatus
4. Unidentified. (After
Need to be Need to be
4. Distillation section is not repairing all other parts of
inspected inspected
working. this equipment, the
thoroughly. thoroughly.
problem can be identified).
Page - 10
1. Column need to be
1. Extensive leakages in the Abkari
replaced due to very In Search
column. Road LHR.
Gas extensive leakages.
Absorption 2. Manometers are not 2. Replacement of Abkari
6 In Search
Column working. Manometers. Road LHR.
Apparatus 3. Packing needs to be refiled.
3. Column is chocked at a
(New packing is not - -
specific point.
required).
Shahalam
1. Weight Balance is not Rs. 500 to
1. Replace Weight Balance. Market
working. 1000
Tray Drier LHR.
7
Apparatus Need to be Need to be
2. Psychrometric Gun is 2. Replace Psychrometric
inspected inspected
Problematic. Gun.
thoroughly. thoroughly.
Fluid Bed 1. It needs to be checked from Need to be Need to be
1. Equipment is burned from
8 Dryer inside the unit. (Need an inspected inspected
inside the unit.
Apparatus expert person). thoroughly. thoroughly.
Page - 11
List of Consumables for Mass Transfer Operations Lab
S. Required Available
Chemicals Equipment Experiment
No. Quantity Quantity
1 Acetone Gas Diffusion Experiment-1 2 liter 0 liter
Sufficient
Cation Exchange Experiment-2
2 Ion Exchange 0 kg Quantity is
Resin Experiment-3
Available
Sufficient
Anion Exchange Experiment-2
3 Ion Exchange 0 kg Quantity is
Resin Experiment-3
Available
Experiment-2
4 HCl Ion Exchange 1 kg 0 kg
Experiment-3
Experiment-2
Experiment-3
Ion Exchange
Experiment-9
5 NaOH Gas Absorption 1 kg 0 kg
Experiment-10
L-L Extraction
Experiment-11
Experiment-12
Experiment-2
6 Ca(OH)2 Ion Exchange 1 kg 0 kg
Experiment-3
Experiment-2
7 Mg(OH)2 Ion Exchange 1 kg 0 kg
Experiment-3
Experiment-2
8 Distilled Water Ion Exchange 20 liter 0 liter
Experiment-3
Experiment-4
Experiment-5
Batch Distillation
9 Ethanol Experiment-6 45 liter 0 liter
Conti. Distillation
Experiment-7
Experiment-8
Experiment-9
10 CO2 Gas Gas Absorption 20 kg 0 kg
Experiment-10
11 Phenolphthalein Gas Absorption Experiment-10 200 gram 0 gram
Page - 12
L-L Extraction Experiment-11
Experiment-12
12 NaHCO3 Gas Absorption Experiment-10 1 kg 0 kg
Experiment-11
13 Propionic Acid L-L Extraction 5 liter 0 liter
Experiment-12
Experiment-11
14 Trichloroethylene L-L Extraction 20 liter 0 liter
Experiment-12
Experiment-13
15 Sand Tray Drier 5 kg 0 kg
Experiment-14
Page - 13
List of Glass Wares for Mass Transfer Operations Lab
S. Required Available
Item Equipment Experiment
No. Quantity Quantity
1 Beaker (500 ml) Ion Exchange Experiment (2, 3) 0 2
Batch Distillation
Conti. Distillation Experiment
2 Beaker (400 ml) 0 1
Gas Absorption (4,6,7,8,10,11,12)
L-L Extraction
Batch Distillation
Conti. Distillation Experiment (4, 6,
3 Beaker (250 ml) 0 4
Gas Absorption 7, 8, 10, 11, 12)
L-L Extraction
Batch Distillation
4 Beaker (100 ml) 0 6
L-L Extraction
7 Glass Stirrer Ion Exchange Experiment (2, 3) 2 0
Batch Distillation
Measuring
8 Cylinder 0 1
(500 ml)
L-L Extraction
Batch Distillation
Measuring
9 Cylinder 1 0
(250 ml)
L-L Extraction
Measuring
10 Cylinder Batch Distillation Experiment-5 0 2
(100 ml)
Measuring
11 Ion Exchange Experiment (2, 3) 0 2
Cylinder (50 ml)
Page - 14
Measuring
Cylinder (25 ml)
Batch Distillation
13 Stop Watch 2 0
Tray Drier 7, 8, 13)
Fluidized Bed Drier
Hand Held Batch Distillation Experiment (5, 6,
14 0 1
Refractometer Conti. Distillation 7, 8)
Funnel
15 Gas Absorption Experiment-9 2 0
(Small Size)
Funnel
16 L-L Extraction Experiment-11 0 3
(Medium Size)
Pyrex Bottle Ion Exchange Experiment (2, 3,
17 0 1
(1000 ml) Gas Absorption 10)
Pyrex Bottle
(500 ml)
Pyrex Bottle
(250 ml)
Pipette with Gas Absorption Experiment (10,
20 0 1
Rubber Bulb L-L Extraction 11, 12)
Gas Absorption Experiment (10,
21 Burette (50 ml) 0 2
L-L Extraction 11, 12)
Conical Flask
(500 ml)
Conical Flask Gas Absorption Experiment (10,
23 0 4
(250 ml) L-L Extraction 11, 12)
Conical
Gas Absorption Experiment (10,
24 Stoppered Flask 0 2
L-L Extraction 11, 12)
(125 ml)
Separating 2
25 L-L Extraction Experiment-11 0
Funnel (250ml) (Urgent)
Ion Exchange Experiment (2, 3, 2
26 Iron Stand 0
Gas Absorption 10, 11, 12) (Urgent)
Page - 15
L-L Extraction
Gas Diffusion
Experiment (1,
27 Thermometer Tray Drier 10 1
13, 14, 15)
Fluid Bed Drier
Page - 16
Equipment Detail Manuals
1. Gas Diffusion Coefficients Apparatus

2. Ion Exchange Apparatus
3. Batch Distillation Apparatus
4. Continuous Distillation Apparatus
5. Gas Absorption Column Apparatus
6. Liquid-Liquid Extraction Apparatus
7. Tray Drier Apparatus
8. Fluidized Bed Drier Apparatus
Page - 17
Instruction Manual
GAS DIFFUSION COEFFICIENTS APPARATUS
Page - 18
INTRODUCTION
Physical and chemical processes depend on the properties of the materials involved.
Process engineering concerns itself with the transformation and distribution of materials in
bulk. The design and operation of engineering plant to achieve the desired changes in materials
has therefore to take into account the physical and chemical properties of these materials. The
most convenient medium is the fluid state, and hence the majority of plant operations involve
gases or liquids.
One of the most important properties of fluids in such situations is diffusivity. Fluid
flow and mass transfer operations depend partially on this property and such data is always
needed in plant design.
The Gaseous Diffusion Coefficient Apparatus allows students to measure to a

reasonable degree of accuracy this property, by a well-established technique. This practical
exercise involved in this measurement allows students an introduction to handling the basic
equations of mass and momentum transfer, and is a complement to, rather than a substitute for,
the more exacting measurements made by physical chemists.
Page - 19
DIAGRAM
Page - 20
DESCRIPTION
Parts of Equipment
1) Glass Thermometer
2) Capillary Tube
3) Temperature Sensor
4) Compartment
5) Lever Operated Cock
6) Adjustable Feet
7) Cartridge Element
8) Vernier Height Gauge
9) Removable Support Stand
10) Microscope
11) Adjustable ON/OFF Temperature Controller
12) Left-Hand Switch
13) Integral Cable
14) Right Hand Mains Switch
15) Compartment
16) Float Switch
17) Flexible Tube
Brief Description
The equipment consists of an acrylic assembly which is sub-divided into two

compartments. One compartment is constructed from clear acrylic and is used as a constant
temperature water bath. The other compartment incorporates an air pump and the necessary
electrical controls for the equipment. The assembly is mounted on adjustable feet.
Water in the bath is heated by a cartridge element which is controlled by an adjustable

on/off temperature controller connected to a PTC temperature sensor mounted in the wall of
the bath. Temperature in the bath is also indicated on a glass thermometer mounted in a gland
on the top of the bath. The temperature control system is switched on by operating the left-
hand switch. A float switch in the bath disconnects the electrical supply to the cartridge element
if the water level is too low.
Page - 21
The capillary tube for the diffusion experiments is mounted in a gland on top of the
bath. Air is supplied to the capillary tube via a flexible tube connected to the air pump. The air
pump is switched on by operating the right-hand mains switch.
The height of the liquid in the capillary tube is monitored using a travelling microscope
mounted on a removable support stand which incorporates a Vernier height gauge.
The water bath is fitted with a lever operated cock to facilitate draining using a piece
of flexible tubing.
The equipment is connected to the electrical supply using the integral cable. An earth
leakage circuit breaker (RCCB) is installed at the right-hand end of the equipment to protect
the user in the event of an electrical fault. The electrical components are protected by a mains
fuse mounted at the rear of the equipment.
NOTE: The water bath will be damaged if the water temperature exceeds 80oC. Ensure that the
temperature controller is not set above 60oC in use.
Page - 22
COMMISSIONING
Fill the water bath with clean water to approximately 25mm from the top of the bath.
Insert the microscope into the holder on the support stand and clamp by tightening the finger
screw. Ensure that the eyepiece is fitted to the microscope.
Loosen the rear gland on top of the water bath and carefully insert the glass
thermometer. Tighten the gland to retain the glass thermometer but do not-overtighten.
Do not fit the fragile capillary tube at this stage as it will be necessary to clean the tube
then fill it with acetone before use. When installed, the capillary is inserted in the gland located
at the front on top of the water bath. Do not over-tighten the gland.
Connect the mains cable to the electrical supply ensuring that the voltage of the supply
is correct to suit the equipment. Switch on the Earth Leakage Circuit Breaker (ELCB) at the
right-hand end of the equipment by pressing the white lever towards the black test button. Press
the black test button and observe that the white lever disengages. Reset the white lever to the
“on” position.
NOTE: If the ELCB does not trip when the black test button is depressed DO NOT USE THE
EQUIPMENT. The ELCB must be checked by a competent electrician before the equipment
is used.
Operate the heater switch and set the temperature controller to 50oC. The temperature
controller usually indicates the current temperature of water in the bath. To display the current
set point of the controller, press the set point membrane key pad (top left). To change the set
point, press the increase (˄) or decrease (˅) key, as required, while pressing the set point key.
To avoid damage to the equipment do not set the temperature controller above 60oC. Check
that the water heats to 50oC and remains at constant temperature (±1oC).
Operate the air pump switch. Check that a stream of air is delivered at one end of the
flexible tubing. The stream of air is only low velocity a may be detected by placing the end of
the flexible tube against the cheek.
Page - 23
Instruction Manual
ION EXCHANGE APPARATUS
Page - 24
INTRODUCTION
Ion Exchange is a natural process in which ions held on the surface of a solid displace
other ions, of similar and equivalent electrical charge, from a solution in contact with the solid.
The displaced ions become attached (i.e. held by electrostatic attraction) to the surface, while
those originally on the surface go into solution. This process of exchange continues until the
relative concentration of the two types of ions, on the surface and in solution, reach an
equilibrium. The process is reversible, the direction of the exchange depending upon these
relative concentrations.
The simplest example of practical ion exchange is in the softening of water, when Ca2+
ions in the water (causing hardness) are exchanged for Na+ ions on the exchange material.
When equilibrium is reached, i.e. when the exchange capacity of the material is exhausted, it
can be regenerated by applying a concentrated solution of a sodium salt, usually sodium
chloride, to restore Na+ ions on the surface.
By the use of suitable ion exchange materials in two or more stages it is possible to
remove all dissolved salts from solution – the process of demineralization.
The ion exchange apparatus described in this manual enables both softening and
demineralization to be studied.
Besides these uses in the treatment of water supplies, ion exchange processes are also
widely employed in industry.
Page - 25
DIAGRAM
Page - 26
DESCRIPTION
Parts of Equipment
1) Two Vertical Columns

2) Manifolds at the top.
3) Manifolds at the bottom.
4) Tank
5) Pump
6) Flowmeter
7) Sliding Tube Arrangement
8) Controlled Valves
9) Conductivity Meter
10) Cell
11) Backboard
12) Joint
Brief Description
The apparatus, which is designed for experiments on both water softening and
demineralization, consists of two vertical columns of 15mm internal diameter, mounted on a
backboard containing respectively a cation exchange and an anion exchange resin. Manifolds
at the top and bottom of the columns are fitted with valves which allow flow to be controlled
through on or both columns, in an upward or downward direction.
The liquids to be passed through the columns are stored in the tank to the left of the
apparatus and applied via the pump and flowmeter. The liquids are selected by lifting and trans
versing the sliding tube arrangement at the front of the tank. After passing through the columns
they may be collected for analysis by way of lengths of tubing attached to the nozzle equipment
includes a conductivity meter connected to a cell on the outlet line to monitor the demineralized
water.
The various processes to be used in the experiments are as follows:
a. Water to be softened, which will pass downwards through the cation exchanger
only.
Page - 27
b. Water to be demineralized, which will pass downwards through the cation
exchanger and then upward through the anion exchanger.
c. Regenerated solutions (followed by distilled or demineralized water for flushing),
which are stored in separate tanks, and will pass downwards through either the
cation or the anion exchange column.
d. Water (preferably distilled or demineralized) which will pass upwards through
either column to flush out any sediment and to release any air trapped in the resin.
Page - 28
CONNECTION TO SERVICES
ELECTRICAL SUPPLY FOR VERSION W 9-A:
The equipment requires connection to a single phase, fused electrical supply. The
standard electrical supply for this equipment is 20-240V, 50Hz. Check that the voltage and
frequency of the electrical supply agree with the label attached to the supply cable on the
equipment. Connection should be made to the supply cable as follows:
GREEN/YELLOW - EARTH
BROWN - LIVE (HOT)
BLUE - NEUTRAL
FUSE RATING - 25 AMP
ELECTRICAL SUPPLY FOR VERSION W9-B:
standard electrical supply for this equipment is 120V, 60Hz. Check that the voltage and
BROWN - LIVE (HOT)
BLUE - NEUTRAL
FUSE RATING - 0.5 AMP
Page - 29
COMMISSIONING
For initial testing fill all four tanks with ordinary tap water.
1. Place backboard and tank on a firm level surface.

2. Fill tanks with ordinary tap water (1 liter approximately).
3. Connect pump supply tube to flowmeter nozzle, and effluent return
tubes to sump tank nozzle.
4. Lift selector tube and traverse along to each compartment.
5. Connect to electrical supply.
6. Check all pipe connections are secure and all valves are closed.
7. Set flowmeter to mid-position.
8. Select tank C, open valves 3 and 6. Switch on pump and check that water returns to
sump tank. Close valves.
9. Open valves 2 and 12 and check that water returns to sump tank. Close valves.
10. Open valves 2 and 10. A container will be required to catch the water (sample) from
valve 10. Close valves.
11. Open valves 3 and 9, check that water returns to sump tank. Close valves.
12. Open valves 1 and 15, check that water returns to sump tank. Close valves.
13. Open valves 2, 13 and 15, check that water returns to sump tank. Close valves.
14. Open valves 2, 13 and 16. A container will be required to catch the water (sample)
from valve 16. Close valves.
15. Open drainage valve on sump tank, ensure it operates correctly.
16. Switch on conductivity meter, check that it operates correctly.
17. Wait 10 minutes and check for leaks at base of sump tank.
Page - 30
OPERATION OF CONDUCTIVITY METER
The conductivity meter is supplied attached to the backboard of the W9. It is powered
by a 9 Volt power supply which plugs into a 3-pin socket situated at the rear of the backboard.
This supplies power to the meter via a jack plug plugged into the top of the unit.
Connections for the conductivity probe run up the side of the W9. The 2 black
banana plugs are plugged into the left-hand set of banana sockets.
To operate the conductivity meter, switch the left-hand switch to [XI]. Switch the
right-hand switch to [x10-2] (fully anti-clockwise) and increase the sensitivity of the meter by
switching clockwise until a reading is obtained. Multiply the reading by the switch positions
indication which will produce the correct conductivity of the solution.
Page - 31
Instruction Manual
BATCH DISTILLATION APPARATUS
Page - 32
INTRODUCTION
Distillation has always been and will continue to be one of the most important industrial
processes for separating the different components of a liquid mixture. Laboratory scale
distillation columns are needed to provide adequate practical training for student engineers and
plant operators in a safe environment. They may also be used to acquire process separation
data, of use in full-scale plant design.
Traditionally, large scale "pilot plant" has been used for this purpose and that has
presented problems particularly those of large volumes of chemicals required and long time
periods to reach equilibrium. Also, restrictions in the chemicals used due to their inflammable
nature have limited the use of the equipment.
The batch distillation column has been developed specifically to overcome these main
disadvantages and present training equipment which is both economical and safe to use. Almost
all of the well documented binary mixtures are flammable and this has dictated the design of
the electrical equipment used. The flameproof electrical equipment specification used complies
with relevant British Standards for equipment being used in a Zone 1 area. This is the area
within the framework of the process where "an explosive gas – air mixture is likely to occur in
normal operation".
An area extending for 2m around and above the equipment is a Zone 2 area where no
non-flameproof electrical equipment can be used and the control console is attached to the
process by a suitable length of cable to allow it to be positioned outside this area. A variety of
batch distillation experiments can be carried out using packed or sieve plate columns and the
process can be operated at atmospheric pressure or under vacuum.
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DIAGRAMS
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DESCRIPTION
Parts of Equipment
1) Steel Framework
2) Adjustable Feet
3) Glass Section-1
4) Glass Section-2
5) Condenser
6) Top Product Tank
7) Decanter Vessel
8) Reflux Ratio Control Valve
9) Reboiler
10) Level Sensor
11) Sight Glass
12) Vacuum Pump
13) Filler Plug
14) Hose Nozzle
15) Vacuum Pump
16) Overflow
17) Underflow
Nomenclature
V1 to V15 = Valves
T1 to T13 = Thermocouples
P1 = Pressure Gauge
D = Plate
E = Central Support Rod
F = Weir
G = Downcomer
H = U-Tube
PRV1 = Pressure Relief Valve
FI1 = Rotameter
Page - 37
Brief Description
The equipment is mounted on a floor standing, welded tubular steel framework fitted
with four adjustable feet. The frame is designed to allow the use of a fork lift or pallet truck to
maneuver the unit into position initially.
The equipment comprises a 50mm diameter sieve plate column made up of two glass
sections each containing four sieve plates. The columns are separated by a central feed section
and arranged vertically for counter-current vapor / liquid flow. Also, installed within the
framework are: Reboiler, condenser, top product lank, decanter, reflux valve, vacuum pump
and all appropriate instrumentation. The reboiler situated at the base of the column is
manufactured from 316 stainless steel and incorporates a flameproof immersion type heating
element.
For batch operation, valve (V1) remains closed so that the reboiler can be filled with
the initial charge (10 to 12 liters) of binary mixture. Valve (V1) must remain closed at all times
as it is only used on the continuous feed version of this equipment. The column and reboiler
are both insulated to minimize heat loss. A level sensor inside the reboiler protects the heating
element from overheating due to low operating level and a sight glass allows the level in the
reboiler to be observed.
The glass column incorporates a total of eight sieve plates in two sections each
containing four plates. Each plate (D) is located by a central support rod (E) and incorporates
a weir (F) and downcomer (G) to create a liquid seal between successive stages. The liquid seal
on the final plate in each section is achieved by U-tube (H).
Vapor from the top of the column passes to a water-cooled, coil-in-shell condenser
which can be insulated to allow heat balances to be carried out. (The insulated jacket should
not be fitted to the condenser for normal operation.) The shell of the condenser incorporates a
pressure relief valve (PRV1) to protect the system in the event of a blocked vent and cooling
water failure. Cooling water enters the condenser at a regulated rate through a rotameter (FI1)
and the flowrate is controlled by diaphragm valve (V5). A cooling water supply is connected
to the inlet nozzle and serves also to operate the vacuum pump when operation at reduced
pressure is required. Water supply to the vacuum pump is controlled by valve (V14).
Condensate is collected in a glass decanter (phase separator) which is by-passed for

normal distillation experiments by opening valve (V10). When the decanter is in use
Page - 38
(separation of two immiscible liquids as condensate), valve (V10) is closed so that the overflow
and underflow pipes inside the vessel, can take effect.
With valve (V10) open, condensate from the condenser outlet passes directly through
the decanter to the inlet of the reflux ratio control valve which is a 3-way solenoid operated
valve. Depending on the setting of the reflux timers, condensate is directed by the reflux valve
either back to the top of the column or to the top product collecting vessel. When directed to
the column, the reflux passes through a U-seal where a valve (V3) can be used for measuring
boil-up rate or for draining the U-seal. The contents of the top product tank can be drained into
the reboiler for re-use via valve (V12).
Temperatures within the system are monitored by thirteen thermocouple sensors (T1 to
T13) located at strategic positions in the system. T1 to T8 are located in the column and
measure, the temperature of the liquid on each sieve plate.
The total pressure drop across the column is indicated on a U-tube manometer (deltaP1)
via appropriate tapings in the column fitted with isolating valves (V6) and (V7). All of the
vessels in the system are connected to a common vent on the top product receiver. This vent is
normally connected through a 4.0m length of tubing to a fume cupboard or safe atmospheric
vent outlet.
Operation at reduced system pressures is achieved using the water powered vacuum
pump. When in use, the flexible vent pipe from the common connection on the top product
receiver is attached to the inlet of this vacuum pump at, and motive water admitted via valve
(V14). The level of vacuum is adjusted using needle valve (V15) and is indicated on pressure
gauge (P1).
Control Console
The individual sections of the console are described in this article on the next page. The
console is attached to the process unit by an umbilical cable which is of adequate length to
allow the console to be positioned at least 2.0m away (outside the "Zone 2" area).
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Page - 41
Page - 42
ELECTRICAL SUPPLY FOR VERSION-A:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
ELECTRICAL SUPPLY FOR VERSION-B:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Page - 43
COMMISSIONING
The following procedure is intended as a series of checks to ensure that the equipment
is operating correctly. Water is used in place of organic solvents for safety purposes.
1. Switch on electrical power to the control console. This is achieved by moving the ELCB
switch to the UP position. The LOW-LEVEL lamp in the reboiler heater section of the
console will be illuminated. The reboiler power, reflux timer, column temperature and
process temperature digital display will also be illuminated.
2. Ensure that all valves (V1 to V15) are in the closed position. Valves included are V1,
V2, V3, V4, V5, V6, V7, V10, Vl2, V14 and V15. For normal operation ensure that the
insulated jacket has been removed from the shell of the condenser.
3. Remove the filler plug from the top of the reboiler and, using a suitable funnel, fill the
reboiler with 10 liters of water. The LOW-LEVEL lamp will go out. The reboiler level
switch operation should be tested by draining water from the reboiler using drain valve
(V2) and refilling through the filler cap.
4. Turn on laboratory cold water supply. Open flow control valve (V5) to give maximum
flow into the condenser via flowmeter (FI1). Check for leaks.
5. To prime the U-lube manometer (deltaP1), disconnect the black Viton tubing at the
valves (V6) and (V7). Using a suitable syringe filled with clean water, inject the water
into the manometer. It is advisable to hold one end of the Viton tubing of valve (V7)
vertically, insert the syringe and very slowly inject the water so that it flows down the
inside wall of the tube. This will prevent slugs of water causing air locks in the tube.
Fill the manometer tube until an equal level is visible about halfway up the scale, close
valves (V6) and (V7).
6. Switch on reboiler heater power at the console and adjust power to the heater to 1.50
kW. The water in the reboiler will begin to heat up and this can be observed by selecting
(T9) on the process temperature digital display.
7. As the water begins to boil, vapor will rise up the distillation column and this can be
observed on the top plate of each of the two column sections as the insulation has been
cut away in this area for this purpose. Turn the heater power down to 1.00 kW.
Eventually vapor will reach the condenser and drops of condensate will be
observed entering the glass decanter vessel. Allow water condensate to build up in the
Page - 44
decanter vessel until it reaches the adjustable overflow and observe the condensate
overflowing to the top product receiver vessel.
8. The reflux valve, when in the de-energized state (reflux control switch on the console
is in the OFF position), will direct all condensate back to the top of the column as reflux.
Open valve (V10) at the base of the decanter and observe condensate flowing to the top
of the column via the reflux valve. When a proportion of the condensate is required to
be directed to the top product receiver vessel, it is necessary to set the reflux timer to
give the ratio required. Set the timer to give 4 sec. to both column and receiver. This is
achieved by first pressing the SET button on the reflux timer three times. The flashing
digits are adjusted in turn using the (delta) button. The CY- and CY+ digits in the
bottom right of the display indicate flow of condensate back to the column and to the
top product tank respectively. Switch on the reflux control at the console. Observe
condensate being directed to the column and receiver for the set time periods.
9. Observe the flows and temperatures for several minutes and allow the equipment to
establish an equilibrium condition making slight adjustments where necessary. Ensure
that all thermocouple sensors are giving sensible readings on the digital display at the
console. In normal operation ensure that the power to the reboiler is not too high and
the flow of cooling water is sufficient to prevent loss of vapor through the vent system
(by overloading the condenser).
10. Open V6, and V7 and observing the pressure difference in the manometer. Close V6
and V7.
11. Open valve V14, allowing water to flow to the vacuum pump. After a few minutes,
observe on gauge P1 the pressure in the system begin to fall. Check for leaks. Even a
very small leak of air into the system will affect the achievable vacuum. Allow the
vacuum to reach a level of 200 mbar (-0.8 bar on P1). This should be achievable
in 30-40 minutes from the time of opening V14. Close V14 and ensure that the non-
return valve in the vacuum pump stops ingress of air and water. Break the vacuum by
opening slowly, valve V15.
12. The equipment can now be shut down and allowed to cool. Switch off heater power and
reflux valve at the console. Drain all of the water from the system using the drain valves
V2, V3, V4. It is important that all water be removed from the system as the presence
of water with a mixture of solvents will adversely affect the experiments.
Page - 45
OPERATIONAL PROCEDURES
a) Reflux Ratio Control
The reflux ratio timer on the control console is used to set the quantity and
frequency of condensate returning to the distillation column. With the timer switched
off, all of the condensate will be directed to the column (total reflux).
Example of Setting the Timer:
If the reflux ratio required is 2:1 and the total cycle required is 9 seconds:
This means that condensate will be directed by the reflux ratio valve to the
column for 6 seconds, then to the top product receiver for 3 seconds. This cycle will
then be repeated continuously until different values are inserted to the controller or until
the reflux control is switched off.
If a ratio of 4:1 is required over the same cycle time:
Condensate will be directed to the column for 7.2 seconds and to the top product
receiver for 1.8 seconds.
4 + 1 = 5; 9/5 = 1.8; 4 x 1.8 = 7.2
To set the controller:
This is achieved by first pressing the SET button on the reflux timer three times.
The flashing digits are adjusted in turn using the (delta) button. The CY- and CY+ digits
in the bottom right of the display indicate flow of condensate back to the column and
to the top product tank respectively.
b) Pressure Drop in Column
The overall pressure drop over the column can be measured using the
manometer delta P1.
Always open V6 before V7, take the pressure reading then immediately close
both valves. This will reduce the risk of contamination of the manometer water by the
hydrocarbons. Also, to prevent contamination, never open valves V6 or V7 when
flooding is occurring on the sieve plates (boil-up rate too high).
Page - 46
c) Sampling Valves
Samples for analysis can be taken from pertinent points in the system as follows:
Liquid in reboiler - V2 take care, liquid at boiling point
Condensate from condenser - V3 (reflux/ top product)
Top product receiver - V4
Note:
When using valve V3 to obtain a sample of top product or to measure boil up

rate the valve should not be fully opened to. prevent vapor from escaping. Gradually
open valve V3 until flow of reflux into the column stops but liquid is retained in the
flexible connecting pipe. Small adjustments of the valve position can be applied to
maintain the desired level in the pipe. Provided that the same level in the pipe is
maintained at the start and finish of the timing operation then the boil up rate measured
will be accurate.
d) Suitability of Test Mixtures

The following binary mixtures have been selected as the most suitable for use
with the distillation column.
Methylcyclohexane / Toluene
Toluene / Chlorobenzene
Cyclohexane / n-Heptane
Methanol / Water
Chlorobenzene / Ethylbenzene
Methanol / Ethanol
Ethanol / Water
Boiling Point oC Flash Point oC Ignition Temperature oC
Toluene 111 6 535
Ethanol 78 12 425
Cyclohexane 81 -18 259
Methylcyclohexane 101 -4 260
Chlorobenzene 132 28 637
n-Heptane 98 -4 215
Methanol 65 11 455
Ethylbenzene 136 15 431
Page - 47
Many other liquids can be used but the information above is required to ensure
that their characteristics are within the flameproof specification of the equipment.
e) Operation of the Decanter (Phase Separator)
The decanter in normal operation is used with valve (VI0) open which allows
condensate entering the vessel to flow directly to the reflux valve.
When carrying out an experiment which utilizes a third liquid component, valve
(V10) is closed and the decanter comes into operation. The condensate entering the
decanter will be made up of the miscible binary mixture plus an immiscible component.
The heavier component will separate and collect at the base of the decanter and its' level
will begin to rise. Eventually the lighter phase will overflow the fixed overflow and,
when the level is sufficiently high, the heavier phase will overflow the adjustable
overflow. The adjustable overflow will always be below the level of the fixed overflow
and when adjusted will determine the height of the interface between the light and
heavy components.
Page - 48
f) Reboiler
Heating of the liquid in the reboiler is achieved by an electrical heating element.
The maximum power of the element is 2.0 kW and this is adjustable at the control
console.
Due to the various flux requirements of the liquids which can be used in the
reboiler, the heater must always be switched on at zero power (adjustment fully anti-
clockwise). The power can then be increased carefully until boiling is achieved and fine
adjustment is carried out to cause the required activity on the sieve plates (observed on
Trays 1 and 5). Excessive power to the reboiler may cause vapor to escape from the
vent pipe due to overloading of the condenser.
NOTE:
The reboiler heater maximum power is 2.0 kW rated at a supply voltage of 240V
(120V). 2.0 kW will not be achieved if the supply voltage is low but this will not affect
the process as maximum power is rarely, if ever, required.
Page - 49
Instruction Manual
CONTINUOUS DISTILLATION APPARATUS
Page - 50
INTRODUCTION
Distillation has always been and will continue to be one of the most important industrial
processes for separating the different components of a liquid mixture. Laboratory scale
distillation columns are needed to provide adequate practical training for student engineers and
plant operators in a safe environment. They may also be used to acquire process separation
data, of use in full-scale plant design.
Considerable advances in the instrumentation and control of distillation columns have

been made in recent years, prompted by the advent of computer-linked systems supported by
software packages for handling plant operating data. There- is a consequent need for state-of-
the-art training and project equipment which reflects these advances.
The range is based on a common distillation column arrangement, which uses

flameproof components throughout. Depending on the options selected, the following
distillation processes may be demonstrated and form student practical assignments:
1. Batch or continuous operation

2. Packed or plate column operation
3. Vacuum distillation
4. Azeotropic or extractive distillation
5. Alternative feed tray locations
6. Varying the feed temperature.
An important new feature is incorporated within the plate column, whereby the
temperature on each sieve tray is measured and displayed. The Continuous Distillation Column
incorporates an electrical console which provides access to the various signals associated with
measurement and control of the process allowing a variety of control possibilities:
1. Manual operation
2. Data logging using PC or chart recorder
3. Manual control via an operator VDU using a mimic diagram
4. Direct digital control using PC
5. Use of industrial PID or programmable controllers
6. Use of customer-provided controllers
Page - 51
DIAGRAMS
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Page - 54
DESCRIPTION
Parts of Equipment
1) Tubular Steel Framework

2) Four Adjustable Feet
3) Glass Section
4) Glass Section
5) Feed Tank
6) Feed Tank
7) Peristaltic Type Feed Pump
8) Condenser
9) Bottom Product Tank
10) Top Product Tank
11) Decanter
12) Reflux Valve
13) Reboiler
14) Union
15) Bottom Product Cooler
16) Compression Union
17) Level Sensor
18) Sight Glass
19) Inlet Nozzle
20) Vacuum Pump
21) Filler Plug
22) Hose Nozzle
23) Vacuum Pump
24) Azeotropic Dosing Vessel
25) Overflow
26) Underflow
Page - 55
Nomenclature
V1 to V15 = Valves
T1 to T14 = Thermocouple Sensors
PRV1 = Pressure Relief Valve
FI1 = Rotameter
Delta P1 = U-Tube Manometer
A = Base Connection
B = Centre Connection
C = Top Connection
D = Plate
E = Central Support Rod
F = Weir
G = Downcomer
H = U-Tube
Brief Description
The equipment is mounted on a floor standing, welded tubular steel framework fitted
with four adjustable feel. The frame is designed to allow the use of a fork lift or pallet truck
to maneuver the unit into position initially.
The equipment comprises a 50mm diameter sieve plate column made up of two glass
sections and each containing four sieve plates. The columns are separated by a central feed
section and arranged vertically for countercurrent vapor / liquid flow. Also, installed within the
framework are: reboiler, two 5-liter feed tanks and, a peristaltic type feed pump, condenser,
bottom and top product tanks, decanter, reflux valve, azeotropic dosing vessel, vacuum pump
and all appropriate instrumentation.
The reboiler situated at the base of the column is manufactured from 316 stainless steel
and incorporates a flameproof immersion type heating element Either batch or continuous
distillation can be carried out using this reboiler.
Page - 56
In continuous operation, valve (V1) is open and bottom product flows from the reboiler
through the bottom product cooler to the bottom product tank. It is possible to preheat the feed
to the column by directing the feed through a spiral coil in the bottom product cooler where
heat is transferred from product leaving the reboiler at the boiling point. When feeding cold
feed directly to the column, the product from the reboiler is cooled in the bottom product cooler
by circulating cold water through the spiral coil.
For batch operation, valve (V1) remains closed so that the reboiler can be filled with
the initial charge (10 to 12 liters) of binary mixture. The column and reboiler are both insulated
to minimize heat loss. A level sensor inside the reboiler protects the heating element from
overheating due to low operating level and a sight glass allows the level in the reboiler to be
observed.
Feed mixture from either of the feed tanks is pumped by pump to the base, center or
top of the distillation column at connections (A), (B) or (C) respectively. The feed pump
incorporates a length of Viton rubber tubing. This tubing is suitable for all of the recommended
test mixtures. Where other test mixtures are being used, the suitability of this material must be
checked.
The glass column incorporates a total of eight sieve plates in two sections and each
containing four plates. Each plate (D) is located by a central support rod (E) and incorporates
a weir (F) and downcomer (C) to create a liquid seal between successive stages. The liquid seal
on the final plate in each section is achieved by U-tube (H). Vapor from the top of the column
passes to a water-cooled, coil-in-shell condenser which can be insulated to allow heat balances
to be carried out. (The insulated jacket should not be fitted to the condenser for normal
operation.) The shell of the condenser incorporates a pressure relief valve to protect the system
in the event of a blocked vent and cooling water failure. Cooling water enters the condenser at
a regulated rate through a rotameter and the flowrate is controlled by diaphragm valve (V5). A
cooling water supply is connected to the inlet nozzle and serves also to operate the vacuum
pump when operation at reduced pressure is required. Water supply to the vacuum pump is
controlled by valve.
Condensate is collected in a glass-decanter (VI ) (phase separator) which is bypassed

for normal distillation experiments by opening valve. When the decanter is in use
(demonstration of azeotropic distillation), valve (V10) is closed so that the overflow and
underflow pipes inside the vessel, can take effect. With valve (V10) open, condensate from the
Page - 57
condenser outlet passes directly through the decanter to the inlet of the reflux ratio control
valve which is a 3-way solenoid operated valve. Depending on the setting of the reflux timers,
condensate is directed by the reflux valve either back to the top of the column or to the top
product collecting vessel. When directed to the column, the reflux passes through a U-seal
where a valve (V3) can be used for measuring boil-up rate or for draining the U-seal. The
contents of the top product tank can be drained into the reboiler for re-use via valve (V12).
Temperatures within the system are monitored by fourteen thermocouple sensors (T1 to T14)
located at strategic positions in the system. T1 to T8 are located in the column and measure the
temperature of the liquid on each sieve plate. There are seventeen locations for the temperature
sensors, three of which do not have sensors installed but which can be fitted with sensors moved
from other, less relevant locations when necessary. The total pressure drop across the column
is indicated on a U-tube manometer (API) via appropriate tapings in the column fitted with
isolating valves (V6) and (V7).
All of the vessels in the system are connected to a common vent on the top product
receiver. This vent is normally connected through a 4.0m length of tubing to a fume cupboard
or safe atmospheric vent outlet. Operation at reduced system pressures is achieved using the
water powered vacuum pump. When in use, the flexible vent pipe from the common connection
on the top product receiver is attached to the inlet of this vacuum pump, and motive water
admitted via valve (V14). The level of vacuum is adjusted using needle valve (V15) and is
indicated on pressure gauge (P1). A packed column is supplied loose. This column can be fitted
in place of the sieve plate column where it is required to demonstrate the characteristics of a
packed column.
Control Console
The console is attached to the process unit by an umbilical cable which is of adequate
length to allow the console to be positioned at least 2.0m away (outside the "Zone 2" area).
The lower part of the console (beneath the control sections) contains the Zener diode barriers
which provide intrinsic safety to the thermocouple sensors and the level switch in the reboiler.
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Page - 61
Page - 62
ELECTRICAL SUPPLY FOR VERSION-A:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
ELECTRICAL SUPPLY FOR VERSION-B:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Page - 63
COMMISSIONING
The following procedure is intended as a series of checks to ensure that the equipment is
operating correctly. Water is used in place of organic solvents for safety purposes.
1. Switch on electrical power to the control console. This is achieved by moving the ELCB
switch to the UP position. The LOW-LEVEL lamp in the reboiler heater section of the
console will be illuminated. The reboiler power, reflux timer, column temperature and
process temperature digital display will also be illuminated.
2. Ensure that all valves (V1 to V15) are in the closed position. Valves included are V1,
V2, V3, V4, V5, V6, V7, V10, Vl2, V14 and V15. For normal operation ensure that the
insulated jacket has been removed from the shell of the condenser.
3. Remove the filler plug from the top of the reboiler and, using a suitable funnel, fill the
reboiler with 10 liters of water. The LOW-LEVEL lamp will go out. The reboiler level
switch operation should be tested by draining water from the reboiler using drain valve
(V2) and refilling through the filler cap.
4. Open valve (V1) and observe water flowing from the reboiler through valve (V1) and
through the bottom product cooler to the bottom product receiver. Water will continue
to flow until it reaches the overflow level in the reboiler. The LOW-LEVEL lamp
should not come back on. Close (V1) and replenish the reboiler with 6.0 liters of water.
5. Fill the feed tanks with clean water (approximately 4 liters in each).
6. Turn on laboratory cold water supply. Open flow control valve (V5) to give maximum
flow into the condenser via flowmeter (FI1). Check for leaks.
7. To prime the U-lube manometer (deltaP1), disconnect the black Viton tubing at the
valves (V6) and (V7). Using a suitable syringe filled with clean water, inject the water
into the manometer. It is advisable to hold one end of the Viton tubing of valve (V7)
vertically, insert the syringe and very slowly inject the water so that it flows down the
inside wall of the tube. This will prevent slugs of water causing air locks in the tube.
Fill the manometer tube until an equal level is visible about halfway up the scale, close
valves (V6) and (V7).
8. Switch on reboiler heater power at the console and adjust power to the heater to 1.50
kW. The water in the reboiler will begin to heat up and this can be observed by selecting
(T9) on the process temperature digital display.
Page - 64
9. As the water begins to boil, vapor will rise up the distillation column and this can be
observed on the top plate of each of the two column sections as the insulation has been
cut away in this area for this purpose. Turn the heater power down to 1.00 kW.
Eventually vapor will reach the condenser and drops of condensate will be
observed entering the glass decanter vessel. Allow water condensate to build up in the
decanter vessel until it reaches the adjustable overflow and observe the condensate
overflowing to the top product receiver vessel.
10. The reflux valve, when in the de-energized state (reflux control switch on the console
is in the OFF position), will direct all condensate back to the top of the column as reflux.
Open valve (V10) at the base of the decanter and observe condensate flowing to the top
of the column via the reflux valve. When a proportion of the condensate is required to
be directed to the top product receiver vessel, it is necessary to set the reflux timer to
give the ratio required. Set the timer to give 4 sec. to both column and receiver. This is
achieved by first pressing the SET button on the reflux timer three times. The flashing
digits are adjusted in turn using the (delta) button. The CY- and CY+ digits in the
bottom right of the display indicate flow of condensate back to the column and to the
top product tank respectively. Switch on the reflux control at the console. Observe
condensate being directed to the column and receiver for the set time periods.
11. Start the feed pump at the console after first ensuring the speed control is set to
minimum. Gradually increase the speed of the pump to graduation 4 on the dial
indicator. The pump will require calibration but, as a guide, the variable speed control
of the motor speed will give flows of 0 to 270 ml/min corresponding to 0 to 10 on the
dial control. Water will begin to flow from the feed tank to the column. The feed to the
column is set initially at the column mid-point. There are connections also for the feed
at the top and base of the column and feed can be directed to any of the eight sieve
plates if required by removing a thermocouple and replacing with the feed pipe.
12. Observe the flows and temperatures for several minutes and allow the equipment to
establish an equilibrium condition making slight adjustments where necessary. Ensure
that all thermocouple sensors are giving sensible readings on the digital display at the
console. Whenever the flow rate of reflux or feed needs to be altered, only very small
increments must be used in order not to unbalance the system. In normal operation
ensure that the power to the reboiler is not too high and the flow of cooling water is
sufficient to prevent loss of vapor through the vent system (by overloading the
condenser).
Page - 65
13. Open V6, and V7 and observing the pressure difference in the manometer. Close V6
and V7.
14. Open valve V14, allowing water to flow to the vacuum pump. After a few minutes,
observe on gauge P1 the pressure in the system begin to fall. Check for leaks. Even a
very small leak of air into the system will affect the achievable vacuum. Allow the
vacuum to reach a level of 200 mbar (-0.8 bar on P1). This should be achievable
in 30-40 minutes from the time of opening V14. Close V14 and ensure that the non-
return valve in the vacuum pump stops ingress of air and water. Break the vacuum by
opening slowly, valve V15.
15. The equipment can now be shut down and allowed to cool. Switch off heater power,
feed pump motor and reflux valve at the console. Drain all of the water from the system
using the drain valves V2, V3, V4, VI1 and by breaking the pipe connections of the
bottom product cooler (15) and the feed pump (7). It is important that all water be
removed from the system as the presence of water with a mixture of solvents will
adversely affect the experiments.
Page - 66
OPERATIONAL PROCEDURES
a) Reflux Ratio Control
The reflux ratio timer on the control console is used to set the quantity and
frequency of condensate returning to the distillation column. With the timer switched
off, all of the condensate will be directed to the column (total reflux).
Example of Setting the Timer:
If the reflux ratio required is 2:1 and the total cycle required is 9 seconds:
This means that condensate will be directed by the reflux ratio valve to the
column for 6 seconds, then to the top product receiver for 3 seconds. This cycle will
then be repeated continuously until different values are inserted to the controller or until
the reflux control is switched off.
If a ratio of 4:1 is required over the same cycle time:
Condensate will be directed to the column for 7.2 seconds and to the top product
receiver for 1.8 seconds.
4 + 1 = 5; 9/5 = 1.8; 4 x 1.8 = 7.2
To set the controller:
This is achieved by first pressing the SET button on the reflux timer three times.
The flashing digits are adjusted in turn using the (delta) button. The CY- and CY+ digits
in the bottom right of the display indicate flow of condensate back to the column and
to the top product tank respectively.
b) Pressure Drop in Column
The overall pressure drop over the column can be measured using the
manometer delta P1.
Always open V6 before V7, take the pressure reading then immediately close
both valves. This will reduce the risk of contamination of the manometer water by the
hydrocarbons. Also, to prevent contamination, never open valves V6 or V7 when
flooding is occurring on the sieve plates (boil-up rate too high).
Page - 67
c) Sampling Valves
Samples for analysis can be taken from pertinent points in the system as follows:
Feed Liquid - From feed tank
Liquid in reboiler - V2 take care, liquid at boiling point
Condensate from condenser - V3 (reflux/ top product)
Top product receiver - V4
Bottom product receiver - V11
Note:
When using valve V3 to obtain a sample of top product or to measure boil up

rate the valve should not be fully opened to. prevent vapor from escaping. Gradually
open valve V3 until flow of reflux into the column stops but liquid is retained in the
flexible connecting pipe. Small adjustments of the valve position can be applied to
maintain the desired level in the pipe. Provided that the same level in the pipe is
maintained at the start and finish of the timing operation then the boil up rate measured
will be accurate.
d) Suitability of Test Mixtures

The following binary mixtures have been selected as the most suitable for use
with the distillation column.
Methylcyclohexane / Toluene
Toluene / Chlorobenzene
Cyclohexane / n-Heptane
Methanol / Water
Chlorobenzene / Ethylbenzene
Methanol / Ethanol
Ethanol / Water
Boiling Point oC Flash Point oC Ignition Temperature oC
Toluene 111 6 535
Ethanol 78 12 425
Cyclohexane 81 -18 259
Methylcyclohexane 101 -4 260
Chlorobenzene 132 28 637
n-Heptane 98 -4 215
Page - 68
Methanol 65 11 455
Ethylbenzene 136 15 431
Many other liquids can be used but the information above is required to ensure
that their characteristics are within the flameproof specification of the equipment.
e) Operation of the Decanter (Phase Separator)
The decanter in normal operation is used with valve (VI0) open which allows
condensate entering the vessel to flow directly to the reflux valve.
When carrying out an experiment which utilizes a third liquid component, valve
(V10) is closed and the decanter comes into operation. The condensate entering the
decanter will be made up of the miscible binary mixture plus an immiscible component.
The heavier component will separate and collect at the base of the decanter and its' level
will begin to rise. Eventually the lighter phase will overflow the fixed overflow and,
when the level is sufficiently high, the heavier phase will overflow the adjustable
overflow. The adjustable overflow will always be below the level of the fixed overflow
and when adjusted will determine the height of the interface between the light and
heavy components.
Page - 69
f) Reboiler
Heating of the liquid in the reboiler is achieved by an electrical heating element.
The maximum power of the element is 2.0 kW and this is adjustable at the control
console.
Due to the various flux requirements of the liquids which can be used in the
reboiler, the heater must always be switched on at zero power (adjustment fully anti-
clockwise). The power can then be increased carefully until boiling is achieved and fine
adjustment is carried out to cause the required activity on the sieve plates (observed on
Trays 1 and 5). Excessive power to the reboiler may cause vapor to escape from the
vent pipe due to overloading of the condenser.
NOTE:
The reboiler heater maximum power is 2.0 kW rated at a supply voltage of 240V
(120V). 2.0 kW will not be achieved if the supply voltage is low but this will not affect
the process as maximum power is rarely, if ever, required.
Page - 70
Instruction Manual
GAS ABSORPTION COLUMN APPARATUS
Page - 71
INTRODUCTION
The packed tower, in which two fluids flowing in opposite directions enable a chemical
component to be transferred from one fluid phase to the other, occurs in almost all chemical
plants. The process may be gas absorption, distillation, solvent extraction or chemical reaction.
A knowledge of the characteristics of both fluid flow and of mass transfer in such towers is
necessary for both plant operators and designers.
The Gas Absorption Apparatus has been designed to allow these studies to be made,
and the instrumentation and layout enables students to follow both the hydrodynamic
characteristics in the absence of mass transfer, and also, separately, to advise the performance
of the mass transfer process involved in gas absorption. The size of the equipment has been
chosen so that experiments may be completed in a typical laboratory class period, while at the
same time being capable of demonstrating full scale plant behavior. Considerable attention is
directed towards matters of safety which is of crucial importance in the process industries.
Page - 72
DIAGRAM
Page - 73
DESCRIPTION
Parts of Equipment
1) Sump Tank
2) Valve in the Discharge Pipe
3) Mercury Manometers
4) Flowmeter
5) Hempl Gas Analysis Apparatus
6) Air Flow Control Valve
7) Gas Sampling Cock
8) Water Flow Control Valve
9) Flowmeter
10) Gas Flow Control Valve
11) Gas Sampling Cock
12) Air Compressor
13) Water Pump
14) Drain Cock
15) C2 Control Valve
16) C4 Outlet Valve
Brief Description
The equipment consists of a 75mm diameter column in which there are two lengths of
Raschig ring packing material. Pressure tapings are provided at the base, center and top of the
column to determine pressure drops across the column. Sampling points are also provided for
the gas at the same three points. The liquid outlet stream and feed solution are also equipped
with sampling points. Suitable manometric measurement is included. Water is taken from a
sump tank, and pumped to the column via a calibrated flowmeter. Gas is taken from a pressure
cylinder through a calibrated flowmeter, and mixed with air supplied and monitored from a
small compressor in a pre-determined (but variable) mixed ratio. The mixture is fed to the base
of the tower in which a liquid seal is provided. The effluent gas leaves the top of the column
and is intended to be exhausted to atmosphere outside the laboratory building. The apparatus
Page - 74
is designed to absorb carbon dioxide/air mixture into an aqueous solution flowing down the
column. Gas analysis apparatus is provided for this system.
Diluted ammonia may be used as alternative to carbon dioxide but this is not
recommended unless safe operating/disposal procedures are adopted.
STANDARD ELECTRICAL SUPPLY
The equipment requires connection to a 0.6kW, single phase fused electrical supply.
The standard electrical supply for this equipment is 220/240V, 50Hz. Check that the voltage
and frequency of the electrical supply agree with the label attached to the supply cable on the
BROWN - LIVE (HOT)
BLUE - NEUTRAL
FUSE RATING - 7 amp
NON-STANDARD ELECTRICAL SUPPLY
When supplied for operation from a non-standard electrical supply (110/130V, 50/60Hz
or 220V, 60Hz), the equipment incorporates a transformer of appropriate current rating. In this
case the transformer is mounted behind the sump tank. Check that the voltage and frequency
of the electrical supply agree with the label attached to the supply cable on the transformer.
Connection should be made as follows:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
FUSE RATING - 13 amp at 110/130 V
7 amp at 220V
Page - 75
COMMISSIONING
1. Fill sump tank with clean water.

2. Connect the electrical supply cable to the appropriate mains supply.
3. Prime the water and mercury manometers as appropriate.
4. Fill the Hempl gas analysis apparatus with water up to the '0' mark on the scale.
5. Connect a CO2 gas cylinder, fitted with a regulator, to the inlet regulator on the
equipment with a flexible tube, and set the cylinder regulator to minimum pressure.
6. Open fully the gas flow control valve on the gas flowmeter (small, center flowmeter)
and open the main gas cylinder valve.
7. Increase the cylinder regulator output pressure to give maximum flow on the gas
flowmeter and dose the main cylinder valve.
8. Close the air and water flow control valves. Close the gas sampling cocks on the
absorption column. Check that the valve in the discharge pipe into the sump tank is
fully open. Switch on the water pump and check that water flow is obtained through the
flowmeter and down the column on opening the control valve.
9. Switch on the air compressor and check that air flow is obtained through the flowmeter
and up the column on opening the control valve.
10. Check that the manometers indicate the pressure drop across the column (connecting
valves must be correctly set). (The water manometer range will cover all normal
situations).
11. Check that the Hempl gas analysis apparatus operates correctly by following the
instructions in the appropriate experiment sheet.
12. Close the flow control valves and switch off the pumps.
13. Drain the Hempl apparatus.
14. Drain the water seal with the small drain cock at the bottom of the “U” beneath the
column.
The equipment is now ready for use.
Page - 76
Instruction Manual
LIQUID-LIQUID EXTRACTION APPARATUS
Page - 77
INTRODUCTION
Many processes in chemical engineering require the separation of one or more of the
components of a liquid mixture by treating the mixture with an immiscible solvent in which
these components are preferentially soluble. In some cases, purification of a liquid may be the
function of the process, in others the extraction of a dissolved component for subsequent
processing may be the important aspect. An example of the former is the preparation of pure
organic liquids from products of the oil industry. Liquid-Liquid Extractions may also be used
as energy-saving processes by, for example, eliminating distillation stages. It is possible, of
course that the substance of interest may be heat-sensitive anyway and that distillation is
accordingly an unacceptable process.
The rate at which a soluble component is transferred from one solvent to another will
be dependent, amongst other things on the area of the interface between the two immiscible
liquids. Therefore, it is very advantageous for this interface to be formed by droplets and films,
the situation being analogous to that existing in packed distillation columns.
The Liquid-Liquid Extraction Unit takes the form of a vertically oriented packed
column which may be operated either, by filling the column with water and allowing a solvent
to flow down the column over the packing, or filling the column with solvent and allowing
water to flow up the column over the packing. In either case the process is continuous, both
liquids being pumped into the column. Sensing electrodes at the top and bottom of the column
determine whether the column is filled with water or with solvent. This is achieved by sensing
and maintaining the position of the water level at the appropriate height. A solenoid valve
controlling the flow of solvent under gravity from the column is operated by the sensing
electrode system. A distillation unit with a fractionating column is included to allow the
reclamation of solvent where appropriate.
Page - 78
DIAGRAMS
Page - 79
Page - 80
Page - 81
Page - 82
DESCRIPTION
Parts of Equipment
1) Stroke Adjustment Knob

2) Drain Cock
3) Solvent Supply Tank
4) Centrifugal Pump
5) Air Bleed Valve
6) Solenoid Valve
7) (Number Not Exist on Any Diagram)
8) Steel Framework
9) Extra Cross Member
11) Bottom Plate
12) Adjustable Feet
13) Stainless Steel Plate
14) End Section
15) Flanges
16) Perforated Stainless Steel Plate
17) Flow Control Valve
18) Valve
19) LLE Column (19a and 19b)
20) Distillation Column Boiler
22) Glass Section
23) Flow Control Valve
24) Flowmeter
25) End Section
26) Stainless Steel Plate
27) Pipeline
28) Injector
29) Condenser
30) Thermometer
Page - 83
31) Top Plate
32) Copper Pipes
33) Glass Reflux Divider
34) System Control Panel
35) Distillation Column
36) Receiver Vessel
37) Supply Tank
38) Valve
39) Middle Solvent Tank
40) Polythene Tank
41) Valve
42) Transformer
43) Metering Pump
Brief Description
The equipment is mounted in a floor-standing, welded steel framework fitted with

adjustable feet. The frame contains an extra cross-member at the front and a similar one at the
rear to allow the use of a fork-lift truck.
The glass liquid-liquid extraction column is fitted with enlarged end sections which are
closed by stainless steel plates, the lower one being bolted to the framework and supporting the
column. The four sections of the column proper and the two end plates are all fastened together
with flanges, the joints between the sections being sealed with moulded PTFE gaskets. The
column is filled with Raschig rings which are supported on a perforated stainless steel plate
fitted between the bottom enlarged portion and the lower section of the column.
Water for the column is stored in the supply tank (L2) from where it is pumped by the
centrifugal pump, through an air bleed valve (V3), a flow control valve (Cl) and a flowmeter
(Fl) to an injector mounted in the baseplate and with its exit about 150mm above the plate.
Water leaves the top of the column through a pipe, and is collected in a polythene tank (L1).
All storage tanks for solvent are constructed in stainless steel. The organic solvent
supply tank (L5) provides the feed for the metering pump (F2), the pumping rate of which is
varied by a stroke-adjustment knob and indicated by a digital read-out as a percentage of the
Page - 84
maximum flow (300 ml/min). Pumped solvent enters the top of the column via an injector
similar to that fitted at the base for the water. A sampling and drain cock (V6) is fitted in the
solvent feed line. Solvent from the base of the column is returned under gravity to the receiver
vessel (L3) via a pipeline which is also fitted with a solenoid valve (C3) and a sampling cock
(V9).
The Level of the water/solvent interface in the column is determined by. the operation
of the solenoid valve (C3) in the solvent outlet pipeline. The operation of this valve is controlled
by water-sensing electrodes, one set fitted to the top plate and another set to the bottom plate.
A switch (S2) on the system control panel selects the electrodes in use and hence determines
whether the interface is at the top or bottom of the column. Each electrode set consists of three
stainless steel electrodes, a bare earth electrode to make continuous contact with the water and
two others of different lengths insulated to points 5mm from their ends. These insulated
electrodes are set to heights differing by 5mm which produces a liquid level differential of
5mm.
The purpose of this arrangement is to avoid frequent opening and closing of the
solenoid valve which would occur with a simple single-electrode system. The electrical sensing
system operates at a low AC voltage and the conduction current through the water is small, the
latter being translated into a solenoid-operating voltage by a plug-in module behind the control
panel.
The receiver vessel (L3) may be connected to the solvent supply vessel via a pipeline
and a valve (V4). Thus, liquid which has passed through the column once may be treated again
in a batch wise fashion or the valve (V4) may be left open during the extraction to provide a
closed circuit, the solvent then being re-circulated continuously.
The distillation column boiler (L6), mounted behind the extraction column, is fitted at
such a height that liquid may be drained into it from the upper of the three solvent tanks and
can be drained from it into the lowest tank. The valve (V7) controls the release of solvent into
the boiler. Like pipework, valves and fittings, the boiler is constructed in stainless steel.
Heating is by means of two 500W cartridge elements inserted at the base of the boiler and
boiler temperature is indicated on a thermometer in the side. The boiler lid is perforated where
the distillation column is fitted and three blind tapped holes around this area accept bolts fixing
the column flange to the boiler.
Page - 85
The column proper is made up of a glass section containing four sieve plates. The glass
reflux divider bolts to the column top and to the stainless-steel condenser above it with bolts
and flanges and all the sections are sealed together with moulded PTFE gaskets.
The reflux divider is fitted with a thermometer (T2) to indicate the vapor temperature
beneath the divider. The condensate outlet tube and the thermometer tube on the divider are
terminated with glass screw - thread connectors and screw caps to form secure but demountable
connections. The condenser is vented to atmosphere at the top, and its jacket is water-cooled
by a supply via the copper pipes at the rear. The boiler, distillation column and condenser are
all lagged to minimize heat losses.
Condensate from the reflux divider flows under gravity into the middle solvent tank
(L4) via the flow control valve (C2) which thus determines the reflux ratio. The contents of the
middle tank (L4) can be drained into the solvent supply tank by opening the valve (V5) between
the two.
The three solvent tanks (L3), (L4), (L5) are vented to atmosphere through a vent pipe
which is inserted into the top of the condenser. Solvent levels in the tanks and boiler are
indicated with glass sight tubes protected by clear polyethylene sleeves.
Control of the equipment is simplified with a system diagram panel. The complete
solvent/water flow system is shown with electrical controls at the appropriate points on the
diagram. These are mains on/off switch (S1), water pump on/off switch (S3), solvent pump
on/off switch (S4), boiler heater switch (S5) and power regulator (R1), electrode changeover
switch (S2), and solenoid valve “open” indicator light. The four mains supply switches are self-
illuminating in the “on” position. A mains transformer is fitted when the electrical supply is
120V, 60Hz A.C.
ELECTRICAL SUPPLY FOR VERSION UOP5-A:
standard electrical supply, for this equipment is 220-240V, 50Hz. Check that the voltage and
Page - 86
BROWN - LIVE (HOT)
BLUE - NEUTRAL
FUSE RATING - 10 amp
ELECTRICAL SUPPLY FOR VERSION UOP5-B:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Note:
A transformer is fitted to this version to step up the supply voltage from 120V AC to
240V AC. The transformer is mounted on the equipment frame behind the solvent pump.
ELECTRICAL SUPPLY FOR VERSION UOP5-G:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Page - 87
COMMISSIONING
The following procedure is intended for initially checking that the equipment is
operating correctly after assembly. Water is used in place of organic solvents on the grounds
of safety.
Before proceeding with the commissioning ensure that the gearbox on the solvent pump
has been filled with oil (indicated by the presence of oil half way up the sight gauge on the side
of the gearbox).
1. Close all valves on the equipment - including drain valves. Check longest and middle
electrodes at top of extraction column, and shortest and middle electrodes at bottom of
column are approximately 5mm apart. Adjust if necessary.
2. Fill tank L2 with tap water.
3. Connect the equipment to the electrical supply.
4. Set electrode switch to top position (switch S2). Operate mains switch S1 - check S3,
S4 and S5 are 'OFF' and S1 is illuminated. Check solenoid valve C3 is open (light on).
Set the electrode switch to bottom position then check that solenoid valve C3 is still
open (light on).
5. Open vent valve V3 then switch on water pump (switch S3). Allow water pump to
prime (water discharges at V3), then close vent valve V3.
6. Open control valve C1. Check flow of water on flowmeter FI. Check water is delivered
to injector at base of extraction column.
7. Allow column to start filling with water at a slow rate. The solenoid valve C3 will be
open (light on) until water covers the short electrode when C3 will close (light off).
Open the drain valve (V11) at the base of the extraction column and drain water until
the tip of the short electrode is exposed and the valve will again open.
8. Close drain valve (V11) in base of column. Open control valve Cl and adjust to give
full scale reading on flowmeter F1. C3 will close again when the water level reaches
the short electrode then the column will gradually fill. Leave the electrode switch in the
down position. Check C3 is still closed (light off). Wait for water level to reach the top
plate i.e. column completely full. Make sure water flows from the top of the column to
the polythene storage tank (L1).
9. Switch S2 to top electrodes position. Check C3 remains closed. Close the flowmeter
control valve Cl. Open the drain valve V11 at the base of the column and allow water
Page - 88
to drain until the water level falls below the long electrode. Check valve C3 opens (light
on). Water will drain into tank L3 until level in column equals level in tank L3.
10. Check pipework and column for leaks.
11. Switch off water pump (switch S3). Drain all remaining water from column through
drain valve V11 in base of column.
12. Fill vessel L3 with tap water through top filler. Check sight gauge on L3 operates.
13. Half fill vessel L4 with tap water through top filler. Check sight gauge on L4 operates.
14. Open valve V7. Allow boiler L6 to l /3rd fill with water. Close valve V7. Check sight
gauge on L6 operates.
15. Open valve V4. Allow vessel L5 to fill with water - allow L3 to drain. Close valve V4.
Check, sight gauge on L5 operates.
16. Set calibration valve V8 to the column position, open bleed valve V13 at the solvent
pump discharge and place a suitable container beneath the valve to allow the water
which will discharge to be collected. Set pump delivery to 100% (F2) then switch on
solvent pump (switch S4). When water flows from bleed valve V13 close valve V13
and check that water is delivered to injector at top of extraction column. Set calibration
valve V8 to the calibrate position and check that water is delivered to the bypass. Close
calibration valve V8. Check F2 regulates delivery to extraction column. Switch off
solvent pump (switch S4). Check system for leaks. DRAIN WATER.
NOTE: Solvent pump needs to be calibrated before experiments can take place.
17. Connect cooling water to lower connection on condenser. Connect top connection on
condenser to drain.
18. Turn on cooling water supply. Check flow of water to drain. Check for leaks.
19. Set power control R1 to minimum (fully anti-clockwise). Switch on heating elements
(switch S5). Rotate power control R1 to maximum (fully clockwise). Check
temperature of water increases (Thermometer Tl). Check boiler for leaks. Allow water
to boil. When condensate collects in reflux divide open control valve C2. Check water
flows from reflux divider to vessel L4.
20. Set power control R1 to minimum (fully anti-clockwise) then drain the boiler by
opening valve V10. When the level falls below the level switch power should be
disconnected (S5 not illuminated). Switch off the boiler (S5).
21. Disconnect the electrical supply, turn off cooling water and drain all water from the
equipment.
Page - 89
Instruction Manual
TRAY DRIER APPARATUS
Page - 90
INTRODUCTION
A large number of manufacturing processes necessitate the drying of a product or

material and the equipment used in these industrial operations depends on the particular process
and type of material being dried. For example, the requirements for food processing are more
stringent than for agricultural fertilizer materials, and the design of driers for these purposes
will be dictated by the relative importance of such factors as heat sensitivity, porosity, bulk
density and particle size of the dried material. In fact, since the dried solid is generally a
valuable product, its shape, color, stability, stickiness and hence its overall sale ability, all
depend upon the drying processes to which it has been subjected.
Although there are many different types and operating characteristics of industrial
driers, the Tray Drier has been designed to provide an experimental facility based on one of
the most fundamental designs. Drying involves the transfer of liquid from a wet solid to an
unsaturated gas phase such as air, and the solid itself can exert a considerable influence on the
drying process. The Tray Drier enables the basic principles of drying to be investigated and
students of process engineering may examine the problems of fluid mechanics, surface
chemistry, solid structure and mass and heat transfer associated with general drying behavior.
Page - 91
DIAGRAMS
FIGURE-A
Page - 92
FIGURE-B
Page - 93
DESCRIPTION
Parts of Equipment
For Figure-A
1) Heating Section of the Tunnel

2) Drying Section of the Tunnel
3) Weight Balance
4) Four Sample Trays
5) Tray Support
6) Support Legs
7) Aspirated Psychrometer
8) (Unknown on Figure)
9) (Number Not Present on Figure)
10) Balance Clamp
For Figure-B
1) Aspirated Psychrometer
2) Psychrometer Bracket
3) Plug
4) Switch
5) Speed Control Knob
6) Switch
7) Power Control Knob
8) Fan
9) Aperture Upstream
11) Digital Balance
13) Tunnel Access Door
14) Sample Trays
15) Aperture Downstream
Page - 94
Brief Description
The apparatus comprises of an air duct mounted on a floor standing frame to give a
comfortable working height for the operator. Air is drawn into the duct through a mesh guard
by a motor driven axial flow fan impeller whose speed can be controlled to produce a range of
air velocities up to 1.5 m/s in the duct. The air passes over an electrically heated element
controlled by a power regulator to provide a variation in air temperature up to a maximum of
80°C at low air velocities.
The air passes into the central section of the duct where four trays of material to be
dried are suspended in the air stream. The trays are carried on a support frame which is attached
to a digital balance mounted above the duct and on which the total weight is continuously
indicated. The trays are inserted or removed from the duct, through a latched side door with a
glass panel for viewing purposes.
After passing over the drying trays, the air is discharged at atmosphere through an outlet
duct section where a vane anemometer, with resolution counter for measurement of air velocity,
can be positioned.
Wet and dry bulb temperatures of the air are measured using an aspirated psychrometer
which is powered from a socket outlet on the control panel mounted on the duct. Access points
for the psychrometer are provided both upstream and downstream of the drying trays and are
covered by flaps when not in use.
Page - 95
ELECTRICAL SUPPLY FOR VERSION UOP8-A:
The equipment requires connection to a single phase fused electrical supply. The
standard electrical supply for this equipment is 220/240V, 50Hz. Check that the voltage and
BROWN - LIVE (HOT)
BLUE - NEUTRAL
ELECTRICAL SUPPLY FOR VERSION UOP8-B:
When supplied for operation from a non-standard electrical supply (120V, 60Hz), the
equipment incorporates a transformer of appropriate current rating. In this case the transformer
is attached to the left-hand leg of the drier. An in-line connector is provided to connect the drier
to the transformer.
Check that the voltage and frequency of the electrical supply agree with the label
attached to the supply cable on the equipment. Connection should be made as follows:
BROWN - LIVE (HOT)
BLUE - NEUTRAL
ELECTRICAL SUPPLY FOR VERSION UOP8-G:
The equipment requires connection to a single phase fused electrical supply. The
standard electrical supply for this equipment is 220/240V, 60Hz. Check that the voltage and
BROWN - LIVE (HOT)
BLUE - NEUTRAL
Page - 96
COMMISSIONING
1. Connect the equipment to the electrical supply. Check switches are in the OFF position.
Check that the power supply, for the digital balance is connected and plugged into the
mains outlet socket at the rear of the heating section.
2. Disconnect the aspirated psychrometer from the electrical console by removing the
plug.
3. Remove the water chamber from the handle of the aspirated psychrometer. Fill the
chamber with distilled water and replace the chamber, ensuring that the wick is
immersed.
4. Replace the psychrometer into its bracket and reconnect the plug at the electrical
console. Raise the psychrometer until the inlet duct is horizontal. Check that the
electrical fan, within the psychrometer, operates and observe that the dry and wet bulb
temperatures are indicated satisfactorily on the thermometers. Replace the
psychrometer into its bracket and check that the electrical fan switches off.
NOTE:
In normal operation, the inlet duct of the psychrometer is inserted into the tunnel
through the aperture upstream or downstream of the working section. These apertures
are shielded to prevent loss of air when the psychrometer is not in use.
5. Close the tunnel access door. Operate the fan on/off switch, rotate the fan speed control
knob clockwise and check that the fan operates.
6. With the fan operating, operate the heater on/off switch, rotate the power control knob
clockwise and check that the air is heated by the electrical elements downstream of the
fan.
NOTE:
The heating elements are thermostatically protected. In the event of overheating,
power will be cut to the elements until a normal operating temperature is attained. This
process may be speeded up by operating the fan at full speed.
7. Set the fan and heater switches to the OFF position. Depress the ON button on the
digital balance and observe the digital reading. Check operation of the tare by
depressing the tare button, the display should zero. Open the access door in the wall of
the tunnel and place a suitable weight on the sample trays. Check correct operation of
the balance. Remove the weight from the sample tray and check balance returns to
original reading.
Page - 97
NOTE:
The two hooks on the tray support are adjustable in position to allow the trays
to remain horizontal when suspended from the balance. If adjustment is necessary, it
should be carried out with the trays in position but empty. When filling the trays with
samples for drying, ensure that the filling is evenly distributed to maintain the trays in
a horizontal position.
To perform the experiments outlined in the laboratory sheets, the following will be required:
a. A supply of sand or alternative medium for drying will be required, together with sieves
for grading purposes.
b. A supply of water will be required for wetting the samples.
c. A stop watch will be required.
Page - 98
Instruction Manual
FLUIDIZED BED DRIER APPARATUS
Page - 99
INTRODUCTION
When a stream of gas is passed upwards through a bed of material at a certain velocity
the bed will first expand, then become suspended and agitated by the gas stream to form a
fluidized bed. This has the appearance of boiling liquid due to the formation of many small
bubbles-the so-called ‘bubbling fluidization’.
At higher gas velocity, larger bubbles and plugs of material are formed resulting in a
more violent type of fluidization called slugging or spouting. The optimum operating gas
velocity for bubbling fluidization lies above the minimum fluidizing velocity but below the
velocity of entrainment of the material.
If a bed of wet material is fluidized by a heated air stream, as in the laboratory batch
dryer, the conditions are ideal for drying. The very efficient contact between gas and solid
particles results in heat transfer rate causing evaporation (mass transfer) of moisture which is
carried away with the exit air.
The same principles apply for industrial fluid bed dryers-both batch and continuous
types; therefore, the laboratory fluid bed dryer can be used to assess the feasibility of different
materials for large scale fluidized drying.
Page - 100
DIAGRAM
Page - 101
DESCRIPTION
Parts of Equipment
1) Jar Containing Sold Particles Need to be Dried

2) Control Unit (Having On/Off Control and Air Pump Control and Heating Element)
Brief Description
The drier can be used with a wide range of materials including fine powders, coarse
particles, crystals, granules, even slurries or pastes (after decanting or pre-drying or by spraying
onto an initial bed of the dried material). Heat sensitive materials including foodstuffs like peas,
wheat or lentils may be dried at relatively low temperatures.
The drier is of simple, compact design, conveniently portable and easy to operate, the
only requirement being a mains power supply.
Air is drawn through a mesh filter in the base of the cabinet and blown by a centrifugal
fan over a 2kW finned electrical heater and through a stainless-steel filter gauze before being
delivered to the distributor gauze at the base of the drier body which supports the bed and
distributes the air uniformly.
The air blower is controlled by a thyristor circuit to give a smooth vibration over a wide
range of motor speeds, enabling efficient fluidization to be achieved for a variety of materials
and giving fine control of the drying temperature. Readings are selected and displayed using a
digital meter. The unit can be manually operated or interval timing can be carried out with the
timer unit, which gives a 0-10-minute timing range and an alarm facility to notify completion
of the operation.
The tube unit locks into position on the cabinet top by a simple bayonet fitting and the
base of the tube is removeable to allow replacement of the distributor gauze. A filter bag is
employed to retain any stray particles of the sample being fluidized, allowing the passage of
the exit gasses.
Page - 102
ELECTRICAL SUPPLY
FT31-A: 220-240V / Single Phase / 50Hz

FT31-B: 120V / Single Phase / 60Hz
Power Consumption: 3kW
TECHNICAL SPECIFICATIONS
Temperature Range: 20 to 100oC (±1oC)

Timer Range: 0 to 10 minutes
Max. Sample Weight 5kg
COMMISSIONING
1. Connect power plug to power source.

2. Turn on air pump to check that it is working correctly.
3. Turn on heating element to check that it is heating the air or not.
4. Apparatus is ready for experiment.
Page - 103
Lab Manuals (Experiments)
1. General Safety Precautions

2. Experiment 1
(Gas Diffusion Coefficients Apparatus)
3. Experiment 2
(Ion Exchange Apparatus)
4. Experiment 3
(Ion Exchange Apparatus)
5. Experiment 4
(Batch Distillation Apparatus)
6. Experiment 5
7. Experiment 6
8. Experiment 7
(Continuous Distillation Apparatus)
9. Experiment 8
(Continuous Distillation Apparatus)
10.Experiment 9
(Gas Absorption Apparatus)
11.Experiment 10
(Gas Absorption Apparatus)
12.Experiment 11
(Liquid-Liquid Extraction Apparatus)
13.Experiment 12
(Liquid-Liquid Extraction Apparatus)
14.Experiment 13
(Tray Drier Apparatus)
15.Experiment 14
(Tray Drier Apparatus)
16. Experiment 15
(Fluidized Bed Drier Apparatus)
Page - 104
General Safety Precautions
Precautions: (Common for all experiments)
1. Personal Safety:
 Check the proper working of residual current circuit breaker (RCCB).
 Ensure that there is no leakage of any fluid especially water to contact with
electrical supply.
 Always disconnect equipment from the electrical supply when not in use.
 Use fire extinguishers in case of fire or explosion.
 Do not smoke because flammable liquids, gases, and vapors can cause fire.
2. Equipment Safety:
 Do not exceed upper limits of operating conditions (T = Temp., P =
Pressure, F = Flowrate, S = Speed).
 Check proper working of equipment ON/OFF Circuit Breaker or Switch.
 Do not use equipment without lab attendant.
 Do not try to become a juggler with equipment but if you don’t know
anything then report and ask for it.
3. Chemical Safety:
 Drain any residual water present in the apparatus
 Do not expose flammable organic fluids with flame or spark.
 Do not eat any food in chemical laboratory because its contamination with
any dangerous chemical can cause death.
 Do not taste any chemical it can cause death.
 For dilution purposes of acids and alkalis, the acid or alkali should be added
slowly drop by drop into water while stirring. The reverse process surely
causes explosive phase change of water. (e.g. H2SO4 dilution).
 Gloves and Googles must be worn whenever there is a risk to the eyes.
 Wear lab coat.
Page - 105
Experiment 1
(GAS DIFFUSION COEFFICIENTS APPARATUS)
Objective:
To determine the diffusion coefficient of a gas by evaporation from a liquid surface.
Equipment Setup / Apparatus:
Gaseous Diffusion Coefficient Unit
Reagents:
Water, Acetone, Detergent.
Theory:
The diffusivity of the vapor of a volatile liquid in air can be conveniently determined
by WINKLEMANN’S method in which liquid is contained in a narrow diameter vertical tube,
maintained at a constant temperature, and an air stream is passed over the top of the tube to
ensure that mass transfer of the acetone will take place from the surface of the liquid to the air
stream by molecular diffusion.
Page - 106
Consult the book “TRANSPORT PHENOMENA” 2nd Ed., Section “MASS TRANSPORT”
by “R. Byron Bird” for further elaboration and derivation of relationships used in calculations.
Procedure:
1) Use detergent solution to clean the capillary tube. A weak solution of the detergent
should be injected into the tube slowly as shown below:
2) To empty the tube simply shake the tube whilst it is upside down until all detergent
solution has gone. Repeat these two steps for water as a fluid in order to remove any
detergent solution left.
3) The capillary tube can now be primed (filled) with acetone using the same procedure.
The depth of Acetone should be approximately 35mm when filled.
4) Insert the capillary tube into apparatus.
5) Connect AIR TUBE to one end of the “T” piece.
6) Adjust the object lens in such a way as to see the capillary tube meniscus.
7) Adjust the position of the viewing lens in or out of the microscope body as necessary
for clearer vision of meniscus level. (Note that when viewing the capillary tube the
image will be upside down, so that the bottom of the tube is at the top of the image.)
8) Record the level inside the capillary tube.
9) Switch on the air pump. Switch on temperature controlled water bath, adjust set point
on controller to 40oC and obtain a steady temperature.
10) After some suitable time period, approximately 45 mints record the change in level
inside the capillary tube.
11) Repeat the procedure to take at least three to four readings. At the end switch off the
apparatus.
Page - 107
Data Analysis:
(L-Lo) at time t = Reading on Vernier at time (t) - Initial reading on Vernier at (t = 0sec)
Results:
Time from commencement Change in Liquid Level 𝑡

of Experiment. (L-Lo) (𝐿 − 𝐿𝑜 )
ks (killo seconds) mm ks/mm
1) Plot
𝑡
𝑜𝑛 𝑦 𝑎𝑥𝑖𝑠
(𝐿 − 𝐿𝑜 )
(𝐿 − 𝐿𝑜 ) 𝑜𝑛 𝑥 𝑎𝑥𝑖𝑠
And determine the slope of the plot and name it “s”.
𝑦2 − 𝑦1
𝑆= =?
𝑥2 − 𝑥1
2) Use the following formulas to determine the mass diffusivity:
𝜌𝐿 𝐶𝐵𝑚
𝔇𝐴𝐵 =
𝑠(2𝑀𝐶𝐴 𝐶𝑇 )
𝑚2
𝔇𝐴𝐵 = 𝑀𝑎𝑠𝑠 𝐷𝑖𝑓𝑓𝑢𝑠𝑖𝑣𝑖𝑡𝑦 𝑜𝑓 𝐴𝑐𝑒𝑡𝑜𝑛𝑒 𝑖𝑛 𝐴𝑖𝑟 ( )
𝑠
𝑘𝑚𝑜𝑙
𝐶𝐴 = 𝑆𝑎𝑡𝑢𝑟𝑎𝑡𝑖𝑜𝑛 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑎𝑡 𝑖𝑛𝑡𝑒𝑟𝑓𝑎𝑐𝑒 ( )
𝑚3
Page - 108
𝑘𝑔
𝜌𝐿 = 𝐷𝑒𝑛𝑠𝑖𝑡𝑦 𝑜𝑓 𝑡ℎ𝑒 𝐿𝑖𝑞𝑢𝑖𝑑 (𝐴𝑐𝑒𝑡𝑜𝑛𝑒) = 790
𝑚3
(𝐶𝐵1 − 𝐶𝐵2 ) 𝑘𝑚𝑜𝑙

𝐶𝐵𝑚 = = 𝐿𝑜𝑔𝑎𝑟𝑖𝑡ℎ𝑚𝑖𝑐 𝑚𝑒𝑎𝑛 𝑚𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑣𝑎𝑝𝑜𝑢𝑟 ( 3 )
𝐶 𝑚
ln(𝐶𝐵1 )
𝐵2
𝐶𝐵1 = 𝐶𝑇
1 𝑇𝑎𝑏𝑠 𝑘𝑚𝑜𝑙
𝐶𝑇 = ( ) = 𝑇𝑜𝑡𝑎𝑙 𝑀𝑜𝑙𝑎𝑟 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 ( 3 )
𝑉𝑚 𝑇𝑎 𝑚
𝑚3
𝑉𝑚 = 22.414
𝑘𝑚𝑜𝑙
𝑇𝑎𝑏𝑠 = 273 𝐾
𝑇𝑎 = 313𝐾 = 40𝑜 𝐶 (𝑆𝑒𝑡 𝑃𝑜𝑖𝑛𝑡 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒)
𝑃𝑎 − 𝑃𝑣
𝐶𝐵2 = ( )𝐶𝑇
𝑃𝑎
𝑘𝑁
𝑃𝑎 = 101.3
𝑚2
𝑃𝑣 = 𝑉𝑎𝑝𝑜𝑟 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝑜𝑓 𝐴𝑐𝑒𝑡𝑜𝑛𝑒 = 𝑓(𝑇)
𝑘𝑁
𝐴𝑡 40𝑜 𝐶 (313𝐾) 𝑡ℎ𝑒 𝑃𝑣 = 56
𝑚2
𝑘𝑔
𝑀 = 𝑀𝑜𝑙𝑒𝑐𝑢𝑙𝑎𝑟 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐴𝑐𝑒𝑡𝑜𝑛𝑒 = 58.08
𝑘𝑚𝑜𝑙
𝑃𝑣
𝐶𝐴 = ( )𝐶𝑇
𝑃𝑎
Note:
1) To prevent the acetone from boiling do not set the temperature controller above 50oC.
2) If the experiment is performed with the water bath set to different temperatures than
40oC it will be necessary to obtain suitable values for Pv.
3) The experiment can be repeated at different temperatures and the effect of temperature
on the mass diffusivity can be study if necessary.
𝔇𝐴𝐵 = 𝑓(𝑇, 𝑃)
Page - 109
Sample Results:
A set of typical results are presented overleaf for information.
Diffusivity of Acetone in air at 40oC (313K) and atmospheric pressure (Pa = 101.3kPa) from
the following experimental data.
Time from commencement 𝑡

Liquid Level (L-Lo)
of Experiment (𝐿 − 𝐿𝑜 )
ks mm ks/mm
0.000 0.00 Undetermined Form
3.600 2.20 1.636
7.200 4.20 1.714
11.160 6.30 1.771
15.900 8.80 1.807
19.980 10.80 1.850
23.400 12.40 1.887
78.780 34.50 2.283
83.520 36.10 2.314
87.240 37.30 2.339
91.800 38.90 2.360
97.320 40.80 2.385
101.100 42.00 2.407
𝑡
Plot of (𝐿−𝐿 ) vs (𝐿 − 𝐿𝑜 ).
𝑜
t/(L-Lo) vs (L-Lo) Line

3.000
2.500
2.000
1.500
1.000
0.500
0.000
0 5 10 15 20 25 30 35 40 45
Page - 110
Sample Calculations:
Point-1: (x1, y1) = (2.200, 1.636)
Point-2: (x2, y2) = (42.000, 2.407)
𝑦2 − 𝑦1 2.407 − 1.636 𝑘𝑠 9
𝑠 7
𝑠
𝑆= = = 0.0194 = 0.0194×10 = 1.94×10
𝑥2 − 𝑥1 42.000 − 2.200 (𝑚𝑚)2 𝑚2 𝑚2
1 𝑇𝑎𝑏𝑠 1 273𝐾 𝑘𝑚𝑜𝑙

𝐶𝑇 = ( )= × = 0.0389
𝑉𝑚 𝑇𝑎 𝑚3 313𝐾 𝑚3
22.414
𝑘𝑚𝑜𝑙
𝑘𝑚𝑜𝑙
𝐶𝐵1 = 𝐶𝑇 = 0.0389
𝑚3
𝑘𝑁 𝑘𝑁
𝑃𝑎 − 𝑃𝑣 101.3 2 − 56 2
𝐶𝐵2 =( ) 𝐶𝑇 = 𝑚 𝑚 ×0.0389 𝑘𝑚𝑜𝑙 = 0.0174 𝑘𝑚𝑜𝑙
𝑃𝑎 𝑘𝑁 𝑚3 𝑚3
101.3 2
𝑚
𝑘𝑚𝑜𝑙 𝑘𝑚𝑜𝑙
(𝐶𝐵1 − 𝐶𝐵2 ) 0.0389 𝑚3 − 0.0174 𝑚3 𝑘𝑚𝑜𝑙
𝐶𝐵𝑚 = = = 0.0267
𝐶 𝑘𝑚𝑜𝑙 𝑚3
ln(𝐶𝐵1 ) 0.0389 3
𝐵2 ln( 𝑚
𝑘𝑚𝑜𝑙 )
0.0174
𝑚3
𝑘𝑁
𝑃𝑣 56 2
𝐶𝐴 = ( ) 𝐶𝑇 = 𝑚 ×0.0389 𝑘𝑚𝑜𝑙 = 0.0215 𝑘𝑚𝑜𝑙
𝑃𝑎 𝑘𝑁 𝑚3 𝑚3
101.3 2
𝑚
𝑘𝑔 𝑘𝑚𝑜𝑙
𝜌𝐿 𝐶𝐵𝑚 790 3 ×0.0267
𝑚 𝑚3
𝔇𝐴𝐵 = =
𝑠(2𝑀𝐶𝐴 𝐶𝑇 ) 1.94×107 𝑠 ×2×58.08 𝑘𝑔 ×0.0215 𝑘𝑚𝑜𝑙 ×0.0389 𝑘𝑚𝑜𝑙
2 𝑚 3
𝑘𝑚𝑜𝑙 𝑚 3 𝑚
−5
𝑚2
𝔇𝐴𝐵 = 1.12×10
𝑠
Page - 111
Experiment 2
(ION EXCHANGE APPARATUS)
Objective:
To study the demineralization of water and to determine the exchange capacities of a

hydrogen ion cation exchanger and an anion exchanger.
Ion Exchange Unit, Beaker 500 ml, Glass Stirrer.
Reagents:
Cation Exchange Resin, Anion Exchange Resin, HCl, NaOH, Test Water containing
dissolved solids, Distilled or Demineralized Water.
Page - 112
Theory: (DEMINERALIZATION)
The removal of all dissolved salts from water can be achieved by using a two-stage ion
exchange process. The water is first passed through a strong cation exchanger working on the
hydrogen ion cycle, when cations in the water are replaced by H+ ions, giving a solution of
acids. This is then passed through an anion exchanger in the hydroxyl ion form, when the acid
ions are replaced by OH- ions, which with the H+ ions, produce water.
It is often sufficient to use a weakly basic anion exchanger, which will remove all anions
except HC03- (due to dissolved carbon dioxide) and H3Si04- (due to dissolved silica).
For a higher quality product water, a strongly basic anion exchanger must be used as
the final stage, but it is generally more economical to precede this with a weakly basic anion
exchanger of high exchange capacity to remove the bulk of the anions, and a degassing tower
to release CO2 from solution. The strongly basic resin is then required only to remove silica
and any residuals of other anions which may still be present. This process can reduce total
dissolved solids to below 1mg/liter.
Demineralization can also be performed in a single stage by using a mixed bed of strong
cation and anion exchangers. The water repeatedly comes in contact with the two resins
alternately, and is ultimately of very high purity. To enable the two resins to be regenerated
with sulphuric acid and sodium hydroxide respectively, they are first stratified with an upward
flow of water, the anion resin being of lower density and therefore carried to the top. After
regeneration, the two resins are re-mixed by compressed air.
Procedure:
A. Preliminary Requirements
1) Fill cation column to a depth of 300mm with a cation exchanger resin in the
hydrogen ion form.
2) Fill anion column to a depth of 300mm with an anion exchange resin in the hydroxyl
form.
3) Fill tank A with 100ml of a 10% HCl solution.
4) Fill tank B with 100ml of a 5% NaOH solution.
5) Fill tank C with test water containing 800 to 1000 mg/liter of dissolved solids.
6) Fill tank D with distilled or demineralized water.
Page - 113
7) If tap water is used, the concentrations of the principal cations and anions, as well
as the total dissolved solids, must be determined if not already known.
8) From a knowledge of the concentrations of the main cations and anions in the water
to be used, calculate the total strength in meq/liter.
9) This will be used in calculating the exchange capacities of the two resins. The
electrical conductivity should also be measured.
B. Demineralization:
1) Select tank C, open valves 2, 13 and 15. Set flow rate to between 50 and 70 ml/min.
2) Note time at which flow is started and take conductivity readings at 5 minute
intervals.
3) At 20 minute intervals draw off samples from valve 10 and measure pH value.
4) Note the time when the conductivity of the demineralized water begins to rise, i.e.
the breakthrough point at which one of the resins has become exhausted.
5) As soon as possible after this point, take another small sample from valve no. 16
and measure its pH.
6) If this pH is higher than the values previously recorded, it indicates that the cation
exchanger has become exhausted.
7) It is advisable to confirm this by drawing one or two further samples for pH
determination.
8) The experiment should be stopped at this point, and the exchange capacity of the
cation exchanger calculated.
9) It is then possible to determine the exchange capacity of the anion exchanger in this
experiment.
10) If, on the other hand, the pH of the cation exchanger effluent continues at a low
value, the rising conductivity of the final effluent indicates that the anion exchanger
is exhausted, and its capacity can be calculated.
11) In the latter event, the exchange capacity of the cation exchanger can be determined
by continuing the flow of water through the first column only, collecting the water
which passes through it and measuring pH values until the breakthrough point,
when the pH begins to rise.
Page - 114
In all of the figures:
C. Backwashing:
1) Each column should be separately backwashed.
2) In each case, the rate of backwashing should be controlled to give not more than
50% expansion of the bed.
3) Measure the final depths of the two beds.
Page - 115
D. Cation Regeneration:
1) Regenerate the cation exchanger.
2) Select tank A, open valves 2 and 12. Follow the acid with distilled or
demineralized water from tank D, to flush out any surplus acid.
3) Check pH of effluent and continue flushing until pH has returned to above 5.0.
E. Anion Regeneration:
1) Regenerate the anion exchanger.
2) Select tank B, open valves 1 and 15, followed by distilled or demineralized water
from tank D until pH of the effluent has returned to below 9.0.
Page - 116
Data Analysis:
In the demineralization experiment, the breakthrough point is detected by readings of

pH (for the cation exchanger) or conductivity (for the anion exchanger) instead of by direct
measurement of concentrations.
Time (min) 0 5 10 15 20 25 30 35 40 45 50 55 60
Conductivity
PH Values
In order to calculate the exchange capacities in terms of milli-equivalents (meq), it is

necessary to convert pH or conductivity readings to meq/liter.
(a) To convert pH values to meq/liter.
If pH reading is “x”
Hydrogen ion concentration = 10-x moles/liter
= 103-x meq/liter
(b) To convert conductivity values to meq/liter.
For a water with a given content of salts, the electrical conductivity is closely
proportional to the concentration of total dissolved solids. Although these solids consist
of several salts of varying electrolytic properties, it is sufficiently accurate to assume
that electrical conductivity is also proportional to the the total concentration in terms of
meq/liter.
The constant of proportionality was established by determination of the
electrical conductivity and the strength of meq/liter of the raw water. Hence the
electrical conductivity of the demineralized water can be converted to meq/liter. In
any event these figures should be very low.
(c) Other Calculations
Final Depths:
CATION = _______________
ANION = _______________
Page - 117
(π×15×10−3 )2
Wet Volume = ×Final Depth
4
Exchange capacities can now be calculated.

𝑆𝑜𝑑𝑖𝑢𝑚 𝐼𝑜𝑛 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛
𝐸𝑥𝑐ℎ𝑎𝑛𝑔𝑒 𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑊𝑒𝑡 𝐵𝑒𝑑
Page - 118
Experiment 3
(ION EXCHANGE APPARATUS)
Objective:
To determine the regeneration efficiency of cation resin and an anion resin.
Ion Exchange Unit, Beaker 500 ml, Glass Stirrer.
Reagents:
Cation Exchange Resin, Anion Exchange Resin, HCl, NaOH, Test Water containing
dissolved solids, Distilled or Demineralized Water.
Page - 119
Theory: (REGENERATION)
Theoretically, for every milli-equivalent of hardness as CaCO3 removed from the water
under treatment, one milli-equivalent of NaCl is required for regeneration, i.e. l g of hardness
as CaCO3 removed requires 1.17 g NaCl for regeneration (Molecular weights: CaCO3 50.0,
NaCl 58.5).
In practice, it is not possible to achieve complete regeneration with this quantity of

NaCl, since this would require an unacceptable long contact period. Larger quantities of NaCl
are therefore used, generally twice or more the theoretical amount. Tire regeneration efficiency
is thus around 50%.
A high level of regeneration gives a resin with a high exchange capacity approaching
its theoretical, but it is uneconomic to operate at such a rate that this capacity is fully used in
softening. In other words, a high regeneration efficiency is associated with a low degree of
column utilization, and vice versa. The practical operation of an ion-exchange bed is therefore
a compromise in which the regeneration efficiency and the column utilization are both in the
region of 50% (Optimization is requires).
After regeneration, distilled or demineralized water is passed through the bed to wash
out any remaining regenerator.
Water to be treated by ion exchange must be free of suspended solids which would
block the passage-ways, reduce flow rates and interfere with the exchange process. To remove
fine solids which may get into the bed, and to release any air pockets, the column is backwashed
periodically by an upward flow of water which fluidizes the bed and agitates the resin beads.
The rate of flow of water through the bed in softening is usually not more than 40
ml/(min.cm2) of surface area of bed. Regeneration rates are about one tenth of this.
Page - 120
Procedure:
A. For Cation Resin Regeneration Efficiency

1) Fill cation column to a depth of 300mm with a cation exchanger resin in the
hydrogen ion form.
2) Fill anion column to a depth of 300mm with an anion exchange resin in the hydroxyl
form.
3) Fill tank A with 100ml of a 10% HCl solution.
4) Fill tank B with 100ml of a 5% NaOH solution.
5) Fill tank C with test water containing 800 to 1000 mg/liter of dissolved solids.
6) Fill tank D with distilled or demineralized water.
7) If tap water is used, the concentrations of the principal cations and anions, as well
as the total dissolved solids, must be determined if not already known.
8) From a knowledge of the concentrations of the main cations and anions in the
water to be used, calculate the total strength in meq/liter.
9) This will be used in calculating the regeneration efficiency of the two resins. The
electrical conductivity should also be measured.
10) Backwash: Select tank D, open valves 3 and 6.
11) Regenerate: Select tank A, open valves 2 and 10. Collect whole of the solution.
B. For Anion Resin Regeneration Efficiency

1) To determine the regeneration efficiency of the anion resin it will be necessary to
carry out the full demineralization experiment.
2) Since the exchange capacities of cation resins are generally greater than those of
anion resins, it is expected that the anion resin will be first to be exhausted.
Page - 121
Data Analysis:
Final Depths:
CATION = _______________
ANION = _______________
Sodium ion concentration (meq/ml) =
(π×15×10−3 )2
Volume of solution used (ml) = ×Final Depth
4
Exchange capacities can now be calculated.

Sodium Ion Concentration
Theoretical Exchange Capacity =
Volume of NaOH used
Original quantity of NaOH used =
Amount of NaOH collected =
Actual Exchange Capacity = Original Quantity – Amount Used
Actual Exchange Capacity

Regeneration Efficiency =
Theoretical Exchange Capacity
Page - 122
Experiment 4
(BATCH DISTILLATION APPARATUS)
Objective:
To determine the pressure, drop over the distillation column for various boil-up rates.

Batch Distillation Apparatus, Measuring Cylinder 250ml, Stop Watch
Reagents:
Ethanol, Water
Page - 123
Theory:
The total pressure drop across each tray is the sum of that caused by the restriction of
the holes in the sieve tray, and that caused by passing through the liquid (foam) on top of the
tray. As the velocity of the vapors passing up the column increases then so does the overall
pressure drop. The velocity is controlled by varying the boil-up rate which is done by varying
the power input to the reboiler. Under conditions with no liquid present, the sieve trays will
behave like an orifice in that the pressure drop will be proportional to the square of the velocity.
Due to the fact that there is a liquid head however, this square relationship does not become
apparent until the head of liquid has been overcome and foaming is taking place. In a graph of
pressure drop vs. boil up rate (log/log), at low boil-up rates the pressure drop will remain fairly
constant until foaming occurs when the pressure drop would be expected to rise sharply for
unit increases in boil-up rate.
Procedure:
1) Make 10 Liters of mixture of 50 mole percent ethanol and 50mol percent water.
Molar Mass Density

Species Formula Mole Fraction
(kg/kmole) (kg/m³)
Ethanol
(Component A)
C2H5OH 46 789 0.5
Mixture Data
Water
(Component B)
H2O 18 1000 0.5
Required Volume of Mixture = V = 10 Liters

nA nB
xA = = 0.5 xB = = 0.5
nT nT
nA = 0.5nT = 0.5CV nB = 0.5nT = 0.5CV
kg
MMixture = xA MA + xB MB = (0.5)(46) + (0.5)(18) = 32
kmole
kg
ρMixture = xA ρA + xB ρB = (0.5)(789) + (0.5)(1000) = 894.5 3
m
kg
ρMixture 894.5 3 kmole 1m3 kmole
C= = m = 27.9531 × = 0.028
MMixture kg m3 1000L L
32
kmole
kmole kmole
nA = 0.5×0.028 ×10L nB = 0.5×0.028 ×10L
L L
Page - 124
nA = 0.14 kmole nB = 0.14 kmole
kg kg
mA = 0.14 kmole×46 mB = 0.14 kmole×18
kmole kmole
mA = 6.44 kg mB = 2.52 kg
ρA 𝑉𝐴 = 6.44 kg 𝜌𝐵 𝑉𝐵 = 2.52 kg
6.44 kg 2.52 kg
𝑉𝐴 = 3 = 8.1622 𝐿 𝑉𝐵 = = 2.52 𝐿
kg 1𝑚 kg 1𝑚3
789 3 × 1000𝐿 1000 3 × 1000𝐿
m m
So, 8.1622 L of Ethanol and 2.52 L of Water are required for making 10 Liters of
Mixture of 0.5, 0.5 Mole Fraction.
2) The equipment will be set up to operate at total reflux meaning all the formed vapor
will after condensation return to the column. The charge of feed mixture can be loaded
directly in the reboiler through the filler cap provided without first charging the feed
tank. At total reflux, there will be no feed or top product or bottom product.
3) Before starting, make sure all valves on the equipment are closed. Open valve V10 on
the reflux pipe. Fill the boiler with mixture to be distilled. Make sure the filler cap on
the top of the reboiler is firmly replaced.
4) Turn on the power to the control panel. Set the temperature selector switch to T9, the
temperature in the reboiler and open valve V5 admitting the cooling water to the
condenser at a flow rate on FI1 of approximately 3 liters/ min.
5) On the control panel turn the power controller for the reboiler heating element fully
anti-clockwise and switch on the power to the heating element to "power on" position.
Another red lamp will illuminate indicating the heating element is on.
6) Turn the power controller clockwise until a reading of approximately 0.75kW is
obtained on the digital wattmeter. The contents of the reboiler will begin to warm up
and this can be observed on the temperature readout meter.
7) Open valves V6 and V7 which connect base and top of the distillation column,
respectively, to the manometer. Initially there will be no pressure difference in the
column meaning no reading on the manometer.
8) Close valve V6 and V7. The 1st and 5th plates in the column sections are not insulated
so that observation of the sieve plates are possible. Eventually, vapor will begin to rise
up the column and the progress of this can be clearly observed as well as detected by
the increasing temperatures when switching the temperature selector on T8, T7, T6, T5,
T4, T3, T2 and Tl.
9) Vapor will enter the condenser and reappear as droplets into the glass walled distillate
receiver vessel. The distillate will build up a small level in the receiver and eventually
overflow to the reflux regulator valve. Since the valve is not on (on the control pane!),
and it will not be necessary to have it on in this experiment, which is run under total
reflux, the condensate vapor will return to the column.
10) The cool distillate is then returning on the top of the column and will cascade down the
trays forming a liquid level on the trays and bubbling of vapor passing through the
liquid. The system will have reached an equilibrium condition when the temperatures
Tl, T2, T3, T4, T5, T6, T7 and T8 are constant.
11) The boil-up rate can be measured by operating valve V3 so that all the condensate is
diverted into a measuring cylinder and the time observed to collect a set quantity. This
Page - 125
will not disrupt the equilibrium conditions in the column provided a liquid level is
maintained in the condensate feeding pipe.
12) When taking a sample, partially open valve V3 and drain the condensate (in a separate
measuring cylinder) from the reflux system until a steady flow is obtained. (Ensure that
liquid remains in the flexible connecting tube to prevent vapor from escaping.)
13) Start sample collection and timing at the same time. Collect a sizeable amount
approximately 90 ml in a 100ml measuring cylinder. Pour the first non-representative
collected amount in a bottle labelled "recyclable Ethanol / Water".
14) After taking the samples, take readings of pressure drops over both the rectifying (top)
and the stripping (bottom) sections by opening the valves V6 and V7 on the manometer.
15) When opening the valves, make sure always to open valve V6 then V7 to prevent vapor
from the column entering the manometer. If this happens, it can be seen as two separate
phases in the U-tube. Close the valves in the same order, when finished the pressure
drop reading.
16) Repeat these readings until two in a row agree fairly closely. Allow 5 to 10 minutes
between each set of measurements before starting the next set in order for the system
to reach equilibrium again.
17) Step up the boil-up rate in 250 Watt increments up to maximum 1.5 kW by adjusting
the boiler heater power controller (on the control panel). Take-similar readings of the
boil-up rate and pressure drops after having allowed at least 10 minutes to let the
column stabilize.
Page - 126
Data Analysis:
Power Boil-up Rate Pressure Drop (cm Degree of Foaming on
(kW) (Liters/hr) H2O) Trays
0.50
0.75
1.00
1.25
1.50
1.75
NOTE:
The comment "Degree of Foaming on Trays" should be filled in using descriptive words
e.g.
None
Gentle Localized
Violent Localized
Foaming Gently Over Whole Tray
Foaming Violently Over Whole Tray Liquid Flooding in Column
From the results, plot the curve relating pressure drop as a function of boil-up rate on log/log
graph paper.
Result obtained will be like this:
Relate the descriptive comments observed (and noted in the table of results) to zones on the
curve.
Page - 127
Experiment 5
Objective:
Use of the refractometer for determining mixture compositions.

Batch Distillation Apparatus, Hand Held Refractometer, Measuring Cylinder 100ml
Throughout the experimental procedures carried out on the Distillation Column, it is
essential to have a convenient quick method of determining the composition of the binary
mixture taken from the various sample points on the equipment. Such a method involves the
use of a refractometer since the refractive index of these mixtures varies with composition. It
is needed to have a suitable container to mix the sample in, and a bottle of each of the pure
components of the binary mixture to be analyzed.
Reagents:
Ethanol, Water
Theory:
For the system, Ethanol / Water, mixtures of known concentration can be made up and
their refractive indexes measured. The refractometer measures the critical angle of the liquid
under test and each concentration will show a different critical angle Theta. Beyond the critical
angle is darkness and refractometers are calibrated along this light/dark boundary.
Page - 128
Procedure:
1) Measure the refractive index (R.I.) of pure Ethanol and pure Water.
2) Make up small quantities of 25 mole percent, 50 mole percent and 75 mole percent
Ethanol using the similar procedure as in previous experiment and measure their R.I.
3) Calculate the volume of constituents to use as in the previous experiment:
Data Analysis:
Mole Fraction of Ethanol Refractive Index

1.00
0.75
0.50
0.25
0.00
Plot graph of refractive index versus mole fraction of methylcyclohexane in

methylcyclohexane / toluene mixture.
General trend of this graph is shown below.
For any mixture composition of these two constituents simply measure the refractive index y
and read off the composition x.
Page - 129
Experiment 6
Objective:
To determine the overall column efficiency at varying boil-up rates.

Batch Distillation Apparatus, Hand Held Refractometer, Measuring Cylinder 250ml,
Stop Watch.
Reagents:
Ethanol, Water
Page - 130
Procedure:
1) Make 10 liters of a mixture of 50 mole percent Ethanol and 50 mole percent Water by
using the steps of solution preparation of experiment 4.
2) The equipment will be set up to operate at total reflux so the charge of feed mixture can
be loaded directly into the reboiler through the filler cap provided without first charging
the feed tanks. At total reflux, there will be no feed or top product or bottom product.
3) Start up the unit, set the heat controller high at first then reduce heat; as reflux is
introduced to give steady bubbling on all tray and total reflux. Leave the apparatus for
at least 30 minutes so that the system can reach an equilibrium condition.
4) Measure the boil-up rate as described under experiment 4 using valve V3. Do this work
three times and take an average value. Take a sample of the overheads through valve
V3. When doing that, be careful never to drain the condensate return line i.e. partially
open valve V3 to leave a small amount of liquid in the line all the time.
5) Generally, when taking samples, drain a "discarding" sample of approximately 5 to 10
ml before taking the representative sample in a small glass. Do not drain too much of
the "discarding" sample because of the disturbance of the mass balance. Discard the
"discarding" sample in safe way. After the representative sample, has been taken, keep
the sample glasses in an upright position. Do not overturn them because of the
possibility of evaporation of the sample.
6) Record the refractive index for the taken overhead sample. In a similar manner take a
sample of the bottom through valve V2. CAUTION! THIS SAMPLE WILL BE HOT,
(take note of T9). Record the refractive index for this sample, too.
7) Repeat this procedure every ten minutes until five samples of both overhead and bottom
are obtained. Record the temperatures T8 and T1 to calculate the average column
temperature.
8) Repeat this procedure for several different boil-up rates to cover over the operating
range of the column.
9) The calibration graph developed in the previous Experiment 5 can be used to determine
the concentrations of the components in the taken samples.
Data Analysis:
Boil-up rate = __________________ liters/hour.

Overhead Concentration (XA)D = a)
(Mole Percent Ethanol) b)
c)
d)
e)
Average = ________________ mole percent of Ethanol.
Bottom Concentration (XA)B = a)
b)
c)
Page - 131
d)
e)
Average Column Temperature (Top Side) = ___________ oC.
Average Column Temperature (Bottom Side) = ___________ oC.
Overall Average Colum Temperature = ___________ oC.
The curve shown in the next page shows:

Vapor-Liquid Equilibrium Data of Ethanol / Water Mixtures
To calculate the number of theoretical plates for a given separation at total reflux.
FENSKE’S METHOD
Fenske developed the following formula:
𝑥 𝑥
log[(𝑥𝐴 )𝑑 ×( 𝑥𝐵 )𝑏 ]
𝐵 𝐴
𝑛+1=
log(𝛼𝐴𝐵 )𝑎𝑣
Where:
Page - 132
𝑛 = 𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑡ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑝𝑙𝑎𝑡𝑒𝑠
𝑥𝐴 = 𝑀𝑜𝑙𝑒 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝑀𝑜𝑟𝑒 𝑉𝑜𝑙𝑎𝑡𝑖𝑙𝑒 𝐶𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
𝑥𝐵 = 𝑀𝑜𝑙𝑒 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝐿𝑒𝑠𝑠 𝑉𝑜𝑙𝑎𝑡𝑖𝑙𝑒 𝐶𝑜𝑚𝑝𝑜𝑛𝑒𝑛𝑡
𝛼𝐴𝐵,𝑎𝑣 = 𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑅𝑒𝑙𝑎𝑡𝑖𝑣𝑒 𝑉𝑜𝑙𝑎𝑡𝑖𝑙𝑖𝑡𝑦
Subscripts D, B indicate distillate and bottom respectively.
𝛼𝐴𝐵,𝑎𝑣 = √𝛼𝐷 . 𝛼𝐵
The efficiency is given by:

𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑇ℎ𝑒𝑜𝑟𝑒𝑡𝑖𝑐𝑎𝑙 𝑃𝑙𝑎𝑡𝑒𝑠
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝐸𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑐𝑦 = 𝐸 = ×100
𝑁𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝐴𝑐𝑡𝑢𝑎𝑙 𝑃𝑙𝑎𝑡𝑒𝑠
Knowing the composition of distillate and bottom and the corresponding volatilities, the
column efficiency can be determined.
Page - 133
Experiment 7
(CONTINUOUS DISTILLATION APPARATUS)
Objective:
Steady state distillation of a binary mixture under continuous operation.

Continuous Distillation Apparatus, Hand Held Refractometer, Measuring Cylinder
250ml, Stop Watch.
Reagents:
Ethanol, Water
Page - 134
Theory:
Calculation of Number of Plates using McCabe Thiele Method.
Rectifying Section Operating Line
Stripping Section Operating Line
Page - 135
Above equations combined with the equilibrium curve can be used to calculate the
composition on the various plates working from the condenser down to the still. The plate
which has a composition nearest to that of the feed should, be used as the feed plate.
Consequently, the number of theoretical plates and position of entry for the feed can be
calculated.
Procedure:
1) Charge 10 liters feed mixture of 65 mole percent Ethanol and 35 mole percent Water to
feed tank. Volume of individual components required can be calculated from a
procedure similar to experiment no-4:
2) Charge the reboiler with 10 liters of a mixture of 25 mole percent Ethanol and 75 mole
percent Water. Volume of individual components required can be calculated from a
3) Make sure the filler cap on the top of the reboiler is firmly placed. Turn on the power
to the control panel. Set the temperature selector switch to T9, that is the temperature
in the reboiler, and open valve V5 admitting the cooling water to the condenser at a
flow rate on FI1 of approximately 3 liters/min. This rate may be varied according to
the temperature of the water.
anti-clockwise and turn on the power to the heating element. Another red lamp will
illuminate indicating the heating element is on. Turn the power controller clockwise
until a reading of approximately 1.5 kW is obtained on the digital wattmeter. The
contents of the reboiler will begin to warm up and this can be observed on the
temperature readout, meter.
5) Eventually, vapor will begin to rise up the column and the progress of this can be clearly
observed as well as detected by the increasing temperatures when switching the
temperature selector on T8, T7, T6, T5, T4, T3, T2 and Tl. Vapor will enter the
condenser and reappear as droplets into the glass walled distillate receiver vessel. The
distillate will build up a small level in the receiver and eventually overflow to the reflux
regulator valve. Start the experiment with total reflux, meaning the condensed vapor
will return to the column.
Page - 136
6) The cool distillate is then returning to the top of the column and will cascade down the
Tl, T2, T3, T4, T5, T6, T7 and T8 have reached an average steady temperature (but
note cycling due to the intermittent reflux).
7) Before switching on the reflux switch, set the reflux ratio to 5:1, meaning 5 sec back to
column and 1 sec to top product receiver.
8) The feed to the column must be admitted on the tray 5. When the column has stabilized
at total reflux (it Takes 15 to 30 minutes), the flow of feed and the reflux can be started
at the same time. It is advisable to set a feed flow of 2 liters/hr (from the feed pump
calibration graph). As the flow into the column becomes established so more vapor will
rise up the column and appear as condensate in the distillate receiver, allow this to flow
to the top product receiver.
9) After feeding approximately 3 liters take a sample of the overheads through valve V3.
When doing that, be careful never to drain the condensate return line i.e. partially open
valve V3 to leave a small amount of liquid in the line all the time. Take a further four
samples.
ml before taking the representative sample in a sample glass. Do not drain too much of
"discarding" sample in a safe way. After the representative sample, has been taken, keep
11) Record the refractive index for the taken overhead sample. In a similar manner and
preferably at the same time take a sample of the bottom through valve V2. CAUTION!
THIS SAMPLE WILL BE HOT. Record the refractive index for this sample, too.
12) Repeat the sample taking a further nine times during the experiment (before feed runs
out).
Page - 137
Data Analysis:
Sr. No. Top Product Composition (Mole Bottom Product Composition (Mole
Fraction of Ethanol) Fraction of Ethanol)
1
2
3
4
5
6
7
8
9
10
Equilibrium Data for Ethanol / Water can be calculated using Vapor Liquid Equilibrium Curve
for this system at 1 atm pressure.
Sample Results:
Using a feed of a binary mixture of 60 mole percent Ethanol and 40 mole percent Water.
Top product required: XD = 0.75
Bottom product required: XB = 0.44
Reflux Ratio: 5:1
A material balance on the M.V.C. (More Volatile Component), Ethanol gives:
Units are of molar flow rates:
F=D+B
100 × 0.60 = 0.75 D + 0.44 B
And
D = 100-B
100×0.60 = 0.75(100-B) + 0.44B
B = 48.39
D = 51.61
Ln = 5D
Ln = 258.05
Page - 138
V(n+1) = Ln + D
V(n+1) = 309.66
𝐿𝑛 𝐷
𝑦𝑛+1 = 𝑥𝑛 + 𝑥
𝑉𝑛+1 𝑉𝑛+1 𝐷
258.05 51.61×0.75
𝑦𝑛+1 = 𝑥𝑛 +
309.66 309.66
𝑦𝑛+1 = 0.83𝑥𝑛 + 0.13
L (bar) = 258.05 + 100 = 358.05
V (bar) = L (bar) – B = 358.05 -48.39 = 309.66
𝐿̅ 𝐵
𝑦𝑚+1 = 𝑥𝑚 − 𝑥𝐵
𝑉̅ 𝑉̅
358.05 48.39×0.44
𝑦𝑚+1 = 𝑥𝑚 −
309.66 309.66
𝑦𝑚+1 = 1.16𝑥𝑚 − 0.07

From the equilibrium curve,
1) Use Equilibrium Curve, and plot specific top and bottom operating line equations on
the same diagram.
2) Calculate number of stages:
Page - 139
3) Theoretically, therefore, the distillation column containing eight sieve plates plus the
boiler will give the compositions calculated above. However, as the experiment will
show this is not in fact correct.
4) Determine average column efficiency.
Page - 140
Experiment 8
(CONTINUOUS DISTILLATION APPARATUS)
Objective:
Effect of varying the feed position under continuous operation.

Continuous Distillation Apparatus, Hand Held Refractometer, Measuring Cylinder
250ml, Stop Watch.
Reagents:
Ethanol, Water
Page - 141
Theory:
The rig is provided with three feed positions, one above the top plate, one between the
two four-plate sections, (mid-point) and one below the bottom plate. In this way, the rig can be
run as a conventional distillation column (feed between the sections), as a rectifying column
(feed below the bottom plate) or as a stripping column (feed above the top plate). As the
rectifying case is closely approximated, by the batch distillation. The stripping case is chosen
for this experiment.
Calculation of Number of Plates using McCabe Thiele Method.
Material Balance of top of the column
𝑉𝑛 = 𝐿𝑛+1 + 𝐷 − 𝐹
With respect to M.V.C. this becomes
𝑉𝑛 𝑦𝑛 = 𝐿𝑛+1 𝑥𝑛+1 + 𝐷𝑥𝐷 − 𝐹𝑥𝐹
𝐿𝑛+1 𝑥𝑛+1 𝐷𝑥𝐷 𝐹𝑥𝐹
𝑦𝑛 = + −
𝑉𝑛 𝑉𝑛 𝑉𝑛
Since the liquid overflow is constant Ln = Ln+1
𝐿𝑛 𝑥𝑛+1 𝐷𝑥𝐷 𝐹𝑥𝐹
𝑦𝑛 = + −
Material Balance of bottom of the column:

Vm = Lm+1 - W
With respect to M.V.C. this becomes
𝑉𝑚 𝑦𝑚 = 𝐿𝑚+1 𝑥𝑚+1 − 𝑊𝑥𝐵
Page - 142
𝐿𝑚+1 𝑥𝑚+1 𝑊𝑥𝐵
𝑦𝑚 = −
𝑉𝑚 𝑉𝑚
Since the liquid overflow is constant Lm = Lm+1. As the feed is introduced in the top of
the column Lm = Ln and also Vm = Vn. Above equations combined with the equilibrium curve
can be used to calculate the composition on the various plates working from the condenser
down to the still.
Procedure:
1) Charge 10 liters feed mixture of 63 mole percent Ethanol and 37 mole percent Water to
feed tank. Volume of individual components required can be calculated from a
2) Charge the reboiler with 10 liters of a mixture of 25 mole percent Ethanol and 75 mole
percent Water to overflow valve V1. Volume of individual components required can be
calculated from a procedure similar to experiment no-4:
3) Make sure the filler cap on the top of the reboiler is firmly placed. Turn on the power
to the control panel. Set the temperature selector switch to T9, that is the temperature
in the reboiler, and open valve V5 admitting the cooling water to the condenser at a
flow rate on FI1 of approximately 3 liters/min. This rate may be varied according to the
temperature of the water.
anti-clockwise and turn on the power to the heating element. Another red lamp will
illuminate indicating the heating element is on. Turn the power controller clockwise
until a reading of approximately 1.5 kW is obtained on the digital wattmeter. The
contents of the reboiler will begin to warm up and this can be observed on the
temperature readout, meter.
5) Eventually, vapor will begin to rise up the column and the progress of this can be clearly
observed as well as detected by the increasing temperatures when switching the
temperature selector on T8, T7, T6, T5, T4, T3, T2 and Tl. Vapor will enter the
condenser and reappear as droplets into the glass walled distillate receiver vessel. The
distillate will build up a small level in the receiver and eventually overflow to the reflux
regulator valve. Start the experiment with total reflux, meaning the condensed vapor
will return to the column.
Page - 143
6) The cool distillate is then returning to the top of the column and will cascade down the
Tl, T2, T3, T4, T5, T6, T7 and T8 have reached an average steady temperature (but
note cycling due to the intermittent reflux).
7) Before switching on the reflux switch, set the reflux ratio to 5:1, meaning 5 sec back to
column and 1 sec to top product receiver.
8) The feed to the column must be admitted above the top plate. When the column has
stabilized at total reflux (it Takes 15 to 30 minutes), the flow of feed and the reflux can
be started at the same time. It is advisable to set a feed flow of 2 liters/hr (from the feed
pump calibration graph). As the flow into the column becomes established so more
vapor will rise up the column and appear as condensate in the distillate receiver, allow
this to flow to the top product receiver.
9) After feeding approximately 3 liters take a sample of the overheads through valve V3.
When doing that, be careful never to drain the condensate return line i.e. partially open
valve V3 to leave a small amount of liquid in the line all the time. Take a further four
samples.
ml before taking the representative sample in a sample glass. Do not drain too much of
"discarding" sample in a safe way. After the representative sample, has been taken, keep
11) Record the refractive index for the taken overhead sample. In a similar manner and
preferably at the same time take a sample of the bottom through valve V2. CAUTION!
THIS SAMPLE WILL BE HOT. Record the refractive index for this sample, too.
12) Repeat the sample taking a further nine times during the experiment (before feed runs
out).
Page - 144
Data Analysis:
Sr. No. Top Product Composition (Mole Bottom Product Composition (Mole
Fraction of Ethanol) Fraction of Ethanol)
1
2
3
4
5
6
7
8
9
10
Equilibrium Data for Ethanol / Water can be calculated using Vapor Liquid Equilibrium Curve
for this system at 1 atm pressure.
Sample Results:
Using a feed of a binary mixture of 63 mole percent Ethanol and 47 mole percent Water.
Top product required: XD = 0.66
Bottom product required: XB = 0.21
Reflux Ratio: 5:1
A material balance on the M.V.C. (More Volatile Component), Ethanol gives:
Units are of molar flow rates:
F=D+B
100 × 0.63 = 0.66 D + 0.21 B And
D = 100-B
100×0.63 = 0.66(100-B) + 0.21B
B = 6.67
D = 93.33 Also
Ln = 5D
Ln = 466.65
Vn = Ln + D – F = 466.65 + 93.33 - 100
Vn = 459.98
Page - 145
𝐿𝑛 𝐷 𝐹
𝑦𝑛 = 𝑥𝑛+1 + 𝑥𝐷 − 𝑥𝐹
466.65 93.33×0.66 100×0.63
𝑦𝑛 = 𝑥𝑛+1 + −
499.98 499.98 499.98
𝑦𝑛 = 0.933𝑥𝑛+1 − 0.003
It is for the top section and the bottom section of the column due to different feed position.
From the equilibrium curve,
1) Use Equilibrium Curve, and plot specific operating line equation on the same diagram.
2) Calculate number of stages:
3) Theoretically, therefore, the distillation column containing eight sieve plates plus the
boiler will give the compositions calculated above. However, as the experiment will
show this is not in fact correct.
4) Determine average column efficiency.
Page - 146
Experiment 9
(GAS ABSORPTION COLUMN APPARATUS)
Objective:
To measure the absorption of carbon dioxide into water flowing down the tower, using
the gas analysis equipment provided.

Gas Absorption Column Apparatus, CO2 Cylinder with Integral Pressure Regulator,
Small Funnel, and Tubing.
Reagents:
CO2 Gas, Tap Water, Air, and 300ml of 1.0 molar NaOH solution.
Page - 147
Procedure:
1) First fill the two globes of the absorption analysis equipment on the left of the panel
with 1.0 Molar NaOH solution. Adjust the level in the globes to the '0' mark on the sight
tube, using drain valve C into a flask to do this.
2) Fill the liquid reservoir tank to three-quarters full with fresh tap water.
3) With gas flow control valves C2 and C3 closed, start the liquid pump and adjust the
water flow through the column to approximately 6 liters/minute on flowmeter F1 by
adjusting control valve C1.
4) Start the compressor and adjust control valve C2 to give an air flow of approximately
30 liters/minute in flowmeter F2.
5) Carefully open the pressure regulating valve on the carbon dioxide cylinder, and adjust
valve C3 to give a value on the flowmeter F3 approximately one half of the air flow F2.
(Ensure the liquid seal at the of base of the absorption column is maintained by, if
necessary, adjustment of control valve C4.
6) After 15 minutes or so of steady operation, take samples of gas simultaneously from
sample points S1 and S2. Analyze these consecutively for carbon dioxide content in
these gas samples.
7) Flush the sample lines by repeated sucking from the line, using the gas piston and
expelling the contents of the cylinder to atmosphere. Note that the volume of the
cylinder is about l00 cm3. Estimate the volume of the tube leading to the device. Then
decide how many times you need to suck and expel. (Steps B and C)
8) With the absorption globe, isolated and the vent to atmosphere closed, fill the cylinder
from the selected line by drawing the piston out slowly (Step B). Note volume taken
into cylinder V1, which should be approximately 20ml for this particular experiment.
Wait at least two minutes to allow the gas to come to the temperature of the cylinder.
9) Isolate the cylinder from the column and the absorption globe and vent the cylinder to
atmospheric pressure. Close after about 10 seconds (Step D).
10) Connect cylinder to absorption globe. The liquid level should not change. If it does
change, briefly open to atmosphere again.
11) Wait until the level in the indicator tube is on zero showing that the pressure in the
cylinder is atmospheric.
12) Slowly close the piston to empty the cylinder into the absorption globe. Slowly draw
the piston out again (Steps E and F). Note the level in the indicator tube. Repeat steps
Page - 148
E and F until no significant change in level occurs. Read the indicator tube marking =
V2. This represents the volume of the gas sampled.
HEMPL APPARATUS FOR GAS ANALYSIS
Page - 149
WARNING:
If the concentration of CO2 in the gas sampled is greater than 8%, it is possible to suck
liquid into the cylinder. This will ruin your experiment and takes time to correct. Under these
circumstances, do not pull the piston out to the end of its travel. Stop it at a particular mark,
e.g. V1 = 20 on the coarse scale, and read the fine scale.
Data Analysis:
NOTATION:
V1 = Volume of Gas sample taken in Hempl Apparatus (ml).
V2 = Corresponds to amount of Gas Absorbed in Hempl Apparatus (ml).
F = Volumetric Flowrate (liters/sec).
G = Gas Flowrate (gmols/sec).
Y = Mole Fraction of component in gas phase.
SUBSCRIPTS:
T = Total
i = Inlet Conditions to Column
o = Outlet Conditions from Column
CO2 content of gas samples:

From use of Hempl Apparatus,
𝑉2
𝑉𝑜𝑙𝑢𝑚𝑒 𝐹𝑟𝑎𝑐𝑡𝑖𝑜𝑛 𝑜𝑓 𝐶𝑂2 =
𝑉1
For ideal gases, volume fraction = mole fraction = Y. Check that the sample taken from
the inlet to the absorption column should give the same value of CO2 fraction as that indicated
by the inlet flowmeters:
𝑉2 𝐹3
𝑌𝑖 = =
𝑉1 𝐹2 + 𝐹3
Page - 150
READINGS AT INLET CALCULATIONS
F3 F2
V1 V2 𝐹3 𝑉2
(CO2) (Air) 𝑌𝑖 = 𝑌𝑖 =
ml ml 𝐹2 + 𝐹3 𝑉1
Liters/sec Liters/sec
From Hempl Apparatus and

From Flowmeters
Sample Point S3
Calculation of amount of CO2 absorbed in column from analysis of samples at inlet and outlet.
From Analysis with Hempl apparatus, volume fraction of CO2 in gas stream at inlet:
𝑉2
𝑌𝑖 = ( )
𝑉1 𝑖
And at outlet:
𝑉2
𝑌𝑜 = ( )
𝑉1 𝑜
If Fa is liters/second of CO2 absorbed between top and bottom, then:
CO2 IN CO2 OUT CO2 Absorbed

[𝐹2 + 𝐹3 ]𝑌𝑖 − [𝐹2 + (𝐹3 − 𝐹𝑎 )]𝑌𝑜 = 𝐹𝑎
(𝑌𝑖 − 𝑌𝑜 )(𝐹2 + 𝐹3 ) (𝑌𝑖 − 𝑌𝑜 )

𝐹𝑎 = = ×(𝑇𝑜𝑡𝑎𝑙 𝐺𝑎𝑠 𝐼𝑛𝑙𝑒𝑡 𝐹𝑙𝑜𝑤)
1 − 𝑌𝑜 (1 − 𝑌0 )
INLET CONDITIONS OUTLET

ABSORBED
GAS FLOWS [liters/sec] GAS GAS
CO2:
SAMPLE SAMPLE
Air CO2 Total Fa
𝑉2 𝑉2
F2 F3 F2+F3 𝑌𝑖 = ( ) 𝑌𝑜 = ( ) [liters/sec]
𝑉1 𝑖 𝑉1 𝑜
Note: [Liters/second] can be converted to [gmols/second] as follows:

𝐹𝑎 𝐴𝑣𝑔. 𝑐𝑜𝑙𝑢𝑚𝑛 𝑝𝑟𝑒𝑠𝑠𝑢𝑟𝑒 𝑚𝑚 𝐻𝑔 273
𝐺𝑎 = ×( )×( )
22.42 760 𝐴𝑣𝑔. 𝑐𝑜𝑙𝑢𝑚𝑛 𝑡𝑒𝑚𝑝. 0𝐶 + 273
Absorbed CO2 Fa = ___________________
Page - 151
Ga = _______________________________
The assumption implicitly made here is that the volume flow is not affected by the
pressure drop through the column as this drop should be small in comparison with atmospheric
pressure.
Page - 152
Experiment 10
(GAS ABSORPTION COLUMN APPARATUS)
Objective:
To calculate rate of absorption of CO2 into water from analysis of liquid solutions
flowing down absorption column.

Gas Absorption Column Apparatus, CO2 Cylinder with Integral Pressure Regulator,
and Pyrex Bottle, Pipette, Burette, Flask and Measuring Cylinder.
Reagents:
CO2 Gas, Water, Air, Phenolphthalein, 0.0277 Molar NaOH Solution, 0.01 Molar
NaHCO3 Solution.
Page - 153
Procedure:
1) Fill the liquid reservoir tank at the base of the column to approximately three-quarters
full with (preferably) deionized water. Note the volume added [VT liters].
2) With gas flow control valves C2 and C3 closed, start the liquid pump and adjust the
water flow through the column to approx. 6 liters/minute on flowmeter F1 by adjusting
flow control valve C1.
3) Start the compressor and adjust control valve C2 to give an air flow of approx. 10% of
full scale on flowmeter F2.
4) Carefully open the pressure regulating valve on the carbon dioxide cylinder, and adjust
valve C3 to give a value on the flowmeter F3 approx., one half of the air flow F2 ensure
the liquid seal at the base of the absorption column is maintained by, if necessary
adjustment of control valve C4.
5) After 15 minutes of steady operation, take samples at 10 minute intervals from S4 and
S5. Take 150ml samples at known times in each case. Analyze the samples according
to the procedure detailed below.
Analysis of Carbon Dioxide Dissolved in Water:

Note: Water used for absorption should be deionized as presence of dissolved salts affect the
analysis described below. If tap water is used, no metal ions should be present in greater
quantities than 1.0 mg/liter and pH should be just alkaline: 7.1 to 7.8.
1) Phenolphthalein indicator prepared from carbon dioxide – free distilled water.

2) Standard 0.0277M NaOH solution, prepared by diluting 27.70ml of 1M NaOH standard
solution to1 liter with carbon dioxide free distilled water. Prepare fresh and protect from
carbon dioxide in the atmosphere by keeping in a stoppered Pyrex bottle.
3) Standard 0.01M NaHCO3 solution, prepared by dissolving approximately 0.1 gram of
anhydrous NaHCO3 in carbon dioxide free distilled water to 100ml.
4) Withdraw a sample of liquid S5 from the sump tank with the sampler provided,
approximate volume of 150ml, or from liquid outflow point S4.
5) Discharge the sample at the base of a 100 ml graduated cylinder, flicking the cylinder
to throw off excess liquid above the 100 ml mark.
6) Add 5-10 drops of phenolphthalein indicator solution if the sample turns red
immediately, no free C02 is present. If the sample remains colorless, titrate with
Page - 154
standard NaOH solution. Stir gently with a glass rod until a definite pink color persists
for about 30 seconds. This color change is the end point - note volume VB of NaOH
solution added. For best results, use a color comparison standard, prepared by adding
the identical volume of phenolphthalein solution to 100ml of sodium bicarbonate
solution in a similar graduated cylinder.
Data Analysis:
NOTATION:
Cd = Concentration of dissolved free carbon dioxide (gmol/liter).
F = Volumetric Flowrate (liters/sec).
VB = Volume of NaOH Solution Added in liquid analysis (ml).
SUBSCRIPTS:
T = Total
i = Inlet Conditions to Column
o = Outlet Conditions from Column
The amount of free CO2 in the water sample is calculated from:

𝑔𝑚𝑜𝑙 𝑉𝐵 ×0.0277
𝐶𝑑 = 𝑜𝑓 𝑓𝑟𝑒𝑒 𝐶𝑂2 =
𝑙𝑖𝑡𝑒𝑟 𝑚𝑙. 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
Note: Solubility of CO2 in water is a strong function of temperature. And the accuracy of this
titrimetric method is approximately ±10%.
F1 = _________________ liters/sec.
VT = _________________ Volume of Water in System (liters).
Page - 155
From Sump Tank S5
From Liquid Outlet Sample Point
(Correspond to conditions at top of
S4
Time from Start tower)
(minutes) Cd in tank Cd at outlet
VB VB
[Cdi] [Cdo]
ml ml
gmol/liter gmol/liter
10
20
30
40
50
60
CO2 absorbed over a time period (e.g. 30 minutes):

[𝐶𝑑𝑖 𝑎𝑡(𝑡 = 40) − 𝐶𝑑𝑖 𝑎𝑡(𝑡 = 10)]×𝑉𝑇
𝐴𝑣𝑒𝑟𝑎𝑔𝑒 𝑅𝑎𝑡𝑒 = 𝑔𝑚𝑜𝑙/𝑠𝑒𝑐
30×60
CO2 absorbed across the column at any particular time:
Inlet flow of dissolved CO2 = F1×Cdi gmol/sec. = _____________________ gmol/sec.
Outlet flow of dissolved CO2 = F1×Cdo gmol/sec. = ____________________ gmol/sec.
𝐴𝑏𝑠𝑜𝑟𝑝𝑡𝑖𝑜𝑛 𝑅𝑎𝑡𝑒 = 𝐹1 [𝐶𝑑𝑖 − 𝐶𝑑𝑜 ] 𝑔𝑚𝑜𝑙/𝑠𝑒𝑐
Page - 156
Experiment 11
(LIQUID-LIQUID EXTRACTION APPARATUS)
Objective:
To determine the Distribution Coefficient for the system Trichloroethylene – Propanoic
Acid – Water and to show its dependence on concentration.

250ml Conical Stoppered Flask or Beaker, 250ml Measuring Cylinder, 250ml
Separating Funnel, Pipette with Rubber Bulb, Burette, and Funnel.
Reagents:
0.1 Molar NaOH Solution, Phenolphthalein, Propionic Acid, Trichloroethylene, Water.
WARNING:
Concentrated Sodium Hydroxide can form explosive volatile products when in contact
with Trichloroethylene. Ensure that diluted Sodium Hydroxide (NaOH) is used when
performing this experiment.
Page - 157
Theory:
The solvent (water) and solution (trichloroethylene/propionic acid) are mixed together
and then allowed to separate into the extract phase and the raffinate phase. The extract phase
will be water and propionic acid and the raffinate phase is trichloroethylene with a trace of
propionic acid.
The Distribution Coefficient K, is defined as the ratio:
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑡ℎ𝑒 𝑒𝑥𝑡𝑟𝑎𝑐𝑡 𝑝ℎ𝑎𝑠𝑒 𝑌
𝐾= =
𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑜𝑓 𝑠𝑜𝑙𝑢𝑡𝑒 𝑖𝑛 𝑡ℎ𝑒 𝑟𝑎𝑓𝑓𝑖𝑛𝑎𝑡𝑒 𝑝ℎ𝑎𝑠𝑒 𝑋
It is assumed that phase equilibrium exists between the two phases. At low concentrations, the
distribution coefficient is dependent on the concentration and thus Y = KX.
Procedure:
1) Make up in a conical flask a mixture of 50ml trichloroethylene and 50ml of de-
mineralized water.
2) Add 5ml of propionic acid. 5ml can be pipetted into the flask using a pipette with a
rubber bulb.
3) Place a stopper into the flask and shake for a minimum of 5 minutes.
4) Pour into a separating funnel, leave for 5 minutes and remove the lower aqueous layer.
5) Take a 10ml sample of this layer and titrate against 0.1M NaOH solution using
phenolphthalein as an indicator.
6) Repeat the experiment for two further concentrations of propionic acid i.e. for initial
additions of 3ml and 1ml of propionic acid.
Data Analysis:
Propionic Acid Propionic Acid

Volume of Distribution
Concentration Concentration
Propionic Acid 0.1M NaOH Coefficient
in Aqueous in Organic
Added (ml) Solution used. 𝑌
Layer Layer 𝐾=
(ml) 𝑋
Y X
5
3
1
Page - 158
Page - 159
Experiment 12
(LIQUID-LIQUID EXTRACTION APPARATUS)
Objective:
To demonstrate how a mass balance is performed on the extraction column, and to
measure the mass transfer coefficient and its variation with flowrate with the aqueous phase as
the continuous medium.

Liquid-Liquid Extraction Apparatus, 250ml Conical Stoppered Flask, 250ml
Measuring Cylinder, Pipette with Rubber Bulb, Burette.
The solvent metering pump is calibrated in percentage of maximum flow which varies
slightly from pump to pump. The pump should be calibrated initially by setting F2 to 100%,
setting valve V8 to the calibrate position and measuring the flow from the pump, using a
measuring cylinder and stopwatch. Calculate the flow rate produced settings of 10% intervals
(ml per minute), then plot a graph of ml per minute against percentage of metering pump stroke.
Thereafter any selected flow may be obtained by using the graph.
Page - 160
Reagents:
0.1 Molar NaOH Solution, Phenolphthalein, Propionic Acid, Trichloroethylene, Water.
Procedure:
WARNING:
Concentrated Sodium Hydroxide can form explosive volatile products when in contact
with Trichloroethylene. Ensure that diluted Sodium Hydroxide (NaOH) is used when
performing this experiment.
1) Add 100ml of propionic acid to 10 liters of trichloroethylene. Mix well to ensure an

even concentration then fill the organic phase feed tank (bottom tank) with the mixture.
2) Switch the level control to the bottom of the column (electrode switch S2).
Page - 161
3) Fill the water feed tank with 15 liters of clean de-mineralized water, start the water feed
pump and fill the column with water at a high flow rate.
4) As soon as the water is above the top of the packing, reduce the flow rate to 0.2
liters/min.
5) Start the metering pump and set at a flow rate of 0.2 liters/min.
6) Run for 15-20 minutes until steady conditions are achieved, monitor flow rates during
this period to ensure that they remain constant.
7) Take 15ml samples from the feed, raffinate and extract streams.
8) Titrate 10ml of each sample against 0.1M NaOH using phenolphthalein as the indicator.
(To titrate the feed and raffinate they may need continuous stirring using a magnetic
stirrer).
9) Repeat the experiment with both the water and trichloroethylene flow rates being
increased to 0.3 1iters/min.
Data Analysis:
NOTATION:
Vw = Water flowrate (Liters/sec)
V0 = Trichloroethylene flowrate (Liters/sec)
X = Propionic acid concentration in the organic phase (kg/liter)
Y = Propionic Acid concentration in the aqueous phase (kg/1iter)
SUBSCRIPTS:
1 = Top of Column
2 = Bottom of Column
The equations are given for the system Trichloroethylene-Propionic Acid-Water.

Propionic acid extracted from the organic phase (raffinate) = 𝑉𝑜 (𝑋1 − 𝑋2 )
Propionic acid extracted by the aqueous phase (extract) = 𝑉𝑤 (𝑌1 − 0)
Therefore:
𝑉𝑜 (𝑋1 − 𝑋2 ) = 𝑉𝑤 (𝑌1 − 0)
Mass transfer coefficient (based on the raffinate phase) kD:
𝑅𝑎𝑡𝑒 𝑜𝑓 𝐴𝑐𝑖𝑑 𝑇𝑟𝑎𝑛𝑠𝑓𝑒𝑟
𝑘𝐷 =
𝑉𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑃𝑎𝑐𝑘𝑖𝑛𝑔 × 𝐿𝑜𝑔 𝑀𝑒𝑎𝑛 𝐷𝑟𝑖𝑣𝑖𝑛𝑔 𝐹𝑜𝑟𝑐𝑒
Page - 162
∆𝑥1 − ∆𝑥2
𝐿𝑜𝑔 𝑀𝑒𝑎𝑛 𝐷𝑟𝑖𝑣𝑖𝑛𝑔 𝐹𝑜𝑟𝑐𝑒 =
∆𝑥
𝑙𝑛 (∆𝑥1 )
2
Where:
∆𝑥1 = 𝐷𝑟𝑖𝑣𝑖𝑛𝑔 𝐹𝑜𝑟𝑐𝑒 𝑎𝑡 𝑡ℎ𝑒 𝑡𝑜𝑝 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑙𝑢𝑚𝑛 = (𝑋2 − 0)
∆𝑥2 = 𝐷𝑟𝑖𝑣𝑖𝑛𝑔 𝐹𝑜𝑟𝑐𝑒 𝑎𝑡 𝑡ℎ𝑒 𝑏𝑜𝑡𝑡𝑜𝑚 𝑜𝑓 𝑡ℎ𝑒 𝑐𝑜𝑙𝑢𝑚𝑛 = (𝑋1 − 𝑋1∗ )
𝑋1∗ = 𝐶𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑖𝑛 𝑡ℎ𝑒 𝑜𝑟𝑔𝑎𝑛𝑖𝑐 𝑝ℎ𝑎𝑠𝑒 𝑤ℎ𝑖𝑐ℎ 𝑤𝑜𝑢𝑙𝑑 𝑏𝑒 𝑖𝑛 𝑒𝑞𝑢𝑖𝑙𝑖𝑏𝑟𝑖𝑢𝑚
𝑤𝑖𝑡ℎ 𝑐𝑜𝑛𝑐𝑒𝑛𝑡𝑟𝑎𝑡𝑖𝑜𝑛 𝑌1 𝑖𝑛 𝑡ℎ𝑒 𝑎𝑞𝑢𝑒𝑜𝑢𝑠 𝑝ℎ𝑎𝑠𝑒.
The equilibrium values can be found using the distribution coefficient found in the previous
experiment.
Flowrate of Aqueous Phase:

Flowrate of Organic Phase:
Volume of 0.1M NaOH Concentration of Propionic
solution used in titration Acid
(ml) kg/liters
Feed:
Raffinate:
Extract:
Propionic acid extracted from
the organic phase:
Propionic acid extracted from
the aqueous phase:
Mass Transfer Coefficient kD
Page - 163
Experiment 13
(TRAY DRIER APPARATUS)
Objective:
To produce drying and drying rate curves for a wet solid being dried with air of fixed
temperature and humidity.

Tray Drier Apparatus, Digital Weight Balance, Wet and Dry Bulb Thermometer, and
Stop Watch.
Reagents:
Sand, Air.
Theory:
Immediately after contact between the wet solid and the drying medium, the solid
temperature adjusts until it reaches a steady state. The solid temperature and the rate of drying
may increase or decrease to reach the steady state condition. At steady state, the temperature
of the wet solid surface is the wet bulb temperature of the drying medium. Temperatures within
Page - 164
the drying solid also tend to equal the wet bulb temperature of the gas but lag in movement of
mass and heat in some deviation. Once the stock temperatures reach the wet bulb temperature
of the gas, they are quite stable and the drying rate also remains constant. This is the constant
rate drying period which ends when the solid reaches the critical moisture content. Beyond this
point the surface temperature rises, and the drying rate falls off rapidly. The falling rate period
can take a far longer time than the constant rate period even though the moisture removal may
be less. The drying rate approaches zero at some equilibrium moisture content which is the
lowest moisture content obtainable with the solid under the drying conditions used.
Procedure:
1) Take dry sand to fill the four trays to a depth of about 10 mm each should be accurately
weighed before being saturated with water in a container.
2) The sand should be removed from the container and drained of excess “free” water
before being loaded evenly and smoothly into the sand drying trays, taking care to avoid
any spillage.
3) The total weight of the wet sand should be noted before drying commence.
4) At some arbitrary time (t=0), switch on and set the fan speed control to mid-position
and the heater power control to maximum letting them remain constant throughout the
experiment.
5) Record the total weight of sand in the trays at regular time intervals until drying is
complete.
NOTE:
It is recommended that the laboratory be well ventilated to ensure that warm moist air
discharged from the drier does not affect the original inlet conditions over the period of the
experiment.
Data Analysis:
Weight of dry sand = ________________ kg.
XE = Equilibrium Moisture Content
Time (min) 0
Weight of wet sand (kg)
Moisture Content XE
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𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐿𝑖𝑞𝑢𝑖𝑑 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑊𝑒𝑡 𝑆𝑎𝑛𝑑 − 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑
𝑋𝐸 = =
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑
From the results, plot the drying curve relating moisture content as a function of time.
Carefully differentiate data from this curve to produce the drying rate - moisture content plot,
attempting to identify the points (A, B, C and D) at which the drying passes from one regime
to the next.
Comment upon the results obtained and relate the curves to the mechanism by which drying
occurs. What is the significance of the equilibrium moisture content?
Page - 166
Experiment 14
(TRAY DRIER APPARATUS)
Objective:
To investigate the influence of air temperature on the drying rate of a wet solid in air at
fixed velocity.

Tray Drier Apparatus, Digital Weight Balance, Wet and Dry Bulb Thermometer, and
Stop Watch.
Reagents:
Sand, Air.
Procedure:
1) Take dry sand to fill the four trays to a depth of about 10 mm each should be accurately
weighed before being saturated with water in a container.
2) The sand should be removed from the container and drained of excess 'free' water before
being loaded evenly and smoothly into the drying trays, taking care to avoid any
spillage.
3) The total weight of the wet sand should be noted before drying commences.
Page - 167
4) At some arbitrary time (t=0), switch on and set the fan speed control to produce an air
velocity of about 0.5 m/s, Measure the velocity of the air flow through the drier using
the digital anemometer.
5) Set the heater power control to a nominal setting and measure the dry and wet bulb air
temperatures upstream of the sand trays using the aspirating psychrometer.
6) Record the total weight of sand in the trays at regular time intervals until drying is
complete.
7) The experiment should be repeated for other air temperatures by increasing the power
supplied to the heater up to the maximum setting.
8) It is important to keep the air velocity constant and to use the same weight and
distribution of sand in each of the tests.
NOTE:
It is recommended that the laboratory be well ventilated to ensure that moist air
discharged from the drier does not affect the original inlet conditions over the period of the
experiments.
Data Analysis:
The drying rate of a wet solid in air changes throughout the drying period since the
controlling factors are different for each major section of the drying rate curve. However, many
wet solids exhibit a period during which the drying rate is essentially constant and:
𝑅𝑐 ∝ ℎ𝑣 (𝑇𝑣 − 𝑇𝑖 )
Where:
𝑅𝑐 = 𝐷𝑟𝑦𝑖𝑛𝑔 𝑅𝑎𝑡𝑒 𝑑𝑢𝑟𝑖𝑛𝑔 𝑐𝑜𝑛𝑠𝑡𝑎𝑛𝑡 𝑟𝑎𝑡𝑒 𝑝𝑒𝑟𝑖𝑜𝑑
ℎ𝑣 = 𝐻𝑒𝑎𝑡 𝑇𝑟𝑎𝑛𝑠𝑓𝑒𝑟 𝐶𝑜𝑒𝑓𝑓𝑖𝑐𝑖𝑒𝑛𝑡
𝑇𝑣 = 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑑𝑟𝑦𝑖𝑛𝑔 𝑔𝑎𝑠
𝑇𝑖 = 𝑇𝑒𝑚𝑝𝑒𝑟𝑎𝑡𝑢𝑟𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑙𝑖𝑞𝑢𝑖𝑑/𝑔𝑎𝑠 𝑖𝑛𝑡𝑒𝑟𝑓𝑎𝑐𝑒
The temperature of the drying gas (Tv) is the normally measured dry bulb temperature.
At steady state, the temperature of the liquid-gas interface (Tj) is equal to the wet bulb
temperature of the drying air. Thus, the drying rate is proportional to the difference between
the dry and wet bulb temperatures of the air.
Page - 168
Air Velocity = ____________________ m/sec.
Weight of dry sand = _______________ kg.
Dry Bulb Temp. Tv oC

Wet Bulb Temp. Ti oC
(Tv-Ti) oC
Time (min) 0 0 0
Wet Sand Weight (kg)
Moisture Content XE
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐿𝑖𝑞𝑢𝑖𝑑 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑊𝑒𝑡 𝑆𝑎𝑛𝑑 − 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑

𝑋𝐸 = =
𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑 𝑊𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝐷𝑟𝑦 𝑆𝑎𝑛𝑑
From the results, plot the drying curves relating moisture constant and time for each
test. Differentiate data from, these curves to produce the drying rate-moisture content curves:
Comment upon the results obtained, noting the influence that (Tv - Ti) had upon the drying rate
during the constant rate period.
Page - 169
Experiment 15
(FLUIDIZED BED DRIER APPARATUS)
Objective:
To:
1. Investigate the simple drying of a material to give moisture content and the drying
time required.
2. Determine the drying curves to assess the feasibility of fluidized bed drying of a
material on an industrial scale.
3. Calculate heat transfer coefficient (It is important in drier design and comparison of
fluidized beds with other drying methods).

Fluidized Bed Drier Apparatus, Digital Weight Balance, and Wet and Dry Bulb
Thermometer.
Reagents:
Any suitable solid particles which are wet and need to be dried, Air.
Page - 170
Procedure:
1) Determine the optimum bed depth the optimum bed depth is that which can be fluidized
at the required temperature by relative high air velocity. The optimum bed depth will
vary appreciably with the material-an initial bed depth of about 75mm is typical.
2) Remove any excess water from the solid sample by decanting and / or using a filter
pump.
3) Place the sample of material in the jar to an appropriate bed depth. Weigh the jaar alone
then with the material.
4) Fix the sealing ring into the groove.
5) Switch on the mains supply and select the drying temperature required (select three
temperatures).
6) Note the wet and dry bulb temperatures of the inlet air to the fan and outlet air from the
fluidized bed.
7) Weigh the jar with material at 2 minute intervals for about 16 minutes (or as long as it
takes to attain constant weight) recording the wet and dry bulb temperature before
removing the jar for weighing. Continue until constant weigh is achieved indicating
that the equilibrium moisture content has been reached.
8) Record the drying time and moisture content.
Data Analysis:
From the results, plot the drying curve relating moisture content as a function of time.
Carefully differentiate data from this curve to produce the drying rate - moisture content plot,
attempting to identify the points (A, B, C and D) at which the drying passes from one regime
to the next.
Page - 171
CALCULATION OF HEAT TRANSFER COEFFICIENT:
Heat lost by entering gas = Heat transferred to solids to vaporize the liquid
Therefore:
𝑑𝑤 1
= −ℎ𝐴(𝑇𝑎 − 𝑇𝑠 )log 𝑚𝑒𝑎𝑛 ×
𝑑𝑡 𝐿
This equation can be integrated to give:
(𝑊0 − 𝑊𝑐 )×𝐿
ℎ=
𝑡×𝐴×(𝑇𝑎 − 𝑇𝑠 )log 𝑚𝑒𝑎𝑛
Where:
dw/dt = Constant drying rate [kg/s]
L = Latent heat of vaporization [J/kg]
H = Heat transfer coefficient [W/(m2×oC)]
A = Surface area [m2]
Ta = Dry bulb air temperature [oC]
Ts = Wet bulb air temperature, [oC]
Wo = Initial moisture content [kg water/kg dry solid]
Wc = Critical moisture content at end of constant rate period [kg water/kg dry solid]
t = Constant rate drying time [sec]
Page - 172
Lab Flexes
1. Lab Notebook Rubric

2. Experiment Performance Rubric
3. General Safety Precautions
4. List of Equipment
5. List of Experiments
3. Gas Diffusion Coefficients Apparatus
4. Ion Exchange Apparatus
5. Batch Distillation Apparatus
6. Continuous Distillation Apparatus
7. Gas Absorption Column Apparatus
8. Liquid-Liquid Extraction Apparatus
9. Tray Drier Apparatus
10. Fluid Bed Drier Apparatus
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Material Safety Data Sheets for Chemicals
1. Acetone
2. HCl
3. NaOH
4. H2O
5. Methylcyclohexane
6. Toluene
7. CO2
8. Air
9. NaHCO3
10. Phenolphthalein
11. Propionic Acid
12. Trichloroethylene
13. Sand
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MASS TRANSFER

Department of Chemical Engineering

List of Possible Hazards in M.T.O. Lab ...............................................2

Following are the potential hazards and their remedies:

S. No. Potential Hazard Mitigation

The Control of Substances Hazardous to Health Regulations (1988)

Physical data about the substance

Although these regulations may not be applicable in your country, it is strongly

Where practicable the water should be maintained at a temperature below 20°C or

However, it is recommended that the RESIDUAL CURRENT DEVICE (RCD)

Excellent (2) Satisfactory (1) Unsatisfactory (0) Score

Below average Unsatisfactory

1. Gas Diffusion Coefficients Apparatus

GAS DIFFUSION COEFFICIENTS APPARATUS

The Gaseous Diffusion Coefficient Apparatus allows students to measure to a

The equipment consists of an acrylic assembly which is sub-divided into two

Water in the bath is heated by a cartridge element which is controlled by an adjustable

ION EXCHANGE APPARATUS

1) Two Vertical Columns

The various processes to be used in the experiments are as follows:

ELECTRICAL SUPPLY FOR VERSION W 9-A:

ELECTRICAL SUPPLY FOR VERSION W9-B:

1. Place backboard and tank on a firm level surface.

BATCH DISTILLATION APPARATUS

Condensate is collected in a glass decanter (phase separator) which is by-passed for

ELECTRICAL SUPPLY FOR VERSION-A:

ELECTRICAL SUPPLY FOR VERSION-B:

a) Reflux Ratio Control

Example of Setting the Timer:

If a ratio of 4:1 is required over the same cycle time:

4 + 1 = 5; 9/5 = 1.8; 4 x 1.8 = 7.2

To set the controller:

b) Pressure Drop in Column

When using valve V3 to obtain a sample of top product or to measure boil up

d) Suitability of Test Mixtures

CONTINUOUS DISTILLATION APPARATUS

Considerable advances in the instrumentation and control of distillation columns have

The range is based on a common distillation column arrangement, which uses

1. Batch or continuous operation

1) Tubular Steel Framework

Condensate is collected in a glass-decanter (VI ) (phase separator) which is bypassed

ELECTRICAL SUPPLY FOR VERSION-A:

ELECTRICAL SUPPLY FOR VERSION-B:

a) Reflux Ratio Control

Example of Setting the Timer:

If a ratio of 4:1 is required over the same cycle time:

4 + 1 = 5; 9/5 = 1.8; 4 x 1.8 = 7.2

To set the controller:

b) Pressure Drop in Column

When using valve V3 to obtain a sample of top product or to measure boil up

d) Suitability of Test Mixtures

GAS ABSORPTION COLUMN APPARATUS

STANDARD ELECTRICAL SUPPLY

NON-STANDARD ELECTRICAL SUPPLY

1. Fill sump tank with clean water.

The equipment is now ready for use.

LIQUID-LIQUID EXTRACTION APPARATUS

1) Stroke Adjustment Knob

The equipment is mounted in a floor-standing, welded steel framework fitted with

ELECTRICAL SUPPLY FOR VERSION UOP5-A:

ELECTRICAL SUPPLY FOR VERSION UOP5-B:

ELECTRICAL SUPPLY FOR VERSION UOP5-G:

TRAY DRIER APPARATUS