Lab Manual CL Lab 1

Faculty of Engineering and Science (FES)
Department of Chemical Engineering
UEMK2411
CHEMICAL
ENGINEERING
LABORATORY I
MANUAL
1
UEMK 2411 CHEMICAL ENGINEERING LABORATORY I MANUAL
Contents
Introduction............................................................................................................................vii
Subject Synopsis..................................................................................................................vii
Course Objectives................................................................................................................vii
Course Outcomes.................................................................................................................vii
Rules and Regulations..........................................................................................................viii
General Rules......................................................................................................................viii
Laboratory Safety...............................................................................................................viii
Responsibility of Students....................................................................................................ix
Assessments...............................................................................................................................x
Marks Breakdown..................................................................................................................x
Laboratory Performance Marks.............................................................................................x
Laboratory Reports...............................................................................................................xi
Laboratory Report Marks............................................................................................................xi
Laboratory Report Format.........................................................................................................xii
Laboratory Report Specifications..............................................................................................xiv
1.0 Heat Exchangers............................................................................................................1
1.1 Aims............................................................................................................................2
1.2 Introduction.................................................................................................................2
1.2.1 Theory...........................................................................................................................2
1.2.2 The Heat Exchanger apparatus.....................................................................................3
1.3 Safety Precautions.......................................................................................................5
1.4 General Operating Procedures.....................................................................................5
1.5 Experimental................................................................................................................6
1.6 Results Analyses and Discussion.................................................................................6
2.0 Cooling Tower Demonstration..........................................................................................8
2.1 Aims.................................................................................................................................9
2.2 Introduction......................................................................................................................9
2.2.1 Theory..................................................................................................................................9
2.2.2 The Cooling Tower Equipment...........................................................................................12
2.3 Safety Precautions..........................................................................................................13
2.4 General Operating Procedures.......................................................................................14
2.5 Experimental..................................................................................................................15
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2.6 Results Analyses and Discussion...................................................................................16

3.0 Tray Drying..................................................................................................................17
3.1 Aims..........................................................................................................................18
3.2 Introduction...............................................................................................................18
3.2.1 Theory..........................................................................................................................18
3.2.2 The Tray Dryer............................................................................................................20
3.3 Safety Precautions.....................................................................................................20
3.4 General Operating Procedures...................................................................................21
3.5 Experimental..............................................................................................................21
3.6 Results Analyses and Discussion...............................................................................21
4.0 Vapour-Liquid Equilibrium (VLE)...........................................................................23
4.1 Aims..........................................................................................................................24
4.2 Introduction...............................................................................................................24
4.2.1 Theory..........................................................................................................................24
4.2.2 Vapour Pressure...........................................................................................................25
4.2.3 Non-Ideal Behaviour...................................................................................................26
4.2.4 Temperature.................................................................................................................26
4.2.5 Relative Volatility.........................................................................................................27
4.2.6 Refractive Index...........................................................................................................27
4.2.7 The VLE Apparatus.....................................................................................................28
4.4 Chemical Hazards......................................................................................................30
4.6 Experimental..............................................................................................................31
5.0 Liquid Diffusion Coefficient.......................................................................................33
5.1 Aims..........................................................................................................................34
5.2 Introduction...............................................................................................................34
5.2.1 Theory..........................................................................................................................34
5.2.2 The Liquid Diffusion Apparatus...................................................................................35
5.5 Experimental..............................................................................................................36
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6.0 Gas Absorption............................................................................................................37

6.1 Aims..........................................................................................................................38
6.2 Introduction...............................................................................................................38
6.2.1 Theory..........................................................................................................................38
6.2.2 The Gas Absorption apparatus....................................................................................40
6.5 Experimental..............................................................................................................41
7.0 Batch Distillation Column..........................................................................................43
7.1 Aims..........................................................................................................................44
7.2 Introduction...............................................................................................................44
7.2.1 Theory..........................................................................................................................45
7.2.2 The Batch Distillation apparatus.................................................................................47
7.4 Chemical Hazards......................................................................................................49
7.6 Experimental..............................................................................................................50
8.0 Liquid-liquid Extraction.............................................................................................53
8.1 Aims..........................................................................................................................53
8.2 Introduction...............................................................................................................53
8.1.1 Extraction Equipment..................................................................................................54
8.1.2 Theory Material Balance on Solute..........................................................................55
8.2 Liquid-liquid extraction unit......................................................................................56
8.3 Operating Procedures................................................................................................58
8.3.1 Pre-experiment Procedures..........................................................................................58
8.4 Chemical Hazards, Safety and Precautions...............................................................59
8.4.1 Chemical Hazards (refer MSDS in Appendix A for more details)................................59
8.4.2 Safety Precautions.......................................................................................................59
8.5 Experiments...............................................................................................................59
8.5.1 Experiment 1: Determination of Efficiency of Extraction............................................59
8.5.2 Experiment 2: Investigate the Effect of Feed and Solvent Flow Rates on Extraction...60
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9.0 Reverse Osmosis..........................................................................................................61

9.1 Aims..........................................................................................................................61
9.2 Introduction...............................................................................................................61
9.2.1 Theory..........................................................................................................................62
9.3 Reverse Osmosis and Ultrafiltration Unit.................................................................64
9.3.1 Membrane and Membrane Housing............................................................................64
9.3.2 Pumps..........................................................................................................................65
9.3.3 Tanks............................................................................................................................65
9.3.4 Instrumentations..........................................................................................................65
9.4 Operating Procedures................................................................................................66
9.4.1 Pre-experiment Procedures..........................................................................................66
9.4.2 General Operating Procedures....................................................................................66
9.6 Experiments...............................................................................................................68
9.6.1 Experiment 1: Determination of Clean Membrane Resistance, R m..............................68
9.6.2 Experiment 2: Determination Of Membrane Resistance Due to Concentration
Polarization, Rcp and Observed Salt Rejection from Water, ROBS.................................................69
10.0 Filtration......................................................................................................................71
10.1 Aims.......................................................................................................................72
10.2 Introduction............................................................................................................72
10.2.1 Theory..........................................................................................................................73
10.3 Plate and Frame Filter Press.................................................................................73
10.4 Operating Procedures.............................................................................................74
10.5 Safety Precautions..................................................................................................75
10.6 Experiments...........................................................................................................75
10.6.1 Experiment 1A: Determine the Pure Water Flux of Filter Medium (cloth medium).....75
10.6.2 Experiment 1B: Determine the Water Flux and Separation Efficiency of Different
Filter Medium.............................................................................................................................76
10.7 Results Analyses and Discussion...........................................................................77
Appendix A: Material Safety Data Sheet (MSDS)..............................................................78
Ethanoic Acid (Acetic Acid)................................................................................................78
Ethyl Acetate........................................................................................................................79
Ethyl Alcohol (Ethanol).......................................................................................................80
1-propanol............................................................................................................................81
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2-propanol............................................................................................................................82
Appendix B: Psychrometric Chart.......................................................................................83
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Introduction
Subject Synopsis
A laboratory course in pilot-scale processes involves thermodynamics, heat transfer and mass
transfer and fluid separation. Students will acquire the skills in project definition,
experimental operation, analytical procedures, data analysis and technical reports preparation.
Course Objectives
This subject aims to help students to develop their skills of collecting, analysing and
presenting the results of data acquired within a well-defined experimental system. The
specific objectives are to:
Combine elements of theory with practical: particularly in heat and mass transfer,
thermodynamics, and fluid separation;
Develop and demonstrate a knowledge of experimental error analysis, probability and
statistics;
Develop practical skills to plan and design laboratory experiments;
Familiarise with laboratory safety procedures;
Work collaboratively within a group setting.
Course Outcomes
Upon completion of this course, a student should be able to:

Collect and analyse experimental data and its relationship to theoretical principles of:
o Heat and mass transfer,
o Thermodynamics,
o Fluid Separation.
Operate laboratory experiments safely.
Prepare a written report that clearly presents the experimental results, analysis, and
relationship to theory.
Develop skills in operating common chemical engineering equipment and
measurement apparatus.
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8
Rules and Regulations

General Rules
1. Students must abide the dress code while working in the laboratory:
Laboratory coats must be worn at all times.
Only closed-toe shoes and long pants are allowed.
Hair must be tied up tidily.
2. Bags and other belongings must be kept at the designated places.
3. Food, drinks and smoking are strictly prohibited inside the laboratory.
4. Noise must be kept to a minimal level at all times.
5. Students are strictly prohibited from:
Working alone without the supervision of a laboratory instructor. At least two persons
have to be present in the laboratory at the same time.
Bringing any unauthorised outsiders into the laboratory.
Performing any unauthorised experiments.
Removing, dismantling or attempting to steal any parts of equipment and technical
manuals out from the laboratory without permission of a laboratory instructor.
Laboratory Safety
1. The laboratory work space shall always be kept tidy after the experiments.
2. Report to the laboratory instructor immediately if the laboratory equipment is
suspected to be malfunctioning, faulty or damaged.
3. Any accident/injuries shall be reported to the laboratory instructor immediately.
4. Use the emergency stop button should you suspect any serious electrical fault
occurred on the laboratory equipment.
5. Do not work with electricity under wet condition in laboratory. Electric shock is a
serious fatal error due to human negligence and may cause death.
6. Students are required to wear goggles, gloves, apron and mask when handling
corrosive or active chemical agents.
7. Hazardous chemical agents must be properly stored and labelled in a designated
place. Students must acquire and study the material safety data sheet of a
particular chemical agent before using it.
(Extracted from Student Laboratory Guidelines. Refer to the Guidelines for complete rules &
regulations)
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Responsibility of Students
1. It is the responsibility of all students to read and abide the rules stated in Section
2.1 and 2.2.
2. Students shall have instinctive awareness towards the properties of the laboratory
equipment and be responsible when using them. Any damages caused by
vandalism to the equipment may result in serious disciplinary actions.
3. Attendance is compulsory and shall be taken at each laboratory session.
4. Laboratory reports can only be accepted for submission if the student has attended
the laboratory session.
5. Student must be punctual to attend laboratory session. Students who are late for
more than 30 minutes will be barred from attending the laboratory session.
Only students with valid reason of medical basis or unforeseen circumstances can
be considered to apply for laboratory replacement.
6. Students are expected to read and understand their respective experiments before
each laboratory session. This includes understanding all the safety measures and
precautionary steps.
7. Experiments have to be performed at the allocated time. Upon completion of each
laboratory session, students shall:
Switch off all the power and water supply of the equipment following the proper
shutdown procedure.
Clean all glassware and place them back to where they took them from.
Show the results to the laboratory instructor before leaving the laboratory.
8. Students have to hand in their laboratory report (group report) to the laboratory
officer a week after the date of experiment.
9. Fabricating results and plagiarism are strictly prohibited. Strict actions will
be taken if students are found fabricating results or copy from others.
I, ________________________________________ (Student ID: )

hereby confirm that I have read and understood the rules and regulations in the laboratory and
shall abide to them at all times. I understand that failure to do so will result in serious
disciplinary actions by the University.
Signature: Date:
______________________ ___________________
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Assessments
Marks Breakdown
Type of Assessment Marks Contribution

Laboratory Performance
70 %
Laboratory Reports
Laboratory Test 30 %
Laboratory Performance Marks
Performance marks shall be assessed on individuals during the laboratory sessions

throughout the entire semester. Marks will be given based on the following criteria:
Marks
Criteria Description
Contribution
Safety Adhere to laboratory safety, rules and

Awareness regulation as per Sections 2.1, 2.2 and 2.3.
Abide to dress code (Section 2.1.1) while
working in the laboratory. 10 % out of 70 %
Punctuality Attend laboratory sessions on time.
Preparation Show understanding in the experiments.
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Laboratory Reports
Laboratory Report Marks
Laboratory reports will be assessed based on the following criteria:
Marks
Criteria Description
Contribution
Overall Organisation of report with the correct format (as 2.5

Presentation per Section 3.3.2) and necessary information such as
titles, figure explanations.
of Report
Report is written in clear and concise English.
Proper referencing using the APA referencing style.
Observations / Valid observations, consistent with event and 2.5

Data / Result demonstrate attention to detail.
Presentation Data are presented in an organised manner.
Quality of data reflects students ability to perform
experiment successfully and utilise computer
software for analyses (if applicable).
All calculations and graphs are correct.
Discussion Discussion shows complete understanding of 3.5

experiment and the significance of data.
Logical explanation for problems in the data with
the support from the literature.
Conclusion Summary of key findings in a clear statement. 1.5

Clearly show relationships between data and
conclusion.
Express views on the weakness of the experimental
design (if there is any), or what is the implication of
the conclusion.
TOTAL 10 % each
report
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Laboratory Report Format
The laboratory report must follow the following format:
Max number of lines /

Section
pages
UTAR Laboratory Cover Page
1) Title of Experiment 1 2 lines
2) Objectives of Experiment 1 5 lines
3) Introduction page
Provide a scientific background related to the experiment and
provides the reader with justification for why the work was
carried out.
4) Materials and Equipment page

List only the materials/chemicals and equipment/apparatus
used in the experiment.
5) Results and Calculations Depends on results and

Present the data obtained from the experiment. The data calculations
have to be presented in a clear and understandable manner.
All tables must be clearly labelled with numbers and titles.
All necessary calculations based on the raw data should be
provided in this section.
6) Discussion Depends, usually around

This is most important section where detailed analysis of the 2 pages
experimental data should be provided. Factors/issues related
to the obtained results must be explained.
Graphic materials based on the experimental data should be
presented and discussed in this section. All graphs must be
clearly labelled with numbers and titles.
Strategies that can be used in the discussion:
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Compare and explain the results obtained to the

theoretical results.
Relate results to the experimental objectives
Analyse the experimental errors
Find and explain the ambiguities exist, provide logical
explanation for the problems (with proper references)
7) Conclusion 5 lines
Based on the discussion provided, summarise the key
findings in a clear statement. Additionally, the conclusion
can also be used to express views on the weakness of the
experimental design (if there is any), or what is the
implication of your conclusion.
8) References Depends on references

List all references used in the preparation of the report.
Information obtained from any source, including the Internet,
is covered by copyright law. Any source referred in the
report must be acknowledged, both within the text and at
the end of it. The format should follow the Harvard style
referencing.
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Laboratory Report Specifications
Specification Description
Language The report should be written in British (UK) English.

Beware of your tenses:
Past tense should be used when you describe about your
experiment.
Present tense should be used when you describe about a
theory or phenomenon that still exists.
Paper White simile A4 size paper (210 297 mm)
Printing Report must be computer typewritten using word processor and

printed double sided.
Printing must be of high quality. Text and figures must be clear
and legible.
Binding Staple on top left corner
Page Margin Left margin : 4.0 cm

Right, Top, Bottom margins : 2.5 cm
Header and Footer margins : 1.5 cm
Typesetting and Font Type : Times New Roman
Spacing Font Size : 12 pt
Section Title : Uppercase, Bold, Centred
Subsection Title : Title Case, Bold, Align left
Symbol for variable : Italic (e.g. m, P, T, v, , , )
General Spacing : 1.5 lines
General alignment for texts in paragraph should be justified.
Style Description
Numbers Avoid starting a sentence with a number or symbol.

Number has to be used together with course; if not it has to be spelled
out (e.g. three cats; not 3 cats).
If the number is between +1 and -1, the decimal marker is always
preceded by a zero (e.g. 0.15; not .15).
Numbers with many digits may be divided into groups of three by a thin
space, in order to facilitate reading. Neither dots nor commas are
inserted in the spaces between the groups (e.g. 43 765 589, 58.159 25;
15
not 43,765,589; not 58.159,25).

When there are only four digits before or after the decimal marker, it is
customary not to use a space to isolate a single digit (e.g. 5879, 1.5681)
When multiplying numbers, use only the multiplication sign with a
space before and after, not centre dot () nor the letter x or X (e.g.
25 5.3; not 25 5.3; not 25 x 5.3).
Units If possible, use SI units; although other commonly used non-SI units are
also acceptable (e.g. C for temperature, bar for pressure).
Spacing
One spacing between number and unit (e.g. 5 cm, 50 C, 30 %; not

5cm; not 50C; not 30%).
Exception for angular degree (), minute () and second () (e.g. 3, 45)
which are placed immediately after the number.
Symbols for Units
Use symbol for units and not their abbreviation (e.g. 5 s; not 5 sec.).
Symbols for units are written in upright type i.e. not italic (e.g. m for
metres, g for grams). This is to differentiate them from italic type
symbols used for variables (e.g. m for mass).
Symbols for units are written in lowercase, except for symbols derived
from the name of a person, which start with uppercase. However, the
unit name itself is written in lowercase.
(e.g. the unit for pressure is named after Blaise Pascal; the unit itself is
written as pascal whereas the symbol is Pa; 5 Pa or 5 pascal; 5 J or
5 joule; 5 N or 5 newton)
Symbols are not pluralised (e.g. 5 kg; not 5 kgs).
Symbols do not have an appended period / full stop (.) unless at the end
of a sentence.
Symbols derived from multiple units by multiplication are joined with a

space or centre dot () (e.g. N m for Nm). Hyphens (-) should not be
used (e.g. not N-m)
[Note: centre dot () is different from period / full stop (.); centre dot is
available under command Insert > Symbol].
Symbols formed by division of two units are joined with a solidus ( )

(slash ( / ) is also acceptable) or given as a negative exponent (e.g. m/s
or m s-1).
Only one solidus should be used (e.g. kgm-1s-2 or kg/(ms2); not

kg/m/s2).
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Do not mix unit symbols and unit names within one expression (e.g.
coulomb per kilogram; not coulomb per kg).
SI Prefixes Factor Name Symbol Factor Name Symbol
101 deca da 101 deci d
102 hecto h 102 centi c
103 kilo k 103 milli m
106 mega M 106 micro
109 giga G 109 nano n
1012 tera T 1012 pico p
1015 peta P 1015 femto f
1018 exa E 1018 atto a
1021 zetta Z 1021 zepto z
1024 yotta Y 1024 yocto y
Prefix symbols are attached to unit symbols without a space or hyphen

(-) between the prefix symbol and the unit symbol (e.g. km; not k m; not
k-m).
The same also apply for prefix names (e.g. kilometre; not kilo metre;
not kilo-metre)
Prefix symbols are written in upright type, i.e. not italic. (e.g. kPa; not
kPa).
All prefix symbols larger than kilo (103) are uppercase; the rest are
lowercase (see table above) (e.g. MW, GHz, kW, mg, nm).
All prefix names are lowercase, except at the beginning of a sentence
(e.g. megawatt, gigahertz, kilowatt, milligram, nanometre)
A prefix is never used in isolation; and compound prefixes are never
used (e.g. 10-9 m is nm or nanometre; not mm or millimicrometre).
Refer to http://www.bipm.org/en/si/si_brochure/ for more information on writing reports

using the International System of Units (SI).
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1.1 Heat Exchangers
Faculty Lee Kong Chian Faculty of Engineering and

Science
Department: Department of Chemical Engineering
Course Code and Name UEMK2411 Chemical Engineering Lab 1
Experiment No.: 1
Title of Experiment: Heat Exchanger
Laboratory Room No. and Name: KB508 Unit Operation Lab
Experiment Duration (hour): 4 hours
Number of Student per Group 5 Students
Equipment and Materials

Quantity estimation
Item Description *Item category (e.g. per set/group of
student)
Heat Exchanger Unit E 1
*Item category
SP Sample or specimen
C Consumable
C Chemical
H
W Labware, glassware, tool, and
components
E Equipment
S Software
1
1.2 Aims
To study different types of heat exchanger operation.

To study the effect of flow rate on heat transfer.
To perform energy balance around a heat exchanger.
To study temperature profiles across a heat exchanger.
To study and compare the heat losses, heat transfer coefficient and log mean
temperature difference at different setting and exchangers
1.3 Introduction
A heat exchanger is a piece of equipment built for efficient heat transfer from one
medium to another. The media may be separated by a solid wall, so that they never mix,
or they may be in direct contact. Most chemical processes involve heat transfer to and
from the process fluids.
The most commonly used heat-transfer equipment is the shell and tube heat exchanger.
Shell and tube heat exchangers consist of a series of tubes. One set of these tubes contains
the fluid that must be either heated or cooled. The second fluid runs over the tubes that
are being heated or cooled so that it can either provide the heat or absorb the heat
required.
Plate heat exchangers are used extensively in the food and beverage industries due to the
fact that they are easily taken apart for cleaning and inspection. Their used in other
industries will depend on the relative cost as compared to other types of heat exchanger
such as the shell and tube heat exchangers.
1.3.1 Theory
A) If the fluids both flow in the same direction, it is referred to as a co-current flow
type; if they flow in the opposite directions, then it is a counter-current flow type.
B) Conservation of energy
Heat transferred from hot fluid = Heat transferred to cold fluid + Heat Loss
C) The general equation for heat transfer across the tube surface in a shell and tube
heat exchanger is given by
2
q U o Ao Tm U i Ai Tm
where Ao = outside area of the tube, m2

Ai = inside area of the tube, m2
Tm = mean temperature difference, C
Uo = overall heat transfer coefficient based on the outside area of the
tube, kWm-2C-1
Ui = overall heat transfer coefficient based on the inside area of the tube,
kWm-2C-1
This is only the beginning, you need to find out more information about the tube-
side heat transfer coefficient (e.g. Sieder-Tate equation) and shell-side heat
transfer coefficient (Kerns method).
D) The mean temperature difference for both co-current and counter-current shell and
tube heat exchanger with single shell pass and single tube pass is normally
expressed in terms of log-mean temperature difference.
T1 T2
Tlm
ln T1

T2
1.3.2 The Heat Exchanger apparatus
The Heat Exchanger Apparatus provides avenue to collect the necessary experimental
data for the calculation of heat losses, heat transfer coefficient, log mean temperature
difference, etc. The effect of flow rate on the heat transfer rate and the temperature
profile can also be studied and may be applied for complex industrial heat exchangers.
3
Figure 1: Schematic Diagram for Heat Exchanger Training Apparatus
This unit consists of four different types of heat exchangers and two sump tanks for hot
and cold water source. The hot tank is fitted with an immersion type heater that is
protected against possible over heating. Each tank has a centrifugal pump which is
protected from dry-run by electronic level switches.
The four heat exchangers supplied with the unit are:

a) Shell and Tube Heat Exchanger
b) Spiral Heat Exchanger
c) Concentric (Double Pipe) Heat Exchanger
d) Plate Heat Exchanger
All necessary electronic sensors are fitted at respective locations for measuring the inlet
and outlet temperatures of the hot and cold water, and also the flow rates of the hot and
cold water streams. Digital indicators are provided on the control panel to read the
appropriate data.
4
1.4 Safety Precautions
Always check and rectify any leak.

Always make sure that the heater is fully immersed in the water.
Do not touch the hot components of the unit.
Be extremely careful when handling liquid at high temperature.
Always switch off the heater and allow the liquid to cool down before draining.
1.5 General Operating Procedures
Pre-experiment Procedures
1. Read and understand the theory of heat exchanger.

2. Read and understand the equipment used in the experiment (heat exchanger
apparatus).
3. Read the safety precautions before conducting the experiment.
General Start-Up Procedures
1. Perform a quick inspection to make sure that the equipment is in a proper working
condition.
2. Be sure that all valves are initially closed, except V1 and V12.
3. Fill up hot water tank via a water supply hose connected to valve V27. Once the tank
is full, close the valve.
4. Fill up the cold-water tank by opening valve V28 and leave the valve opened for
continuous water supply.
5. Connect a drain hose to the cold water drain point.
6. Switch on the main power.
7. Switch on the hot water tank heater and set the temperature to 50C. (Note:
Recommended maximum temperature set point is 70C)
8. Allow the water temperature in the hot water tank to reach the set point.
9. The equipment is now ready.
General Shutdown Procedures
5
1. Switch off the heater and wait until the hot water temperature drops below 40C.
2. Switch off pump P1 and pump P2.
3. Switch off the main power.
4. Drain off all the water in the process lines. Retain water in the hot and cold water
tanks for next laboratory session. (Note: If the equipment is not to be run for a long
period, drain all water completely.)
5. Close all valves.
1.6 Experimental
There are four heat exchangers in the apparatus shown. Depending on the timetable, you
are required to perform the experiment on either the:
i) Shell-and-tube heat exchanger, or

ii) Plate heat exchanger
You are required to perform experiment on both counter-current and co-current flow
arrangement for the type of heat exchanger that you are assigned to.
Your hot water tank temperature should be set to 50oC.
You will decide which valves to open and close to get the desired flow arrangement.
You will also decide what data you need to collect.
1.7 Results Analyses and Discussion
Although you are only required to perform experiment on either shell-and-tube heat
exchanger or plate heat exchanger, you are required to include and compare the result
between the two types of heat exchangers.
The Theory section provided minimal information for you to get started. You should do
extra research to find out more information (e.g. formula) to enable you to calculate
pressure drop, and heat transfer coefficients (for both tube-side and shell-side).
Discuss all your results. The topics below only serve as a guideline. Your discussion
should not only be limited to these topics.
i) What is the valves arrangement to get counter-current and co-current flow

arrangement?
ii) Which temperature indicators are used to measure the inlet and outlet
temperature of both hot water and cold water?
6
iii) Perform energy balance study. What is the heat transferred and heat loss?
iv) Calculate the LMTD
v) Calculate the heat transfer coefficient
vi) Calculate the pressure drop and compare that with the experimental result
vii) Perform temperature profile study and the flow rate effects on heat transfer
viii) Comparison between co-current and counter-current, shell-and-tube and plate
heat exchangers, in terms of topics covered in iii), iv), v), vi), vii).
ix) Errors and room for improvement
x) Discuss the advantage and disadvantage of using each type of heat exchangers
xi) Discuss the application of each type of heat exchangers
1.8 Equipment data
Shell and tubes heat exchanger
Length of tube = 0.5 m

Tube inner diameter = 7.75 mm
Tube outer diameter = 9.53 mm
Tube pitch = 18 mm
Tube surface area = 0.015 m2
Number of tubes = 10
Shell diameter = 85 mm
Baffle distance = 50 mm
Tube cross sectional area = 4.72 x 10-5 m2
Shell cross flow area = 2.00 x 10-3 m2
Shell equivalent diameter = 27.78 mm
Spiral heat exchanger
Tube diameter (inner and outer) same as shell and tube heat exchanger
Number of coils = 30
Diameter of coil = 78 mm
Plate heat exchanger
Nominal surface = 0.5 m2

Plate width = 124.46 mm
Plate length = 309.88 mm
Plate channel = 43.18 mm
Number of plates = 4
7
8
2.0 Cooling Tower Demonstration

Science
Experiment No.: 2
Title of Experiment: Cooling Tower Demonstrator

Quantity estimation
student)
Cooling Tower Demonstration Unit E 1
Distilled water C 8 liter
Beaker (500 mL) W 2
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
9
2.1 Aims
To determine the end state properties of air and water from tables or charts.
To determine energy and mass balances using steady flow equation on selected
system.
To investigate the effect of cooling load on Wet Bulb Approach.
To investigate the effect of air velocity on: (a) Wet Bulb Approach, (b) pressure
drop through the packing.
2.2 Introduction
Consider an air stream passing over the surface of a warm water droplet or film.
Assuming that the water is hotter than the air, then the water will be cooled down by
radiation, conduction, convection and evaporation. Radiation effect is normally very
small and may be neglected. Conduction and convection will depend on the temperature
difference, the surface area, air velocity, etc. The effect of evaporation is the most
significant where cooling takes place as water molecules diffuse from the surface into the
surrounding air.
2.2.1 Theory
Consider evaporation of a wet surface into the surrounding air. The rate is
determined by the difference between the vapour pressure at the liquid surface and the
vapour pressure in the surrounding air. The vapour pressure at the liquid surface is
basically the saturation pressure corresponding with the surface temperature, whereas the
total pressure of the air and its absolute humidity determines the vapour pressure in the
surrounding air. Such evaporation process in an enclosed space shall continue until the
two vapour pressures are equal. In other words, until the air is saturated and its
temperature equals the surface.
However, if unsaturated air is constantly supplied, the wet surface will reach an
equilibrium temperature at which the cooling effect due to the evaporation equals the heat
transfer to the liquid by conduction and convection from the air, which under these
conditions; will be at a higher temperature. Under adiabatic conditions, this equilibrium
temperature is the wet bulb temperature.
For a cooling tower of infinite size and with an adequate air flow, the water
leaving will be at the wet bulb temperature of the incoming air. Therefore, the difference
between the temperature of the water leaving a cooling tower and the local wet bulb
10
temperature is an indication of the effectiveness of the cooling tower. Thus, approach to

wet bulb an important parameter of cooling towers, which is the difference between the
temperature of the water leaving the tower and the wet bulb temperature of the entering
air.
Consider System A for a cooling tower as

defined in Figure 2.1. It can be seen that for
this system, indicated by the boundary line,
heat transfer at the load tank (Q) and

possibly a small quantity to
surroundings
work transfer at the pump (P)
low humidity air (a) enters at point A
high humidity air (a) leaves at point B
make-up water (E) enters at point E,
the same amount as the moisture
increase in the air stream
Figure 2.1: System A
v ab
va
1
Psychometric chart can be used to determine the value of the specific volume.
However, the values given in the chart are for 1 kg of dry air at the stated total pressure.
For every kilogram of dry air, there is kg of water vapour, yielding the total mass of (1
+ ) kg. Thus, the actual specific volume of the air/vapour (va) mixture is given by:
The mass flow rate of air and steam mixture through the orifice is given by
x
m 0.0137
va
x 1
0.0137
vab
m
where = mass flow rate of air/vapour mixture
11
va = actual specific volume

vab
= specific volume of air at the outlet
x = orifice differential, mm H2O
= humidity ratio of mixture
The mass flow rate of dry air is given by
1
m a mass flow rate of air/vapour mixture
1
1 x 1
0.0137
1 vab
x
0.0137
vab 1
(2.3)
A simplification can be made since in this application, the value of is unlikely to exceed
0.025. As such, neglecting wb would not yield significant error.
From the steady flow equation,
Q P H out H in
ma hda ms hs (mg hda ms hs ) A mE hE
The pump power, P is a work input, therefore it is negative.
If the enthalpy of the air includes the enthalpy of the steam associated with it, and this
quantity is in terms of per unit mass of dry air, the equation may then be written as:
QPm
a (hB hA ) m
E hE
The mass flow rate of dry air, ma through a cooling tower is constant, whereas the mass
m E hE
flow rate of moist air increases as the result of evaporation process. The term can
usually be neglected since its value is relatively small.
Under steady state conditions, by conservation of mass, the mass flow rate of dry air and
of water (as liquid or vapour) must be the same at inlet and outlet to any system.
Therefore,
m a A m a B m a A m E m a B E m
m a B m
aA
and or
12
The ratio of steam to air is known for the initial and final state points on the
psychrometric charts. Therefore, the mass of make-up water should be equal to the
difference between the moisture content between the inlet and the outlet of the air (a).
Lets redefine the cooling tower system to be

as in Figure 2.2 where the process heat and
pump work does not cross the boundary of
the system.
In this case warm water enters the system at

point C and cool water leaves at point D.
Figure 2.2: System B
Q P H out H in
Again from the steady flow energy equation, , where P = 0.
Q
may have a small value due to heat transfer between the unit and its surroundings:
Q m a hB mw hD m a hA m w hC m E hE
Rearranging,

Q m a hB h A m w hD hC m E hE
Q m a hB h A m w C p t D t C m E hE
13
m E hE
Again, the term can be neglected.
2.2.2 The Cooling Tower Equipment
The water cooling tower is designed to demonstrate the construction, design and
operational characteristics of a modern cooling system. The unit resembles a full size
forced draught cooling tower and it is actually an open system through which two
streams of fluid (in this case air and water) pass and in which there is a heat transfer from
one stream to the other.
The unit contains:
Load tank:
o 9 Litres tank fitted with 0.5 kW and 1.0 kW heaters, totalling up to 1.5 kW
heating.
Make-up tank:
o Tank fitted on top of the load tank.
Pump:
o 40 W centrifugal pump to circulate water.
Air distribution chamber:
o Centrifugal fan with the capacity of providing 235 cfm air flow.
o Air flow rate can be adjusted by a Perspex intake damper.
Tower:
o Dimension of 15 cm 15 cm 60 cm.
o Fitted with 8 decks of inclined packing.
o Packing density of 110 m2/m3 for Tower A and 200 m2/m3 for Tower B.
Water circuit:
o Circulates water from the load tank to the top of the tower and back to the
load tank for recirculation.
Air circuit:
o Air is drawn in from the atmosphere by the centrifugal fan and is
circulated from the bottom of the tower and leaves at the top of the tower
to the atmosphere.
Temperature sensors:
o T1 Dry Bulb Inlet Air Temperature
o T2 Wet Bulb Inlet Air Temperature
o T3 Dry Bulb Outlet Air Temperature
o T4 Wet Bulb Outlet Air Temperature
o T5 Inlet Water Temperature
o T6 Outlet Water Temperature
o T7 Make-up Tank Temperature
14
o T8 Hot Water Tank Temperature

Differential pressure sensor:
o V5 remains open at all times.
o Orifice differential pressure: open V4.
o Pressure drop across packing: open V3 and V6.
All operating instructions supplied must be read carefully and understood before
attempting to operate the unit.
Keep hands away from the blower when it is running to avoid serious injury.
Do not connect the power if the unit is damaged or even partially wet.
Do not touch the hot component of the unit.
Do not set the heater temperature above its maximum operating temperature of
70C to avoid pump damage.
Do not use pliers or other tools to tighten the screws. Use only bare hands. Over
tightening could damage the seals and cause leakage.
Exercise caution when pouring water into the make-up tank to ensure no water is
spilt onto the electrical parts.
Start-up:
1. Close V1 to V6. Open V5. Partially open V7.

2. Fill make-up tank until the zero mark.
3. Add distilled water to fill up the wet bulb sensor reservoirs.
4. Set the temperature controller set point to 50 C. Switch on the 1.0 kW water
heater and heat up the water to approximately 40 C.
5. Switch on the pump and slowly open the control valve V1 and set the water
flowrate to 2.0 LPM. Obtain a steady operation where the water is distributed and
flowing uniformly through the packing.
6. Fully open the fan damper and then switch on the fan. Check that the differential
pressure sensor is giving reading when the valve manifold is switched to measure
the orifice differential pressure.
7. Let the unit run for about 10 15 minutes for the float valve to correctly adjust the
level in the load tank. Refill the makeup tank as required.
8. The unit is now ready.
Shut down:
15
1. Switch off the heaters and let the water circulate through the cooling tower system
for 3 5 minutes until the water cooled down.
2. Switch of the fan and fully close the fan damper.
3. Switch off the pump and power supply.
4. Retain the water in reservoir tank for next experiment or completely drain off the
water from the unit if it is not in used.
16
2.5 Experimental
Experiment 1: Determination of the end state properties of air and steady flow
equations.
Set the system to the required operating conditions:
Water flow rate: 2.0 LPM

Air flow: maximum
Cooling load: 1.0 kW
Determine (in intervals of 10 minutes):
Make-up water supply.

Temperatures T1-T7.
Orifice differential pressure.
Heater power (Q).
Experiment 2: Determination of the effect of cooling load to the wet bulb approach.
Similar to the operating conditions of experiment 1, vary the cooling load to determine:
Temperatures T1-T7.
Heater power (Q).
Experiment 3: Determination of the effect of air velocity to the wet bulb approach
and pressure drop.
Similar to the operating conditions of experiment 1, vary the air flow to determine:
Temperatures T1-T7.
Pressure drop across packing.
17
Discuss all your results. The questions below only serve as a guideline. Your discussion
should not only limited to these questions.
Experiment 1:
1. Calculate the make-up rate (kg/s).

2. Verify the mass and energy balance using the steady flow equation (for both
System A and System B). Calculate the percentage error. Discuss your findings.
3. Discuss on the difference (if any) obtained between your calculations done by
using System A and System B.
Experiment 2:
1. Calculate the wet bulb approach and total cooling load.

2. Show the relationship between the approach to wet bulb and the total cooling load.
Discuss your findings.
Experiment 3:
1. Calculate the nominal air velocity.

2. Show the relationship between the nominal air velocity and the approach to wet
bulb. Discuss your findings.
3. Show the relationship between the nominal air velocity and the pressure drop
across packing. Discuss your findings.
Further discussion:
1. State, with support from the literature, a few applications that are similar to the
cooling tower demonstration system.
2. Discuss on the effects of tower packing density to the efficiency of the cooling
tower.
18
3.1 Tray Drying

Science
Experiment No.: 3
Title of Experiment: Tray Drying

Quantity estimation
student)
Tray dryer E 1
Fine sand C 1.5 kg
Distilled water C 2 liter
Timer W 1
Analytical balance E 1
Beaker (100 mL) W 2
Water dispenser W 1
Spatula W 1
Tray (rectangular) W 2
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
19
3.2 Aims
To perform drying test on solids.

To investigate the effects of air velocity on drying rate.
To perform heat and mass transfer analysis of a drying process.
3.3 Introduction
3.3.1 Theory
Drying is one of the food preserving methods beside canning and freezing. It prevents
deterioration by reducing the moisture content of food. In the absence of sufficient water,
the bacteria which cause food spoilage and decay are unable to grow and multiply. Many
of the enzymes which promote undesired chemical changes in the food cannot function
without water.
For effective drying, air should be hot, dry and moving continuously. The water
contained in the food will be vaporised by the hot dry air. For this to happen, latent heat
of vaporization must be supplied to the process.
There are two important process-controlling factors in the operation of drying:
(i) transfer of heat to provide the necessary latent heat of vaporisation and
(ii) movement of water or water vapour through the food material and then away
from to separate the water from the food.
The size of pieces, relative moisture, flow rate and temperature of the moving air will
affect the time required for drying. All these factors are inter-related.
Tray drying should follow the law of conservation of mass and energy. When a sample
does not undergo any chemical reaction, the total mass in should be equal to the total
mass out. Same goes to energy, the total energy supplied will be transferred to heating the
specimen and can be calculated based on the latent and sensible heat of both the specimen
and the moisture content.
In general, drying rate can be divided into two distinct phases: the constant rate period
and the falling rate period. Figure 3.1 illustrates the two drying phases.
In the constant rate period the surface of the food remains wet and it can therefore be
spoiled by moulds and bacteria. In the falling rate period the surface is dry and the risk of
spoilage is much smaller. The food should therefore be dried to a weight that corresponds
to the end of the constant rate period as quickly as possible.
20
Figure 3.1
By calculating the drying rate for each

period, graph for drying rate versus
moisture content can be plotted as
shown in Figure 3.2:
Figure 3.2 gives two important pieces of information: (1) the actual drying rate during the
constant rate period which shows the efficiency of the drier, (2) the final moisture content
of the dried food which shows whether it will be stable during storage.
Figure 3.2
initial weight final weight

Drying rate
time interval
The moisture content of both the fresh food and the final dried food can be found by
weighing the fresh food, then heating it at 100C in an oven for 24 hours and reweighing.
The moisture content is found as follows:
initial weight final weight

Moisture Content (%) 100%
initial weight
21
(3.2)
Other values of moisture content during the drying period can be found by relating these
two results to the weights of food recorded during the drying experiment and applying
similar factors to intermediate weights.
The efficiency of the dryer can be determined by looking at a heat balance over the air,
treating the dryer as adiabatic with no exchange of heat with the surroundings. The heat
transferred to the food for drying corresponds to the drop in temperature in the drying air,
and the heat which has to be supplied corresponds to the rise of temperature of the air in
the air heater. So this adiabatic air-drying efficiency, can be defined by
T1 T2

T1 Ta
where T1 = inlet (high) air temperature into the dryer, C

T2 = outlet air temperature from the dryer, C
Ta = ambient air temperature, C
The numerator, the gap between T1 and T2 is a major factor in the efficiency.
3.3.2 The Tray Dryer
There are three types of drying:
Air and contact drying under atmospheric pressure;

Vacuum drying;
Freeze drying.
The tray dryer uses the first concept, where air flow is subjected at a required temperature
to dry the sample.
The tray drying unit contains:
Temperature sensors (T1-T4):

o T1 Dry bulb temperature before tray
o T2 Wet bulb temperature before tray
o T3 Dry bulb temperature after tray
o T4 Wet bulb temperature after tray
Axial fan
Heater
Weighing balance
22
Do not touch the chamber when the experiment is running. The surface is hot.
Do not switch ON the heater if the fan is OFF.
Always handle the trays with gloves.
Do not place weight of more than 6 kg on the scale.
Keep away from the front and rear side of the chamber.
Start-up:
1. Moist the wet bulb sensors (before and after the tray) with water.
2. Turn on the power supply.
3. Set the axial fan speed to 8 Hz and start running it.
4. Turn on the heater and set it to 65 C.
5. Unit is ready when the temperature reaches approximately 60 C.
Shut down:
1. Switch off the heater and let it cool for approximately 10 15 minutes.
2. Switch off the axial fan.
3. Switch off the mains.
3.6 Experimental
Experiment 1: Determination of the drying profile of moist sand.
Operating conditions:
Heater temperature: 65 C
Axial fan speed: 8 Hz
Mass of dry sand: 500 g
Moisture content: 10 15 %
Determine:
Mass of moist sand every 10 minutes.

Temperatures T1 T4.
Experiment 2: Determine the effects of air velocity on drying rate.
23
Similar to the operating conditions of experiment 1, develop an experiment to compare

the effects of air velocity on drying.
should not only limit to these questions.
1. Determine the change of moisture content with time. Discuss your findings.
2. Determine the change of drying rate with moisture content. Discuss your findings.
Further discuss this with comparison from the literature.
3. Calculate the heat transferred from the air to the sand.
4. Comment on the humidity of the tray dryer before and after drying. Compare this to
the literature. Discuss your discrepancies / similarities.
5. Determine the dryer efficiency.
6. Discuss on the effects of air velocity to drying regime. Compare your findings to the
literature.
24
4.1 Vapour-Liquid Equilibrium (VLE)

Science
Experiment No.: 4
Title of Experiment: Vapor Liquid Equilibrium

Quantity estimation
student)
Vapor Liquid Equilibrium Unit E 1
40 v/v % ethanol-water mixture CH 5 liter
0 v/v % ethanol-water stock solution CH 250 mL
Refractometer E 1
Dripper C 10
Beaker (100 mL) W 10
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
25
4.2 Aims
To find VLE relationship for binary mixture.

To plot the equilibrium curve.
4.3 Introduction
Vapour-liquid equilibrium (VLE) is defined by the condition where a liquid and its
vapour phase are in equilibrium with each other. Under this state or condition, there is no
net change in vapour-liquid phases thus the rate of evaporation (liquid to vapour) is equal
to the rate of condensation (vapour to liquid).
In theory, the state of equilibrium would take forever to be reached but such equilibrium
can be practically achieved within a closed system where the liquid and vapour are
allowed to stand in contact with each other long enough with literally no interference or
only slight interference from the exteriors.
4.3.1 Theory
The concentration of a vapour in contact with its liquid, especially at equilibrium, is

often given by the vapour pressure. The equilibrium vapour pressure of a liquid is
very much dependent on temperature. In the state of equilibrium, a liquid mixture
with individual components in certain composition will have an equilibrium vapour in
which the partial pressures of the vapour components will have certain set values
depending on all of the liquid component compositions and the temperature. This is
also true in reverse whereby a vapour with components at certain composition or
partial pressure is in equilibrium with its liquid, thus the component composition of its
liquid will be dependent on the vapour composition and the temperature.
The equilibrium composition of each component in the vapour phase is often different
from the composition of its liquid phase without a correlation. Such equilibrium
phase data can be determined from a simple experiment with multicomponents of
vapour-liquid mixtures. Most binary component mixtures' equilibrium data can be
found in texts and references. In certain cases, estimation or prediction of equilibrium
data behaviour can be done using theories such as Dalton's Law, Raoults Law or
Henry's Law.
In multicomponent mixtures, the compositions of each component are compared in

both the liquid and vapour phases where the compositions are expressed in mole
fractions. A mole fraction is the number of moles of a certain component divided by
the total number of moles of all components in the mixture in either the liquid or
26
vapour phase. VLE data are often produced and shown in two component systems
(binary) and three component systems (ternary). However, VLE data can exist in
higher order of components but would be complex and difficult to illustrate
graphically.
4.3.2 Vapour Pressure
Vapour pressure is defined as the pressure exerted by the gaseous phase under
equilibrium state. It depends significantly on the surrounding temperature. In
addition, it is known as partial pressure of a component when there is a mixture of
gases present within the vapour.
A vapour with components at certain concentration will have a corresponding

equilibrium liquid concentration. The concentration or partial pressure of the liquid
components will have certain set of values depending on the vapour component
concentrations and the operating temperature. Similarly, this also applies to liquid
with components.
For ideal gas the partial pressure of Component 1 (p1) is given by Dalton's law,
p1 y1 P1
Raoult's Law expressed the partial pressure in terms of vapour pressure of the liquid
where
p1 x1 P1vap
However, this law is only applicable to ideal solutions with high value of x1.
Generally a point is reached where the vapour pressure no longer follows the ideal
relationship as x1 gradually decreases.
Both Dalton and Raoult's Laws can be combined to yield an equation that relates the
vapour and liquid compositions:
x1 P1vap
y1
P
For a dilute real solution, Henry's Law is used to determine the partial pressure of the
component:
27
p1 K x1
where K is the Henry's constant but it is not equal to the vapour pressure of pure
solute.
4.3.3 Non-Ideal Behaviour
For non-ideal system whereby the mixtures no longer obey Raoult's law or Henry's
P1vap
law, activity coefficient, is used to relate x1, y1, and P as follows:
x1 1 P1vap
y1
P
The liquid phase activity coefficients depend on temperature, pressure and

concentration.
4.3.4 Temperature
Temperature has an effect on the VLE of a system since at different temperatures

there will be a corresponding set of liquid and vapour compositions under a constant
pressure. These two compositions are in equilibrium with one another at that
particular point.
For an ideal binary mixture, the relationship between T-x-y at a constant pressure can
be represented in a plot called the phase diagram as depicted in Figure 4.1 below:
28
Temperature
vapour
liquid
x1 y1
Figure 4.1: Phase Diagram
At a particular temperature T1, there will be a corresponding equilibrium composition

x1 and y1 for the liquid and vapour phase respectively.
4.3.5 Relative Volatility
Relative volatility, 12 is an indication on how easily or difficult a particular

separation will be. It is a measure of the difference volatilities between two
components (1 and 2). Ideally, relative volatility can be defined as the ratio of
fraction of a component in the vapour phase to that in the liquid phase where it could
be represented as follows:
y1 / x1
12
y 2 / x2
29
For a binary mixture, the relation can be simplified to:
12 x1
y1
1 12 1 x1
This relationship is only valid when 12 is constant. In actual cases, it varies with
temperature (increases as temperature falls). Yet it remains remarkably steady for
many systems.
4.3.6 Refractive Index
When a chopstick is dipped in water in a glass, it looks bent. If the chopstick is

dipped in thick sugar water, it looks more bent. This phenomenon arises from the
refraction of light beam.
An-increase in concentration of a solution will yield a higher refractive index. When

the refractive index of air at the atmospheric pressure is 1 and a beam of light
penetrates a certain medium %, the ratio between the sine of refraction angle and
the sine of incident angle a to the normal line is called the refractive index of the
medium.
n 1 air
medium X
sin
nX
sin
Figure 4.2: Refraction of Light Beam
30
Since refractive index varies depending on wavelength of light and temperature, it is

t
nD
expressed as , where n = refractive index, t = temperature, D = D-ray of sodium
(589 nm).
When the refractive index of water whose temperature is 20C is measured with D-
ray, it is expressed as: nD20 = 1.33299 or usually expressed as nD = 1.33299.
4.3.7 The VLE Apparatus
The vapour-liquid equilibrium apparatus is designed to study the vapour and liquid
equilibrium of mixtures. The composition relationship between vapour and liquid
equilibrium for binary and multicomponent mixtures at atmospheric and elevated
pressures can be determined.
The unit comprised of a main insulated evaporator made of stainless steel connected
to an overhead condenser. The cooling water flow rate into the condenser can be
regulated with a gate valve and is measured with a flow meter. A coil heater provides
the necessary heat to evaporate the liquid mixture with preset temperatures controlled
by a digital temperature controller. Vapour rises to the top of the unit is then
condensed in the condenser.
Vapour and liquid products are collected in a stainless steel vessel located at the
sampling port lines. A feed port for dosing and sampling ports are provided. Digital
meters are installed on the control panel to display the temperatures and pressures in
the system. A pressure relief valve is connected to the unit to ensure the system will
not be over-pressured at all time. Full jacket insulation ensures minimal heat loss
within the unit.
31
Pressure Relief Valve

Temperature Meter
and Controller Condenser
Pressure Meter
Evaporator Inlet
Insulated Stainless
Control
Steel Evaporator
Panel
Vapour Sampling
Cooling Water
Inlet Valve Liquid Sampling
and Drain
Cooling Water Drain
Figure 4.3: Vapour-Liquid Equilibrium Apparatus
Always wear safety glasses, mask and gloves when handling chemicals. Do not allow
the solution to come into contact with your skin or eyes.
Should any chemicals come into contact with the body, rinse off immediately with
plenty of water and inform the laboratory instructor/officer. Seek medical treatment if
symptoms persist.
Ensure that there is no source of ignition, such as a Bunsen burner, gas flame, hot
plate, hot air gun or hot water pipe near the working area.
Ethanol releases irritating vapours; avoid inhalation and work in a well-ventilated
area.
Good ventilation is essential so that it is not possible for high concentrations of
alcohol vapour to form.
Dispose of all unused chemicals in an appropriate manner after the experiment.
Under no circumstances should the chemicals be allowed to flow into sinks or drains.
Wash your hands thoroughly with soap after the experiment.
Do not switch on the heater if there is no liquid in the evaporator.
Do not pressurise the apparatus for more than 10 bars.
32
Do not boil the liquid in the apparatus for more than 100C.
Do not touch the evaporator (it is hot) and condenser when conducting the
experiment.
Be careful when pouring the test liquid into the evaporator vessel.
Be careful when taking the sample from the sampling port as the product is hot.
4.5 Chemical Hazards
Ethanol is very flammable. It evaporates readily, so it is possible for dangerous levels

of vapour to build up, perhaps reaching a point at which an explosion is possible if a
source of ignition is present.
If ethanol is in contact with oxygen over a long period, explosive peroxides may be
formed. These typically have a higher boiling point than ethanol, so may become
concentrated in the liquid if ethanol is distilled. Therefore, bottles of ethanol, once
opened, should not be stored indefinitely, in order to avoid any risk of peroxide
formation.
Ethanol is very flammable. It can be ignited by flames, but also by contact with items
such as hot plates or hot air guns.
1. Read and understand the theory of vapour-liquid equilibrium.

2. Read and understand the equipment used in the experiment (VLE apparatus).
3. Read the safety precautions and chemical hazards before conducting the experiment.
4. Read the Material Safety Data Sheet (MSDS) for the chemicals (i.e. ethanol) used in the
experiment
5. Prepare the following apparatus and materials needed for the experiment:
Refractometer
Beakers
Syringe / Dripper
Prepare 5 L of ethanol-water mixture
Other Consideration:
33
Measured value for liquid sample changes depending on the change of temperature.
Therefore, samples' temperature must be kept constant.
Do not wet the refractometer with sample liquid unreasonably. If the refractometer gets
wet excessively, it may cause malfunction and breakdown of the refractometer.
Do not tap or pick at the prism surface with a metal spoon, tweezers, etc. because the
prism surface is made of optical glass. If the prism surface is scratched, the refractometer
may fail in measurement.
When measurement is complete, wipe up sample from the prism surface and its
surroundings with soft tissues moistened with water first, and then wipe the wet parts
with dry tissues to dry them up.
After measurement of a sample of a high molecular compound (e.g. oil, fat etc) wipe the
prism surface with tissues moistened with alcohol or neutral detergent first and then wipe
it up again with dry tissues to dry up.
On ending a day's measurement, turn off the power switch.
4.7 Experimental
Experiment 1A: Vapour-Liquid Equilibrium
1. Close the liquid sampling and drain valve.
2. Open the vapour sampling valve and the evaporator inlet valve.
3. Pour ethanol-water mixture into the evaporator. (Caution: The person who pours the
mixture should wear a face shield.)
4. Close the vapour sampling valve and the evaporator inlet valve.
5. Turn on the power supply and main power switch at the front of the control panel.
6. Set the temperature to 75C.
7. Connect the cooling water drain port to drain.
8. Connect the laboratory water supply to the cooling water supply port. Tighten it with
clip.
9. Switch on the heater power supply located at the control panel.
10. Turn on the water supply and allow the water to flow into the condenser. Set the water
flow rate to 12 LPM.
11. Keep an eye on the temperature. When the temperature reaches the set point, wait for
another 5 minutes to allow the system to reach equilibrium, and then record down the
temperature and pressure.
34
12. Take a sample solution from the vapour sampling port and the liquid sampling port.
(Caution: Be careful when taking the sample from the valves.)
13. Label the samples (i.e. temperature, pressure, x-component, y-component).
14. Close both vapour and liquid sampling valves.
15. Use a refractometer to determine the samples' refractive index (RI). (Reminder: You
must take a few readings to obtain the average reading.)
16. Repeat Step 11 to Step 15 with 5C increment until the set temperature reaches 95C.
Experiment 1B: Refractive Index (RI) Measurement of Liquid Sample
1. Open the secondary prism of the refractometer and drip 2 or 3 drops of sample liquid
onto the centre part of the main prism surface. Gently close the secondary prism. The
sample will spreads between the main prism and secondary prim as a thin film.
2. While observing through the eyepiece, gently turn the measurement knob until the
boundary line appears in the field of refraction view. At that time, the boundary line may
be coloured and unclear because it is not yet achromatised.
3. Turn the measurement knob in a wide range so as to set it at a point where the field of
refraction view clearly changes from bright field to dark field or vice versa. The
brightness of the field can be adjusted with the illumination selector switch in the upper
part of the digital thermometer.
4. Turn the colour compensator knob to achromatise the boundary line so that the line
appears clearly in the field. Turn the measurement knob again to set the boundary line at
the intersection of the cross hairs.
5. The upper scale is for reading refractive index (nD) while the lower scale is for Brix
percent. Since the minimal graduation unit for refractive index is 0.001, the scale can be
read at a unit of 0.0001 with the eye.
1. Sketch a schematic diagram, including all valves and sensors/controllers, for the VLE
unit used in the experiment. Label all valves and instruments.
2. Plot a graph of vapour composition (y) versus liquid composition (x) and discuss the
findings.
3. Plot a T-x-y graph and discuss the findings.

35
36
5.1 Liquid Diffusion Coefficient

Science
Experiment No.: 5
Title of Experiment: Liquid diffusion coefficient

Quantity estimation
student)
Conductivity meter with probe E 1
J tube with capillaries E 1
Sodium chloride solution 0.5 M CH 2 liter
Deionised water C 3 liter
Magnetic stirrer bar W 1
Magnetic stirrer W 1
Timer E 1
Measuring cylinder (100 mL) W 1
Stirrer rod W 1
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
37
5.2 Aims
To determine the liquid diffusion coefficient of NaCl solution.
5.3 Introduction
5.3.1 Theory
When a concentration gradient exists within a fluid consisting of two or more components,
there is a tendency for each constituent to flow in such a direction as to reduce the
concentration gradient. This is known as mass transfer. It takes place in either a gas or a
liquid phase or in both phases simultaneously.
Rate of diffusion is given by
C
J D
x
where J = diffusion flux across unit area to the x-direction (right side), mol/cm2s
D = diffusivity, cm2/s
C mol/cm 3
x cm
= concentration gradient in the x-direction,
The negative sign indicates that flow is from high to low concentration.
By expanding Eq. (1) using respective terms constitutive relations, we get
V dk d 2 M
D N
CM dt 4 x
Rearranging gives
4Vx dk
D
d NMCM dt
2
where V = volume of water in diffusion vessel, L

x = length of capillaries, cm
38
d = diameter of capillaries, cm
N = number of capillaries
M = molar concentration of NaCl solution, mol/L
CM
= conductivity change per unit molar concentration change, S/mol/L-1
dk
dt
= rate of conductivity change over time
5.3.2 The Liquid Diffusion Apparatus
The liquid diffusion unit contains:
J-tube with capillaries

o To insert electrolytes to test for its diffusion
Diffusion vessel
Conductivity meter with probe
Magnetic stirrer and stirrer bar
All operating instructions supplied with the unit must be carefully read and understood
before attempting to operate the unit.
Feed stock which severely affects PTFE, PFA, PVC and borosilicate glass are not to be
used.
The system should not be subjected to shock, sudden impact, vibration, additional load, or
permanent external action of aggressive vapours.
Always check and rectify any leakage.
Do not use any coarse or abrasive cleaners on glass and plastic components.
Leaking couplings or fittings should be carefully retightened.
Start-up
1. Prepare the following solutions (200 mL each):

0.5 M NaCl
1.0 M NaCl
39
1.5 M NaCl
2.0 M NaCl
2. Insert deionised water into the diffusion vessel and connect the
conductivity probe to the conductivity meter.
3. Check the diffusivity of deionised water. It should give a relatively
low conductivity reading.
4. Check for any leakages around the J-tube.
5. Insert the stirrer bar into the vessel and start stirring at a
predetermined stirring speed.
Shut down
1. Stop stirring and switch off the magnetic stirrer.

2. Switch off the conductivity meter and unplug the probe.
3. Wash and rinse the vessel and J-tube thoroughly. Have a final rinse with deionised
water and wipe them clean for the next group of users.
5.6 Experimental
Experiment 1:
Determine the conductivity change per unit time for different concentrations of NaCl
solutions.
Experiment 2:
Determine the conductivity change per unit concentration for different NaCl solutions.
1. Determine the liquid diffusivity for different concentrations of

NaCl solution. Compare and discuss your findings.
2. Compare your findings in (1) with the literature. Calculate the percentage error and
discuss on the discrepancies (if any).
3. Predict the change in conductivity per unit time if a different electrolyte is used (e.g.
CaCl2, KCl, Na2CO3, etc.).
4. Provide a possible suggestion to improve the experimental apparatus in order to improve
the experimental data obtained.
40
6.1 Gas Absorption

Science
Experiment No.: 6
Title of Experiment: Gas absorption

Quantity estimation
student)
Gas absorption demonstration unit E 1
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
41
6.2 Aims
To determine the mass transfer coefficient of oxygen (O2) through wetted wall
absorption column.
6.3 Introduction
Gas absorption is a process widely used in industry in which a gaseous mixture is

brought into contact with a liquid. The gas mixture is contacted with a liquid
(absorbent / solvent) to selectively dissolve one or more components from the gas to the
liquid. The components transferred to the liquid are referred to as solutes / absorbate.
Liquid is permitted to flow down the inside surface of a circular pipe while a gas is
blown upward through the central core.
Absorption is used to separate gas mixtures such as remove impurities, contaminants,

pollutants or used to recover valuable chemicals.
6.3.1 Theory
The concentration profile of a diffusing species during mass transfer between two
phases is illustrated in the following figure:
GAS LIQUID
PA
PAi xL = liquid film thickness

xg = gas film thickness
cAi
cA
xg xL
Figure 6.1: Mass Transfer between Gas and Liquid
42
Following the two films theory of Lewis and Whitman, the rate of mass transfer is:
kL
N A k g ( p A p Ai ) k L (c Ai c A ) ( p Ai PA )
H
where pA = partial pressure

cA = concentration
kg = gas phase mass transfer coefficient
kL = liquid phase mass transfer coefficient
NA = rate of mass transfer per unit area of component A (example unit: g/m2.s)
In this experiment, this is given as:

volumetric flow rate C out C in
NA
gas/liquid interfacia l area
Writing the rate of mass transfer in terms of bulk gas partial pressure and bulk liquid
concentration, we obtain:
N A K g ( p Ag p *A )
N A K L (c*A c AL )
where Kg = overall mass transfer coefficient when driving force is

expressed in terms of pressure
KL = overall mass transfer coefficient when driving force is
expressed in terms of concentration
where cA* can be obtained from Henrys law:

p Ai * Hc Ai *
From the mechanism of mass transfer, it can be expected that the liquid film mass
transfer coefficient would depend on diffusivity D, liquid flow rate u, liquid viscosity
, liquid density , acceleration of gravity g and film thickness, L. The dimensionless
equations should be:
43
( Sh) L (Re) nL
n
KLL 4w / W

D L L
where w = liquid mass flow rate

W= the perimeter (width) of the liquid film
Sh = Sherwood number
Re = Reynolds number
6.3.2 The Gas Absorption apparatus
This wetted-wall absorption column is designed to study the absorption of oxygen

from air into de-oxygenated water, prepared by purging with nitrogen gas. The
absorbing liquid is stored in a tank (D1) and is pumped (G1) to the top of the
deoxygenated column (C2) adjacent vertically to the absorption column; the water is
deoxygenated with nitrogen purged at the bottom of the column (C2).
From the bottom of column (C2), the deoxygenated water is pumped (G2), via a
rotameter (FI2), to the top of the absorption column (C1). The flow rate should be
controlled using a valve and must be sufficient to completely wet the inside surface of
the column but do not cause excessive rippling of liquid.
Air is pumped by a compressor (P1) into the base of the column (C1) via a rotameter
(FI1). The air passes up the column (C1), transferring the oxygen to the water. The
concentration of dissolved oxygen and temperature of the liquid entering and leaving
the absorption column (C1) are measured by two probes (AI1 and AI2) at the inlet and
outlet.
The water drains from the absorption column (C1) into the storage tank (D1) and
recycles back to the deoxygenated column via a pump (G2).
All operating instructions supplied with the unit must be carefully read and
understood before attempting to operate the unit.
Always check and rectify any leakage.
44
1. Read and understand the theory of gas absorption.

2. Read and understand the equipment used in the experiment (gas absorption column).
1. Turn off the nitrogen supply by closing the supply valve V1 on the deoxygenator
column.
2. Turn off the compressor P1 and both the pumps G1 and G2.
3. Switch off the main power.
6.6 Experimental
1. Set the pressure reducer on the nitrogen cylinder at 0.5 1 bar.
2. Fill the tank D1 with distilled water.
3. Switch on pump G1 and adjust valve V3 very slowly and carefully. (Note: open this
valve very slowly and carefully to avoid overfilling the deoxygenated column)
4. Switch on pump G2 and adjust the flow rate using the micro valve on flow meter
FI2.
5. Ensure that the wetted-wall column is completely wetted uniformly.
6. Switch on the compressor P1 and adjust the flow rate using the micro valve on flow
meter FI1.
7. Feed nitrogen into the deoxygenated column by opening valve V1 very slowly and
carefully. A steady stream of nitrogen bubbles is sufficient to effectively strip
oxygen from water.
8. Record the oxygen concentration reading by probe AI1 and AI2 and their
temperature.
9. After the experiment, shutdown the unit as per general shutdown procedures in
Section .
45
Discuss all your results. The questions below only serve as a guideline. Your discussion is
not only limited to these questions.
1. Perform the related calculation and plot Sh vs Re to determine the slope.
2. Discuss and compare the result from the experiment with literature.
You will require the following information for your calculation:
Column diameter = 0.34 m
Column height = 0.9 m
46
7.0 Batch Distillation Column

Science
Experiment No.: 7
Title of Experiment: Batch Distillation

Quantity estimation
student)
Batch distillation column E 1
Refractometer E 1
Dripper C 10
Beaker (100 mL) W 10
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
47
7.1 Aims
To understand the principles of distillation column.

To determine the composition of a mixture by using refractive index.
To determine the variation of top product against time at constant reflux ratio.
To investigate the effects of constant reflux ratio and regulating reflux ratio on
product composition.
To determine the temperature profile along the height of the column.
7.2 Introduction
Distillation process is widely applied in industry for separation operations. It is a

process in which a liquid or vapour mixture of two or more substances is separated into
its component fractions of desired purity by the application and removal of heat.
Distillation processes depends on the distribution of components between gas and
liquid phase.
The more volatile, light or low boiling, components will concentrate in the vapour.
The less volatile, heavy or high boiling, components will concentrate in the liquid
phase.
Separation of components from a liquid mixture via distillation depends on the

differences in boiling points of the individual components. Also, depending on the
concentrations of the components present, the liquid mixture will have different boiling
point characteristics.
The simplest distillation is the separation of binary mixtures. The typical binary
equilibrium curves, usually plotted for the more volatile component are shown in the
Figure 7.1. Curve A is the most common case where the more volatile component
remains more volatile throughout the entire composition range.
Curve B is a system with homogeneous azeotrope, where the component which is more
volatile at low values of x1 and becomes less volatile at high values of x1. The vapour
and liquid compositions are equal when the curve crosses the x = y line. The maximum
overhead product composition achievable with a feed of x1 = 0.25 is the azeotropic
composition. Similarly, the maximum bottoms product composition can be no lower
than the azeotrope composition for a feed with x1 = 0.9.
48
Curve C is a system with heterogeneous azeotrope, or two liquid phases in equilibrium

with one vapour phase. The azeotrope determines the maximum possible separation
achievable by simple distillation.
Figure 7.1: Typical Binary Equilibrium Curves
7.2.1 Theory
Batch distillation is a process commonly carried out in small plants to recover volatile
products from a liquid solution. The liquid mixture is charged into a still or reboiler,
and heat is supplied through a heating coil or jacket to partially vaporise the mixture.
The most basic method of operation is to directly take the vapours to a condenser.
The vapour that leaves the still is always in equilibrium with the liquid in the still, but
due to the high concentration of the more volatile component in the vapour, the
compositions of liquid and vapour are not constant.
To determine how the compositions vary with time, consider the case where n0 moles
are charged into a batch distillation unit. Let n be the moles of liquid remaining in the
still at a given time, and x and y be the vapour and liquid compositions respectively.
The total moles of a more volatile component A left in the still, nA, will be
nA xn
49
Differentiating Eq. (1) gives
dnA d ( xn) n dx x dn
If a small amount of liquid, dn, is vaporised, the change in the moles of A is y dn, or
dnA.
From Eq. (2),
y dn n dx x dn
dn dx

n yx
By integrating Eq. (3) between the initial and final concentrations, we obtain
n dn x dx
n0 n

x 0 y x
n x dx
ln
n0 x 0 y x
dx ( y x)
Eq. (4) is known as the Rayleigh Equation. The term can be integrated
graphically or numerically using equilibrium curve.
The Rayleigh equation can also be derived for an ideal mixture based on relative
volatility. Although the temperature in the distillation column increases during a
batch distillation process, the relative volatility, or the ratio of vapour pressures, does
not change drastically. Hence, an average value for relative volatility is used and
assumed to be constant.
yA x
AB A
yB xB
Consider a binary mixture consisting of nA mol of A and nB mol of B. The ratio nA/nB
is equal to xA/xB. When dn mol is vaporised, the change in component A is yAdn or
50
dnA, and the change in component B is yBdn or dnB. Substituting these terms into
equation (4) yields
dn A / dn n
AB A
dnB / dn nB
dnA dn
AB B
nA dnB
Integrating Eq. (6) between the initial and final condition yields
nA n
ln AB ln B
n0 A n0 B
1 / AB
nB n A

n0 B n0 A
Eq. (7) above can be plotted as a straight line on a logarithmic scale. If the recovery
of either component is specified, then Eq. (7) can be used directly to determine the
recovery of the remaining component.
7.2.2 The Batch Distillation apparatus
The batch distillation column is designed to demonstrate the separation of mixture with
different boiling points. This unit comprised of a sieve plate column and a packed column
which is interchangeable. The internal (plate or packings) of the column can be seen clearly
via the borosilicate glass section in the middle.
The overhead condenser at the top of the column is used to condense the product vapour
which is then collected at the reflux drum. The amount of top product to return back to the
column or directed to the top product tank can be controlled by adjusting the reflux ratio.
The range of reflux ratio can be adjusted from 0% to 100% via electronic control valves at
the control panel. The reboiler at the base of the column is used to evaporate feed. A jet
vacuum pump fitted at the top product line allows vacuum distillation.
51
Overhead Condenser
Reflux Drum
Vacuum Pump
Distillation Column with Pressure
Gauge
Flow Meter
Top Product
Main Power
Tank
Switch
Reboiler
Figure 7.2: Batch Distillation Column
Always wear safety glasses, mask and gloves when handling chemicals. Do not allow
the solution to come into contact with your skin or eyes.
Should any chemicals come into contact with the body, rinse off immediately with
plenty of water and inform the laboratory instructor/officer. Seek medical treatment if
symptoms persist.
Ensure that there is no source of ignition, such as a Bunsen burner, gas flame, hot
plate, hot air gun or hot water pipe near the working area.
Propanol releases irritating vapours; avoid inhalation and work in a well-ventilated
area.
Good ventilation is essential so that it is not possible for high concentrations of
alcohol vapour to form.
Dispose of all unused chemicals in an appropriate manner after the experiment.
Under no circumstances should the chemicals be allowed to flow into sinks or drains.
Pour slowly and be very careful when pouring the mixture into the reboiler. The inlet
nozzle is quite small so if the solution is poured too fast, the nozzle will choke and the
solution will spill out.
52
7.4 Chemical Hazards
Ethanol is very flammable, so constitutes a fire risk. Ethanol contact with the eyes
can cause considerable irritation.
Ethanol is very flammable. It evaporates readily, so it is possible for dangerous levels
of vapour to build up, perhaps reaching a point at which an explosion is possible if a
source of ignition is present.
If ethanol is in contact with oxygen over a long period, explosive peroxides may be
formed. These typically have a higher boiling point than ethanol, so may become
concentrated in the liquid if ethanol is distilled. Therefore, bottles of ethanol, once
opened, should not be stored indefinitely, in order to avoid any risk of peroxide
formation.
Ethanol is very flammable. It can be ignited by flames, but also by contact with items
such as hot plates or hot air guns.
Read and understand the theory of distillation.

Read and understand the equipment used in the experiment (batch distillation
column).
Read the safety precautions and chemical hazards before conducting the
experiment.
Read the Material Safety Data Sheet (MSDS) for the chemicals used in the
experiment ethanol
Prepare the following apparatus and materials needed for the experiment:
Refractometer
Beakers
Syringe / Dripper
0%, 10%, 20%, ..., 100% of ethanol-water mixture
Prepare 10 L of 25 v/v% ethanol-water mixture
General Start-Up Procedures
1. Ensure that all valves on the unit are closed.
53
2. Attach the inlet hose from the condenser unit to a water supply and the outlet hose to
a drain.
3. Connect the 3-pin plug to 240VAC main power supply. Turn on the power supply
and main power switch at the front of the control panel.
4. Open valves V5 and V6.
5. Open the cooling water supply and set the flow rate to maximum. Allow it to run for
at least 10 minutes.
6. Close valves V5 and V6. Open valve V4 to allow cold water to circulate inside the
condenser. (Note: Do not open valves V5 and V6 for the vacuum pump during the
experiment)
1. After the experiment, drain off the contents in the reflux drum and top product tank.
2. Dispose all chemicals into the container provided.
3. Switch off the main power switch at the control panel and power supply.
4. Turn off the cooling water supply.
7.6 Experimental
Experiment 1A: Batch Distillation with Constant Reflux
1. Start-up the unit according to procedures in Section .
2. Fill 10 L of 25 v/v% ethanol-water mixture into the reboiler slowly. The inlet nozzle is
quite small so if the solution is poured too fast, the nozzle will choke and the solution
will spill out. (Caution: The person who pours the mixture should wear a face shield.)
3. Collect a sample from the feed and measure its refractive index (see Experiment 2).
Note: Do not open the valves V5 and V6 for the vacuum pump during the
experiment. Operation of the vacuum pump after the mixture is partially vaporised
will cause the fluids to gush upwards and damage the column.
4. Set the temperature of the reboiler, T13 to 85C using the temperature controller on the
control panel.
5. Set the reflux ratio to 100%.
6. Once the top product appears in the reflux drum, run the column at total reflux for
another 10 minutes.
7. Record down all the temperatures, T1 to T13, by turning the temperature selector knob
on the control panel.
54
8. Set the reflux ratio to 80%.
9. At intervals of 10 minutes, record all temperatures and collect a sample from both the top
product tank and reboiler. Measure the refractive index of each sample. (Note: the feed
sample has to be cooled down to room temperature for accurate result)
10. Repeat Step 9 until 4 sets of samples are collected. The system should stabilise after 40
minutes.
11. Empty the top product tank at the end of the 4th set of sample and measure its volume.
12. Tabulate all the data obtained and determine the composition of the feed and product
using the calibrated data from Experiment 2.
13. Shutdown the unit according to procedures in Section .
Experiment 1B: Batch Distillation with Regulating Reflux
By using the same setup and chemicals as Experiment 1, design and run an experiment to
determine the product composition with regulating reflux ratio.
Experiment 2: Calibration of Refractometer
1. Prepare 10 samples of ethanol-water mixture for 0%, 10%, 20%, ..., 100% concentration.
2. Open the secondary prism of the refractometer and drip 2 or 3 drops of 0% mixture onto
the centre part of the main prism surface. Gently close the secondary prism. The sample
will spreads between the main prism and secondary prim as a thin film.
3. While observing through the eyepiece, gently turn the measurement knob until the
boundary line appears in the field of refraction view. At that time, the boundary line may
be coloured and unclear because it is not yet achromatised.
4. Turn the measurement knob in a wide range so as to set it at a point where the field of
refraction view clearly changes from bright field to dark field or vice versa. The
brightness of the field can be adjusted with the illumination selector switch in the upper
part of the digital thermometer.
5. Turn the colour compensator knob to achromatise the boundary line so that the line
appears clearly in the field. Turn the measurement knob again to set the boundary line at
the intersection of the cross hairs.
6. The upper scale is for reading refractive index (nD) while the lower scale is for Brix
percent. Record down the refractive index of the sample.
7. Repeat Step 2 to Step 6 for all the 10 samples mixture.
55
CAUTION!
Measured value for liquid sample changes depending on the change of temperature.
Therefore, samples' temperature must be kept constant.
Do not wet the refractometer with sample liquid unreasonably. If the refractometer gets
wet excessively, it may cause malfunction and breakdown of the refractometer.
Do not tap or pick at the prism surface with a metal spoon, tweezers, etc. because the
prism surface is made of optical glass. If the prism surface is scratched, the refractometer
may fail in measurement.
When measurement is complete, wipe up sample from the prism surface and its
surroundings with soft tissues moistened with water first, and then wipe the wet parts
with dry tissues to dry them up.
After measurement of a sample of a high molecular compound (e.g. oil, fat etc) wipe the
prism surface with tissues moistened with alcohol or neutral detergent first and then wipe
it up again with dry tissues to dry up.
On ending a day's measurement, turn off the power switch.
1. Plot the calibration curve and use it to determine the composition of a mixture.
2. Discuss the variation of top product against time at constant reflux ratio.
3. Discuss the effects of constant reflux ratio and regulating reflux ratio on product
composition.
4. Plot the temperature profile of the distillation column and discuss its relationship with
reflux ratio and composition mixture.
56
8.0 Liquid-liquid Extraction
8.1 Aims
To understand the principles of liquid-liquid extraction.
To determine the amount of solute extracted from feed.
To determine the efficiency of extraction.
To investigate the effects of feed and solvent flow rates on extraction.
8.2 Introduction
When separation by distillation is ineffective or very difficult, liquid extraction is one of the
main alternative to consider. Close-boiling mixtures or substances that cannot withstand the
temperature of distillation, even under a vacuum, may also be separated by extraction.
Extraction utilises chemical differences instead of vapour pressure differences for separation.
Liquid-liquid extraction, also known as solvent extraction, is a method to withdraw solute in

a liquid mixture using a liquid solvent, in which the solvent is immiscible or nearly
immiscible with the liquid. The simplest liquid-liquid extraction involves only a ternary
system. The feed consists of two miscible components, the carrier, C and the solute, A.
Solvent, S is a pure component. C and S are immiscible or only partly miscible. A is soluble
in C and completely or partially soluble in S. During extraction, solute A is transferred from
the feed to solvent S, with less transfer of carrier C to S, or S to feed.
Extract
Feed Solution
Extraction
Column
Solvent
Raffinate
57
Figure 8.1: A Typical Liquid-Liquid Extraction Column
A general extraction column consists of two inlets and two outlets, as shown in Figure 8.1.
Usually, the inlets consist of a feed stream from the top of column, which contains the solute
to be extracted, and a solvent feed from the bottom which extracts the solute from the feed.
After mixing the feed and the solvent, the two phases are separated either by gravity or
centrifugal forces. The solvent that contains the extracted solute leaves the top of the column
and is referred to as the extract stream. The solution that exits from the bottom of the column
which contains only a small amount of solute is referred as raffinate.
In liquid-liquid extraction, as in gas absorption and distillation, two phases must be brought
into good contact to permit transfer of material between the phases. In extraction the two
phases have comparable densities, so the energy available for mixing and separation is small.
The viscosities of both phases are also relatively high and linear velocities through most
extraction equipment are low. Therefore, in some cases, mechanical mixing and separation
are necessary.
8.1.1 Extraction Equipment

Generally, industrial extraction equipment can be divided into 4 types: mixer-settler, columns
with agitator, columns without agitator and centrifugal extractors. The table below shows the
advantages and disadvantages of these extractors.
Types Advantages Disadvantages
Mixer-Settler high efficiency high set-up cost

low head room large scale
induces good contacting high operation cost
can handle any number of stages
Column low investment costs high head room
without low operating costs difficult to scale up from lab
Agitator less efficient than mixer-settler
Column with good dispersion difficult to separate small

Agitator low investment costs density differences
does not tolerate high flow ratios
Centrifugal can separate small density high set-up, operating and
Extractors differences maintenance costs
short holding time cannot handle many stages
small liquid inventory
58
8.1.2 Theory Material Balance on Solute

To obtain the simplest result, it is preferable to express compositions of the solute as
mass/mole ratios instead of mass/mole fraction.
Let FA = feed rate of carrier A

S = flow rate of solvent C
mass/moles of solute B
XB
mass/moles of other component in the feed (F), extract (E) or raffinate (R)
Material balance for Solute B,
B in F B in E B in R
X B( F ) FA X B( E ) S X B( R ) FA
The distribution of solute at equilibrium,
X B( E ) K D B X B( R )
where KDB is the distribution coefficient defined in terms of mass or mole ratios.
Substitute Eq. (2) into (1),
X B( F ) FA
X B( R )
FA K D B S
Extraction factor, EB, for solute B,
59
S
E B K D B
FA
The larger is the value of EB, the greater extent to which the solute is extracted. Large values
of EB result from large values of KDB or large ratios of solvent to carrier, S/FA. Fraction of B
that is not extracted,
X B( R ) 1

XB (F )
1 EB
This clearly shows that the larger the value of EB, the smaller the fraction of B that is not
extracted.
X (mass/mole ratios) are related to x (mass/mole fractions) by
xi
Xi
(1 x i )
KD, in terms of ratio, is related to KD, in terms of fractions by
xi(1) (1 x i(1) ) 1 xi( 2 )

K D i K Di

xi( 2 ) (1 x i( 2 ) )
1 xi
(1)

xi(1)
K Di
xi( 2)
where . When xi are small, KD approaches KD.
The efficiency of the extraction process is given by
60
amount of solute B in extract

Separation Efficiency
amount of solute B in feed
8.2 Liquid-liquid extraction unit

The liquid-liquid extraction unit is designed to demonstrate liquid mixture separation by
solvent extraction. This unit comprised of a glass extraction column, a distillation column for
recovery of solvent (both are packed with Raschig rings), tanks, pumps, water jet vacuum and
all the necessary instrumentation.
The liquid mixture to be separated is delivered from the feed tank to the bottom of the
extraction column via a gear pump. The solvent is then delivered via a diaphragm pump to
the top of the extraction unit to contact with the feed in counter-current flow. The feed
mixture to be separated comprises of a transition component (solute) and a carrier liquid. A
phase boundary is established in the column because the carrier liquid and solvent are
insoluble in one another. The transition component transfers from the carrier liquid into the
solvent in the unit. The system is fitted with two three-way valves to enable the unit to
operate as a closed or open process.
Separation of the transition component and the solvent is done by the distillation unit. The
distillation unit is made up of a glass packed column with a bottom boiler and an overhead
condenser. The mixture of the transition component and the solvent is heated up to the
desired evaporation temperature by using the boiler with a digital temperature controller.
A thermocouple with digital display is provided for measurement of the column top
temperature. Distillation removes the solvent from the transition component, where both are
individually collected as top and bottom products. The recovered solvent is then reused for
the next extraction process. A pH and conductivity meter is provided to monitor the
separation process efficiency.
61
Extraction Column Extract

with Raschig Ring Tank
Packing
SolventDistillate
Pump Tank
Feed Pump
Control
Panel
Distillation Unit
with Boiler Feed Tank
Gate Valve
Solvent Tank
Raffinate Tank
Figure 8.2: Liquid-Liquid Extraction Column with Solvent Recovery
8.3 Operating Procedures
8.3.1 Pre-experiment Procedures

1. Read and understand the theory of liquid-liquid extraction.
2. Read and understand the equipment used in the experiment (liquid-liquid extraction
unit).
3. Read the safety precautions and chemical hazards before conducting the experiment.
4. Read the Material Safety Data Sheet (MSDS) for the chemicals used in the experiment in
Appendix A acetic acid, ethyl-acetate
pH meter
Burette
Erlenmeyer flasks
Beakers
1.0 M NaOH solution
Phenolpthalein
62
Prepare 20 L of 20 v/v% acetic acid solution
8.4 Chemical Hazards, Safety and Precautions
8.4.1 Chemical Hazards (refer MSDS in Appendix A for more

details)
Acetic acid contact with the eyes can cause serious long-term damage. The pure material
and its solutions are corrosive; concentrated solutions can cause serious burns.
Ethyl acetate is very flammable, so constitutes a fire risk. It can be ignited by flames, but
also by contact with items such as hot plates or hot air guns.
8.4.2 Safety Precautions

Always wear safety glasses, mask and gloves when handling chemicals. Do not allow the
solution to come into contact with your skin or eyes.
Should any chemicals come into contact with the body, rinse off immediately with plenty
of water and inform the laboratory instructor/officer. Seek medical treatment if
symptoms persist.
Ensure that there is no source of ignition, such as a Bunsen burner, gas flame, hot plate,
hot air gun or hot water pipe near the working area.
Ensure the heating coil is fully immersed in liquid before switching on the heater.
Do not touch the boiler and distillation column when conducting the experiment.
Be careful when using the handheld pH and conductivity meter.
Do not attempt to change the setting of the pumps.
Dispose of all unused chemicals in an appropriate manner after the experiment. Under no
circumstances should the chemicals be allowed to flow into sinks or drains.
8.5 Experiments
8.5.1 Experiment 1: Determination of Efficiency of Extraction

1. Connect the 3-pin plug to 240VAC main power supply. Turn on the power supply and
main power switch at the front of the control panel.
2. Make sure all the valves are closed.
3. Fill 20 L of 20 v/v% acetic acid solution into the feed tank.
4. Fill 10 L of ethyl-acetate into the solvent tank.
5. Switch on the solvent pump and set the flow rate to 15 L/hr to feed the solvent into the
bottom of the column. (Note: press the up/down soft button to adjust the flow rate, do
not turn the turning knob)
63
6. Once the solvent level reaches about a third of the height of the column, switch on the
feed pump and set the flow rate to 15 L/hr.
7. As the liquid level reaches the top of column reduce the feed and solvent flow rates to 10
L/hr.
8. Open the Gate Valve at the bottom of the extraction column to direct the bottom product
to the raffinate tank
9. Keep an eye at the liquid level; ensure that the liquid level is maintained near the top of
the column by adjusting the feed and solvent flow rates.
10. The boundary between the two immiscible liquids (the feed and solvent) is maintained
around the middle of the column by adjusting the Gate Valve.
11. After 10 minutes, obtained sample from extract tank and raffinate tank respectively and
determine their pH values.
12. Collect 5 ml of sample, from both the extract and raffinate tank, into a Erlenmeyer flasks
and determine the amount of acetic acid by titration method with 1.0 M NaOH solution:
(a) Take the initial NaOH volume.
(b) Drop a few droplet of phenolphthalein into the sample in Erlenmeyer flask.
(c) Titrate the solution with NaOH until the sample turn to pink colour.
(d) Record the NaOH volume after titration.
13. Repeat Step 11 and Step 12 every 10 minutes until 4 sets of samples are collected.
14. Switch off the main power switch at the control panel and power supply after the
experiment.
8.5.2 Experiment 2: Investigate the Effect of Feed and Solvent

Flow Rates on Extraction
By using the same setup and chemicals as Experiment 1, design and run an experiment to
investigate the effect of feed and solvent flow rates on the efficiency of extraction.

1. Sketch a schematic diagram, including all valves and sensors/controllers, for the
extraction unit used in the experiment. Label all valves and instruments.
2. Calculate the amount of solute (acid acetic) in the feed, extract and raffinate.
3. Calculate the efficiency of extraction
64
4. Discuss the effects of feed and solvent flow rates on the efficiency of extraction based on
your experiment. Compared the results with theory.
9.0 Reverse Osmosis
9.1 Aims
To investigate the clean membrane resistance Rm and membrane resistance due to
concentration polarization Rcp.
To study the efficiency of membrane in removing NaCl from NaCl-water solution.
9.2 Introduction
Nowadays, membrane separations are becoming increasingly popular as it provides effective
separation without the use of chemicals and heating energy as in distillation processes.
Figure 2.1 depicts the principle of membrane separation in which the permeate stream passes
through the membrane barrier whereas the retentate stream is rejected by the membrane
barrier. The efficiency of the membrane process in removing the components is based on
differences in physical and/or chemical interactions between the components to be separated
as well as the membrane material.
There are four well-developed pressure-driven membrane water separation processes

available in the membrane industry. These processes are generally classified as
microfiltration (MF) and ultrafiltration (UF), with the latter mostly subdivided into
nanofiltration (NF) and reverse osmosis (RO).
Despite similarity in processes, each of them has its specific characteristics. When membrane
filtration is used for the removal of larger particles, MF and UF are preferentially to be
applied. These membranes offer high water flux at a very low operating pressure due to their
open character. To separate low molecular weight solute and/or charged solute from water,
NF and RO are considered.
65
Figure 9.1: Membrane Process
9.2.1 Theory
Numerous theoretical models have been employed in pressure-driven membrane processes to
investigate their performances when dealing with different properties of feed solution.
Membrane water flux and solute separation efficiency are the most important parameters that
should take into account in membrane selection process. The membrane pure water flux,
JPWF can be expressed in the following equation,
1 dV P
J PW F
Am dt ( Rm )
where Am = membrane effective area, m2

P = gradient of hydrostatic pressures across the membrane, bar
= dynamic solvent (water) viscosity, Pas
Rm = clean membrane resistance, m-1
The membrane resistance can then be determined from the graph of the flux, JPWF versus P.
In terms of permeability, the equation can be expressed as JPWF = LpP where Lp is the
hydraulic permeability coefficient.
Due to the presence of solute in the feed solution, it is found that the water flux of membrane
tends to decrease gradually. This phenomenon can be attributed to the concentration
polarization resulting from the solute concentration build up at membrane interface Cw as
shown in Figure 2.2. The solute buildup would form a boundary layer on membrane surface,
leading to a decrease in membrane water flux. The membrane permeate flux JPF varies with
the feed solute concentration can be expressed as follows,
P
J PF
( Rm Rcp )
where Rcp = membrane resistance due to concentration polarization, m-1
66
Figure 9.2: Concentration Polarization at Membrane Interface
Figure 2.3 shows the effect of solute concentration on membrane water flux. As can be seen,
increasing solute concentration would decrease significantly membrane water flux and in
principles causing a zero flux of membrane when a gel formation concentration, Cg is
reached. The process usually occurs when the wall concentration due to concentration
polarization exceeds the solubility of the organic.
Figure 9.3: The Effect of Solute Concentration on Membrane Water Flux
The effect of concentration polarization introduces complexity into the core membrane
performance parameter retention. It should be distinguished between the terms observed
retention (ROBS) and real retention (RO). The observed retention is usually measured in
membrane applications and calculated as
67
Cp
ROBS (%) 1 100
Cb
where Cp and Cb represent permeate concentration (ppm) and bulk concentration (ppm),
respectively.
Considering concentration polarization, the membrane retention is relatively higher due to the
increased wall concentration Cw at membrane surface. The real retention therefore can be
determined as
Cp
RO (%) 1 100
Cw
Since solute concentration at membrane surface cannot be measured directly from the
membrane process, hence one requires the velocity dependent mass transfer coefficient. The
relationship between real and observed retention is defined in the following equation.
1 ROBS 1 RO J
ln ln
ROBS RO kw
where kw is the solvent mass transfer coefficient that depends on the Reynolds number.
9.3 Reverse Osmosis and Ultrafiltration Unit
9.3.1 Membrane and Membrane Housing

Figure 3.1 shows the schematic diagram of Micro 240 module used in this experiment. The
module is designed to be fitted to a wide range of tubular membranes and is fully compatible
with UF, NF and RO tubular membranes. As can be seen in the figure, the module consists of
two perforated stainless steel (SS) tubes which are designed for feed inlet and concentrate
outlet, respectively. Permeate outlet on the other hand allows the purified feed solution to be
collected.
68
Figure 9.4: Schematic diagram of Mirco 240 module
Membrane information:
Membrane type : AFC 99
Material : Polyamide
Membrane effective area : 0.024 m2
Maximum pH range : 1.5 12
Maximum pressure : 65 bar
Apparent retention character : 99% NaCl
9.3.2 Pumps
The triple plunger pump (P1) is used to pump the liquid from the feed tank into the
membrane module. A pressure regulator is installed to regulate the operating pressure of the
feed system.
9.3.3 Tanks
The unit is supplied with a feed tank and a product tank, both having a maximum capacity of
30 litres. The feed and product tanks are made of stainless steel for corrosion and chemical
resistance. The feed tank has a cooling system to remove the heat generated from the pump.
9.3.4 Instrumentations
The unit is supplied with the necessary instruments to measure flow rate, pressure and
temperature:
Flow meter (FT1) Range: 0 20 LPM
69
Pressure transmitter (PT1) Range: 0 100 barg

Temperature transmitter (TT1, TT2) Range: 0 100 C
Pressure gauge (PI1) Range: 0 70 bar
9.4.1 Pre-experiment Procedures

3. Read and understand the theory of membrane separation.
4. Read and understand the equipment used in the experiment (RO unit).
5. Prepare the following materials needed for the experiment:
Prepare 25 L of NaCl aqueous solution with a concentration of 10,000 ppm.
9.4.2 General Operating Procedures
Control Valves
In order to prevent damage to any parts of the unit, it is very important to fully understand the
flow of the system prior to operating. The correct flow of fluid is achieved by setting the
appropriate valves in the correct direction. The unit has been installed with ball valves and
needle valve as follows:
Description Type
Feed tank drainage valve 2-way
Feed tank outlet flow into the plunger pump 2-way
Plunger pump drainage valve 2-way
Controls of the retentate flow rate and to vary P Needle
Permeate sampling valve 2-way
Product tank outlet flow into the plunger pump 2-way
Product tank drainage valve 2-way
Retentate sampling valve 2-way
Cool water supply valve 2-way
70
Setting the Maximum Working Pressure
1. In order to set the maximum working pressure, close valve V04.

2. Use a wrench to adjust the pressure regulator to a safe low pressure setting by turning the
pressure adjuster nut counter-clockwise.
3. Open valve V02 and close valve V01.
4. Ensure that the feed tank is not empty and then switch on the plunger pump (P1).
5. Observe the pressure (PT1) reading next to the pressure regulator. The pressure will rise
steadily until it reaches the previously set pressure.
6. Using a wrench, adjust the pressure regulator to obtain the desired maximum working
pressure (clockwise to increase pressure; counter-clockwise to decrease pressure).
Note: If the pressure fails to increase or keep-on dropping, there must be air trapped in the
membrane system. Shut off the pump and let the air to escape. Ensure that no air is being
introduced into the system.
Draining the Leftover
Before flushing the membrane, the leftover liquid has to be completely drained after each
session in order to prevent bacterial formation overnight. There are six drainage points
provided with the unit. For a complete drainage of the system, open all valves.
Pumps Limits
The plunger pump has a working pressure range of 7 to 85 bar. However, to protect the
membranes, do not regulate the pressure more than 35 bar.
Membrane Limits
The recommended operating pressures of the RO membrane modules are 35 bar. The
operating temperature shall not exceed 80C for RO membranes.
Operation of membranes at maximum limits of pressure or temperature will affect their
subsequent performance at lower temperatures and pressures. In addition, it is not
advisable to operate at the limits of temperature and pressure at the same time.
Test conditions determine the precise retention character.
The maximum pH range for RO membranes is 1.5 12.
71
Control Valves
All valves must be set at the correct positions in order to avoid possible damage to the unit.
Cleaning Procedures
After each experiment, drain all process liquid from the process lines, product tank and
feed tank.
Rinse and fill up the feed tank with deionised water.
Make sure that all valves are set as follows:
Open Close Leave Alone
V2, V4 V1, V3, V5, V6, V7, V8 V9
Set the pressure at 2 5 bar and start the plunger pump. Fully open the needle valve
(V04) and let the water flow for about 10 minutes.
Repeat the above if necessary. Stop the pump and switch off the power supply after all
were completed.
9.6 Experiments
9.6.1 Experiment 1: Determination of Clean Membrane Resistance,

Rm
Feed: Clean Water
1. Ensure that the RO membranes (AFC99) are in installed in the membrane module and
the rubber seals on both ends do not fold. Tighten the screw if necessary and ensure
there are no leakages.
2. Follow procedures in Section 4.2.2 to set the operating pressure in this experiment to 25
bar. (Note: for RO filtration never operates the membrane more than 35 bar or more
than 80C)
3. After the desired pressure is achieved, stop the plunger pump (P1).
4. Fully open valve V02 and V04 and start the plunger pump (P1) again.
72
5. Connect the cooling coil inlet to cooling water supply and outlet to drain. Open valve
V09 to allow water to flow through the cooling coil. (Note: cooling water is used to
remove the heat generated from the plunger pump)
6. Set the differential pressure across the membrane to 2 bar by adjusting the needle valve
V04. Let the water flow for about 5 minute until the flow rate is stable before taking any
reading.
7. Open the sampling valve V08 and drain off the water leftovers from the last experiment.
8. Measures the permeate flux every 5 min (up to 15 min) and record the average value
from the three replications.
9. Repeat Step 6 and 7 with different pressure (5, 10, 15 and 20 bar).
9.6.2 Experiment 2: Determination Of Membrane Resistance Due

to Concentration Polarization, Rcp and Observed Salt Rejection
from Water, ROBS
(Experiment 2 is run using the same setup Experiment 1)
Feed: NaCl-water solution
1. Set the position of the valves as follows:
Open Close Leave Alone
V2, V4 V1, V3, V5, V6, V7, V8 V9
2. Fill up the feed tank with NaCl solution prepared. Record the initial conductivity of tank
solution.
3. Open valve V09 to allow water to flow through the cooling coil. Wait for the
temperature to stabilise before taking any readings.
4. Start the plunger pump (P1).
5. Set the inlet pressure to 25 bar by adjusting the needle valve V04. Let the solution flow
for about 1 minute until the flow rate is stable before taking any reading.
6. While the plunger pump is running, open the bleed screws slowly on both HI and LO
side of the differential pressure transmitter to bleed the air trapped inside the system.
(Note: the differential pressure reading will be unstable if this step is skipped).
7. Measures the permeate flux every 5 min (up to 15 min) and record the average value
from the three replications.
8. Observe and record the conductivity of permeates solution at the end of experiment.
73
9. Stop the plunger pump and close valve V02. Recycle all the filtrate and retentate back
into the feed tank.
10. Repeat the experiment (Step 5 to 9) for inlet pressure of 5, 10, 15 and 20 bar.

1. Sketch a schematic diagram, including all valves and sensors/controllers, for the reverse
osmosis unit used in the experiment. Label all valves and instruments.
2. Plot the graph of JPWF versus P and calculate the clean membrane resistance, Rm from
the slope of the graph.
3. Determine the membrane resistance due to concentration polarisation Rcp in the filtration
process in the presence of NaCl in feed solution. Discuss the effect of Rcp on membrane
permeate flux and recommend the ways that can diminish the effect of concentration
polarisations.
4. Determine the ROBS (%) of NaCl at different operating pressure from Experiment 2.
Explain the results obtained and further propose a method to evaluate value of RO (%)
based on ROBS (%) obtained. (Hint: to determine the rejection, the conductivity must be
first converted into concentration according to the calibration curve figure as shown
below).
Figure 9.5 Calibration Curve of NaCl Concentration and Conductivity
74
10.1 Filtration

Science
Experiment No.: 10
Title of Experiment: Filtration

Quantity estimation
student)
Filter press unit E 1
Satin cloth C As per filter press
Nylon cloth C As per filter press
Calcium carbonate CH 500 g
Water C 50 liter
Turbidity meter E 1
*Item category
C Consumable
C Chemical
H
components
E Equipment
S Software
75
10.1 Aims
To understand the working principles of plate and frame filter press.
To determine the water flux of filter medium and pollution index (NTU).
10.2 Introduction
Generally, the plate and frame filter presses are utilised as dewatering machines to remove
liquid from liquid-solid slurry at an operating pressure between 60 80 psi (< 5.5 bar). They
are particularly suited for low solids (< 2% solids), or solids composed of fines (~ 200 mesh),
however they will essentially dewater many combinations of particle size distribution and
percent solid slurries.
In this separation process, liquid-solid slurry is first fed into the filter press and pressurised to
travel across the filter membranes or medium. The void between the plates is filled with the
slurry as the liquid passes through the filter medium. The solids are retained from passing
through the filter medium whereas liquid (filtrate) is allowed to permeate freely. The solids
will remain in the void between the plates, until the plates discharge the filtered solids
The advantages of plate and frame filter press include:

Easy to clean and replace the filter cloth or membranes.
Low maintenance cost.
Capable in operating with high pressure drop conditions and difficult slurries or
materials.
Provides large area for filtration on a small floor space.
Ease of internal inspection as leakage is easily detected.
The disadvantages of plate and frame filter press include:

Usually has to operate in batch.
Requires higher labour costs, especially when manual discharge of filter cake is involved.
At larger feed concentration, inlet ports of the filter have a tendency to encounter
blockage and leakage.
76
10.2.1 Theory
The water flux of a filter medium can be determined by the expression as follows:
Q
J
At
(10.1)
where J = water flux, L/m2h

Q = quantity of permeate, L
A = filter area, m2
t = time to obtain the quantity of Q, h
Turbidity is the cloudiness or haziness of a fluid caused by individual particles (suspended

solids) that are generally invisible to the naked eye. The measurement of turbidity is a key
test of water quality. Nephelometric turbidity units (NTU) is used as a measurement unit for
turbidity and 1 NTU is defined as a water containing 1 milligram of finely divided silica per
litre.
10.3 Plate and Frame Filter Press
Figure 10.1: Schematic Diagram of Plate and Frame Filter Press
The plate and frame filter press operates to remove liquids from a slurry feed. Figure 10.1
illustrates the typical working principles of a press and frame filter press. Slurry liquid enters
77
the filter frame after travelling through the feed channel. Feed pump is required in this
filtration process to pressurize feed slurry going to filter frame from feed storage. The solids
are deposited on the filter medium, leaving the filtrate liquid to be discharged from filtrate
port. The filter medium may be washed down periodically, by using a water hose and
washing the medium over the plates while the filter is open, removing any material that may
tend to blind the filter medium.
Legend
A = Water Tank D = Hand Wheel G = Filter Frame J = Seal Gasket

B = Control Panel E = Water Pump H = Movable End Plate K = Filter Plate
C = Stainless Steel Tray F = Filter Plate & Frame I = Filter Medium
Figure 10.2: Plate and Frame Filter Press
78
1. Read and understand the theory of filtration.

2. Read and understand the equipment used in the experiment (plate and frame filter press).
3. Read the safety precautions before conducting the experiment.
Liquid-solid slurry solution
Two different types of fabric as filter medium with a diameter of 190 mm.

Do not switch on the power supply until all the preparation steps are done.
Do not switch on the water pump (power supply) if there is no water/liquid in the water
tank.
Do not mix the slurry/liquid with solid metal pieces as this may damage the impeller of
the water pump.
The arrangement of the filter plate and filter frame must be installed alternately.
Ensure the filter plates and filter frames are properly tighten before conducting the
experiment.
Ensure the inlet port hand valve is closed and the outlet port hand valve is opened before
the experiment.
Stop the experiment if there is water leakage.
No body part should be inserted in between of the filter plate and filter frame when
turning the hand wheel.
10.6 Experiments
10.6.1 Experiment 1A: Determine the Pure Water Flux of Filter

Medium (cloth medium)
1. Release the filter plates and filter frames by turning the hand wheel (D) of the screw
stem.
2. Remove the filter plates (F) and filter frames (G) from the horizontal guided beam.
3. Clean all the filter plates and frames using clean water.
4. Place the filter medium (I) onto the filter frame.
5. Place the filter plates and frames back to the horizontal guided beam. Ensure the filter
plates and filter frames are installed alternatively between the movable heavy end plate
(H) and stationary end plate by following the number engraved on the plates and frames.
79
6. Compress the filter plates and frames by tighten the hand wheel (D). The filter plates
and frames must be fully tightened in order to eliminate water leakage between the plates
and frames.
7. Connect a water hose to the drain (located at the bottom of the stainless steel tray (K)) of
the filter press.
8. Connect a hose to the water tank from the filtrate outlet of the filter press.
9. Fill up the water tank with clean water.
10. Turn on the main switch at the control panel (B).
11. Start the water pump by pressing the green button. Ensure that the MCB/ELCB at the
control panel is switched on.
12. Open the exhaust valve slightly to discharge the air. (Warning: Do not fully open the
exhaust valve as water may split out from the valve).
13. Adjust the operating pressure to 0.1 MPa (1 bar) and ensure that the value constant
throughout the experiment.
14. Allow the liquid to circulate for 10 min.
15. Record the time required to collect 300 ml filtrate every 5 min (last for 30 min) and
average the values obtained.
16. Determine the pure water flux (L/m2h) of the filter medium.
17. Close the feed valve and then stop the pump.
18. Discharge all the liquid in the filtration system.
10.6.2 Experiment 1B: Determine the Water Flux and

Separation Efficiency of Different Filter Medium
1. By using the same setup as Experiment 1A, repeat the experiment with liquid-solid
slurry to determine the water flux (L/m2h) of the filter medium.
2. Measure and record the pollution index (NTU) of the liquid-solid slurry in the water tank
and the filtrate using turbidity meter.
3. Remove all the filter mediums from the filter frames and observe the appearance of the
filter mediums after the experiment.
4. Repeat the experiment using different type of filter medium.
80
81

1. Discuss the difference between the values of water flux of filter medium obtained from
the experiments.
2. Compare and discuss the water flux of two different filter mediums used in the slurry
separation process.
3. Discuss the separation efficiency of filter medium based on the NTU values obtained.
4. Name other filter medium that can be used for this filtration process. What are the
advantages of using this filter medium?
82
Appendix A: Material Safety Data Sheet (MSDS)

Ethanoic Acid (Acetic Acid)
Common Synonyms Acetic acid, glacial acetic acid, vinegar (when very dilute)
Formula CH3COOH
Physical Properties
Form : white semi-transparent solid, or colourless liquid when
pure. Often used as a colourless solution in water.
Stability : stable
Melting point : 16.7C
Boiling Point : 118.1C
Water solubility : miscible in all proportions
Specific gravity : 1.05
Flash point : 40C
Principal Hazards Contact with the eyes can cause serious long-term damage.
The pure material and its solutions are corrosive; concentrated

solutions can cause serious burns.
Safe Handling Always wear safety glasses. Do not allow the solution to come into contact
with your skin.
Emergency Eye contact : Immediately flush the eye with plenty of

water. Continue for at least ten minutes and call for
immediate medical help.
Skin contact : Wash off with plenty of water. Remove
83
any contaminated clothing. If the skin reddens or

appears damaged, call for medical aid.
If swallowed : Drink plenty of water. Call for immediate

medical help.
Disposal Small amounts of dilute ethanoic acid can be flushed down a sink with a
large quantity of water, unless local rules prohibit this. Larger amounts
should be neutralised before disposal.
Protective Equipment Always wear safety glasses when handling concentrated or moderately
concentrated acid solutions. If you need gloves, butyl rubber or neoprene
are suitable.
Source: http://cartwright.chem.ox.ac.uk/hsci/chemicals/ethanoic_acid.html, August 9, 2004
84
Ethyl Acetate
Common Synonyms Ethyl ethanoate, acetic acid ethyl ester, ethanoic acid ethyl ester
Formula CH3COOC2H5
Physical Properties
Form : colourless liquid with a sweet, fruity smell
Stability : stable, but highly flammable
Melting point : -84C
Boiling point : 77C
Water solubility : soluble
Flash point : -4C
Principal Hazards Ethyl acetate is very flammable.
Safe Handling Wear safety glasses. Make sure that there is no source of ignition near
where you work. The vapour may be ignited by contact with a hot plate or
hot water pipe - no naked flame is needed.

water. If irritation persists call for medical help.
Skin contact : Wash off with water.
If swallowed : Flush the mouth out with water if the

person is conscious. If the amount swallowed is
substantial call for medical help.
Disposal Small amounts of ethyl acetate can be flushed down a sink with a large
85
quantity of water, unless local rules prohibit this. This material is very
flammable, so care must be taken to avoid any build-up of vapour in sink
or sewers.
Protective Equipment Safety glasses. If gloves are required, use polyvinyl alcohol (PVA).
Source: http://cartwright.chem.ox.ac.uk/hsci/chemicals/ethyl_acetate.html, January 16, 2004
86
Ethyl Alcohol (Ethanol)
Common Synonyms Ethanol, alcohol, grain alcohol, fermentation alcohol, fermentation ethanol
Formula C2H5OH
Physical Properties Form : colourless fragrant liquid

Boiling point : 78C
Water solubility : miscible in all proportions
Explosion limits : 3.3 - 24.5%
Principal Hazards Contact with the eyes can cause considerable irritation.
"One-off" consumption of small amounts of ethanol is not likely to be

harmful, but consumption of large amounts can be (and has been) fatal.
Chronic (long-term) ingestion of ethanol may lead to damage to a

variety of organs, such as the liver, and may increase the risk of cancer.
Ethanol is very flammable, so constitutes a fire risk.
Safe Handling Wear safety glasses. Ensure that no sources of ignition, such as a gas
flame, hot plate or hot air gun, are present in the working area. Check that
ventilation is good; use a fume cupboard if possible.
Emergency Eye contact : Flush the eye with plenty of water. If

irritation persists call for medical help.
Skin contact : Wash off with water.
If swallowed : If the quantity swallowed is large, call for

medical help
Disposal Small amounts of ethanol can be flushed down a sink with a large quantity
of water, unless local rules prohibit this. Do not forget that this material is
87
very flammable, so precautions must be taken to ensure that flammable

vapour does not build up in the sink or drains.
Protective Equipment Safety glasses
Source: http://cartwright.chem.ox.ac.uk/hsci/chemicals/ethyl_alcohol.html, August 9, 2004
1-propanol
Common Synonyms n-propanol, normal propanol, propan-1-ol, n-propyl alcohol
Formula C3H8O
Physical Properties
Form : colourless liquid
Boiling point : 97C
Water solubility : high
Flash point : 15C
Explosion limits : 2.1% - 12%
Principal Hazards Propanol is very flammable. It evaporates readily, so it is possible for

dangerous levels of vapour to build up, perhaps reaching a point at
which an explosion is possible if a source of ignition is present.
If propanol is in contact with oxygen over a long period, explosive

peroxides may be formed. These typically have a higher boiling point
than propanol, so may become concentrated in the liquid if propanol is
88
distilled. Therefore, bottles of propanol, once opened, should not be

stored indefinitely, in order to avoid any risk of peroxide formation.
Safe Handling Wear safety glasses. Ensure that there is no source of ignition, such as a
Bunsen burner, hot plate or hot air gun, near the working area. Good
ventilation is essential; use of a fume cupboard is desirable.

water. If irritation persists call for medical help.
Skin contact : Wash off with water. Remove any

contaminated clothing. Note that clothing soaked in
propanol will present a significant fire risk, so should be
removed immediately and placed in a safe location
outside the building or in a fume cupboard.
If swallowed : Call for medical help.
Disposal Small amounts of propanol can be flushed down a sink with a large
quantity of water, unless local rules prohibit this. All traces of propanol
should be washed from the sink, or it may evaporate and present a fire
hazard. Larger amounts should be stored for disposal.
Protective Equipment Safety glasses. Gloves are not normally required when handling this
chemical; if desired, neoprene, nitrile or butyl rubber are suitable.
Source: http://cartwright.chem.ox.ac.uk/hsci/chemicals/1-propanol.html, September 30, 2004
2-propanol
Common Synonyms Isopropanol, isopropyl alcohol, rubbing alcohol
Formula CH3CHOHCH3
Physical Properties
Form : colourless liquid with an alcohol smell
89
Boiling point : 82C

Water solubility : high
Flash point : 12C
Principal Hazards 2-propanol is very flammable. It can be ignited by flames, but also by
contact with such items as hot plates or hot air guns.
Safe Handling Wear safety glasses. Make sure that the area in which you work is well
ventilated, so that it is not possible for high concentrations of the vapour to
form. Work well away from possible sources of ignition, such as hot plates
and Bunsen burners.

water. If irritation persists, call for medical help.
Skin contact : Wash off with soap and water. Remove

any contaminated clothing in a safe area. Be especially
careful if a large volume of 2-propanol has been spilled
on clothes, since there is the risk of very serious burns if
the clothing catches fire. If the skin reddens or appears
damaged, call for medical aid.
If swallowed : Call for medical help.
Disposal Small amounts of 2-propanol can be flushed down a sink with a large
quantity of water, unless local rules prohibit this. However, this material
constitutes a fire risk; if large amounts of it are flushed down a sink
dangerous concentrations may build up in the vapour phase in sewers. If
any 2-propanol is poured into a sink, check that it is thoroughly flushed
away. If some remains, a high concentration may build up in the air within
the sink, presenting a fire risk.
Protective Equipment Safety glasses. If you need to use protective gloves, neoprene, nitrile or
butyl rubber are suitable.
Source: http://cartwright.chem.ox.ac.uk/hsci/chemicals/2-propanol.html, June 22, 2005
Appendix B: Psychrometric Chart
90
Source: http://www.sattestpreptips.com/wp-content/plugins/sociable/psychrometric-chart-si-
units-ashrae-743.jpg, March 25, 2013.
91

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Faculty of Engineering and Science (FES)

Department of Chemical Engineering

2.6 Results Analyses and Discussion...................................................................................16

6.0 Gas Absorption............................................................................................................37

9.0 Reverse Osmosis..........................................................................................................61

Upon completion of this course, a student should be able to:

Rules and Regulations

I, ________________________________________ (Student ID: )

Type of Assessment Marks Contribution

Laboratory Performance Marks

Performance marks shall be assessed on individuals during the laboratory sessions

Safety Adhere to laboratory safety, rules and

Laboratory Report Marks

Laboratory reports will be assessed based on the following criteria:

Overall Organisation of report with the correct format (as 2.5

Observations / Valid observations, consistent with event and 2.5

Discussion Discussion shows complete understanding of 3.5

Conclusion Summary of key findings in a clear statement. 1.5

Laboratory Report Format

The laboratory report must follow the following format:

Max number of lines /

UTAR Laboratory Cover Page

1) Title of Experiment 1 2 lines

2) Objectives of Experiment 1 5 lines

4) Materials and Equipment page

5) Results and Calculations Depends on results and

6) Discussion Depends, usually around

Compare and explain the results obtained to the

8) References Depends on references

Laboratory Report Specifications

Language The report should be written in British (UK) English.

Paper White simile A4 size paper (210 297 mm)

Printing Report must be computer typewritten using word processor and

Binding Staple on top left corner

Page Margin Left margin : 4.0 cm

Numbers Avoid starting a sentence with a number or symbol.

not 43,765,589; not 58.159,25).

One spacing between number and unit (e.g. 5 cm, 50 C, 30 %; not

Symbols are not pluralised (e.g. 5 kg; not 5 kgs).

Symbols derived from multiple units by multiplication are joined with a

Symbols formed by division of two units are joined with a solidus ( )

Only one solidus should be used (e.g. kgm-1s-2 or kg/(ms2); not

SI Prefixes Factor Name Symbol Factor Name Symbol

101 deca da 101 deci d

102 hecto h 102 centi c

103 kilo k 103 milli m

106 mega M 106 micro

109 giga G 109 nano n

1012 tera T 1012 pico p

1015 peta P 1015 femto f

1018 exa E 1018 atto a

1021 zetta Z 1021 zepto z

1024 yotta Y 1024 yocto y

Prefix symbols are attached to unit symbols without a space or hyphen

Refer to http://www.bipm.org/en/si/si_brochure/ for more information on writing reports

1.1 Heat Exchangers

Faculty Lee Kong Chian Faculty of Engineering and

Equipment and Materials

To study different types of heat exchanger operation.

where Ao = outside area of the tube, m2

1.3.2 The Heat Exchanger apparatus

Figure 1: Schematic Diagram for Heat Exchanger Training Apparatus

The four heat exchangers supplied with the unit are: