NKB 10402

Chemical Engineering Laboratory 1

Laboratory Manual

1
Contents

INTRODUCTION ........................................................................................................ 3
LABORATORY SAFETY GUIDELINES ..................................................................... 4
SAFETY DECLARATION FORM ............................................................................... 7
REPORT PREPARATION AND MARKING ............................................................... 9
Experiment 1: Ester Saponification .......................................................................... 16
Experiment 2: Synthesis and characterizationof Alkane, Alkene and Alkyne ........... 19
Experiment 3: AAS: Determination of Cooper (Cu) in water by flame atomic
absorption spectroscopic technique ......................................................................... 25
Experiment 4: HPLC: Determination of caffeine in soft drink .................................... 29
Experiment 5: Activation Energy of an Ionic Reaction .............................................. 32
Experiment 6: Refrigeration cycle............................................................................. 35
Experiment 7: Method of Flow Measurement ........................................................... 41
Experiment 8: Drag coefficient ................................................................................. 45

2
 INTRODUCTION

You are required to carry out eight experiments during the first year. Seven out of eight experiments
must be written up and hand in, and will be assessed as described below. You are required to give
an oral presentation for one laboratory report, in which the title will be one of the experiments,
specified by subject leader. You will be working in group of four/five and details of working
arrangements are given on the laboratory sheets together with the timetable. All reports must be
submitted in group (one report only for each experiment).

If you are unable to attend a practical class for a valid reason, please meet subject leader as soon as
possible, preferably before the class is due to take place. It may be possible to rearrange a practical
session, but this cannot be guaranteed. Unexplained absences from laboratory classes may
result a zero mark for that specific experiment. You may not submit a report if you have not
attended the practical class.

There are a number of housekeeping rules which you must abide by in the laboratory:

Coats and bags should be left at the designated area and must not be left on benches or on
the floor between benches.
You must wear a lab coat, safety shoes and safety glasses at all times. Although you
may not be working with hazardous substances, someone near you will be. Under no
circumstances will anyone be allowed to carry out an experiment without labcoat and glasses.
Be careful when moving about the laboratory, someone may be making a delicate
measurement!

The timetable for the year and handouts for each experiment are provided in advance (in this manual)
so that you have the opportunity of finding out about the experiment before you arrive in the
laboratory. Please print out the lab manual and make sure that you read the appropriate part of the
manual before you attend the class, so that you are reasonably familiar with what you are supposed
to be doing. Although demonstrators will be present to assist you in the laboratory, their principal role
is to show you how to use the equipment rather than explain the background to what is going on.

When you arrive in the laboratory, find your place and wait for the demonstrator to show you the
equipment before starting. Be patient! Do not start the experiment without permission!.

After you have finished taking readings, resist the temptation to disappear from the class
straightaway. Before you leave, make sure that you are satisfied with the data analysis that is
required. Demonstrators will help you if there is anything in the handout that is unclear. However,
students are required to understand the theoretical part of the experiments based on the knowledge
learned from lectures.

Laboratory reports must be written up and handed in to lecturer-in-charged within one week after
your laboratory class. Late work is not acceptable.

3
 LABORATORY SAFETY GUIDELINES
General Guidelines

1. Conduct yourself in a responsible manner at all times in the laboratory.

2. Be familiar with your lab assignment before you come to the lab. Follow all written and verbal
instructions carefully. If you do not understand a direction or part of a procedure, ask the
instructor before proceeding.
3. No student may work in laboratory alone. The lab instructor or co-coordinator grant exceptions
on a case by case basis.
4. When first entering a laboratory, do not touch any equipment, chemicals or other materials in the
laboratory area until you are instructed to do so.
5. Do not eat, drink beverages or chew gum in the laboratory. Do not use laboratory glassware as
containers for food or beverages.
6. Smoking is not allowed in any indoor area.
7. No music allowed in the laboratory. Radio (including walkman) and other entertainment devices
are not permitted.
8. No cellular phone is allowed in this laboratory.
9. Perform only those experiments authorized by the instructor. Never do anything in the laboratory
that is not called for the laboratory procedures or by your instructor. Carefully follow all
instructions, both written and oral. Unauthorized experiments are prohibited.
10. Observe good housekeeping practices. Work areas should be kept clean and tidy at all times.
11. Horseplay, practical jokes, and pranks are dangerous and prohibited.
12. Always work in a well-ventilated area.
13. Bring only your laboratory instructions, worksheets and report to the work area. Other materials
(books, purses, backpacks, etc) should be stored in the cabinet.
14. Know the locations and operation procedures of all safety equipment including the first aid kit,
eyewash station, safety shower, spill kit and fire extinguisher.
15. Be alert and proceed with caution at all times in the laboratory. Notify the instructor immediately
of any unsafe condition you observe.
16. Label and equipment instructions must be read carefully before use. Set up and use the
prescribed apparatus as directed in the laboratory instructions provided by your instructor.
17. Experiments must be personally monitored at all times. You will be assigned a laboratory station
at which to work. Do not wander around the room, distract other students or interfere with
laboratory experiments or others.
18. Write your name and equipment use every time you come in to the laboratory in the log book.
19. Defeating safety devices or using equipment in a manner other than that which is intended will be
grounds for dismissal from the lab.

Clothing
1. Safety goggles and safety jacket must be worn whenever you work in lab.
2. Gloves should be worn whenever you use chemicals that cause skin irritations or need to handle
hot equipment.
3. Mask should be worn every time you prepare the chemicals.
4. Safety shoes and hard hat should be worn at all times while in the laboratory.
5. Contact lenses should not be worn in the laboratory unless you have permission from your
instructor.
6. Dress properly during a laboratory activity.
7. Long hair, dangling jewelry and loose or baggy clothing are a hazard in the laboratory. Long hair
must be tied back and dangling jewelry and loose or baggy clothing must be secured.
8. Sandal, open-toed shoes, high heels or shoes with holes in the sols will not be worn in the lab.
9. Short and skirts are not permitted.
10. Instructor and laboratory assistant have a right dismiss to you from the laboratory if they found
that you are not wearing proper safety clothing.

4
 Handling Chemicals
1. Treat chemicals with respect and understand the chemicals you are using with Material Safety
Data Sheet (MSDS). The MSDS are available in the analytical room.
2. All chemicals in the laboratory are to be considered dangerous. Do not touch, taste or smell any
chemical unless specifically instructed to do so.
3. Check the label on chemical bottles before removing any of the contents. Take only much
chemical are you need. Smaller amounts often work better than larger amounts.
4. Label all containers and massing papers holding dry chemicals.
5. Never return unused chemicals to their original containers.
6. Never use mouth suction to fill a pipette. Use pipette bulb or pipette filler.
7. Acids must be handled with extreme care. Always add acids slowly to water, with slow stirring
and swirling, being careful of the heat produced, particularly with sulfuric acid.
8. Handle flammable hazardous liquid over a pan to contain spills. Never dispense flammable
liquids anywhere near a flame or source of heat.
9. Never take chemicals or other materials from the laboratory area.
10. Take good care when transferring acids and other chemicals from one part of the laboratory to
another. Hold them securely and in the method demonstrated by the instructor as you walk.
11. All wastes generated during the course of an experiment must be disposed of according to the
lab instructors directions.
12. Never mix chemicals in sink drains.
13. Sinks are to be used only for water and those solutions designated by the instructor.
14. Solid chemicals, metals, matches, filter paper, and all other insoluble materials are to be
disposed of in the proper waste containers, not in the sink.
15. Checks the label of all waste containers twice before adding your chemicals waste to the
container.
16. Cracked or broken glass should be placed in the special container for broken glass.
17. Keep hands away from your face, eyes, mouth and body while using chemicals. Wash your
hands with soap and water after performing all experiments.

Personal Hygiene
1. Wash hands before leaving the lab and before eating.
2. Gloves should be removed before leaving the lab, using telephones, or entering common areas

Accidents and Injuries

1. Report any accidents (spill, breakage, etc) or injury (cut, burn, etc) to the instructor immediately,
no matter how trivial it may appear.
2. If you or your lab partners are hurt, immediately tell to the instructor.
3. If a chemical should splash in your eye(s), immediately flush with running water from the
eyewash station for at least 20 minutes. Notify the instructor immediately.
4. Spills should be cleaned up immediately.

Handling Glassware and Equipment

1. Inserting and removing glass tubing from rubber stopper can be dangerous. Always lubricate
glassware (tubing, thistle tubes, thermometer, etc) before attempting to insert it in a stopper.
Always protect your hands with tower or cotton gloves when inserting glass tubing into, or
removing it from a rubber stopper.
2. When removing an electrical plug from its socket, grasp the plug, not the electrical cord.
3. Hands must be completely dry before touching an electrical switch, plug or outlet.
4. Examine glassware before each use. Never use chipped or cracked glassware.
5. Never use dirty glassware.
6. Do not immerse hot glassware in cold water; it may shatter.
7. Report damaged electrical equipment immediately. Look for things such as frayed cords,
exposed wires and loose connections. Do not use damaged electrical equipment.
8. If you do not understand how to use a piece of equipment, ask the instructor for help.
9. Be careful when lifting heavy objects. Lift comfortably, avoid unnecessary bending, twisting,
reaching out, and excessive weights, lift gradually and keep in good physical shape.
10. Do not transfer a glassware form one laboratory to another without permission from instructor.

5
 Heating Substances
1. Do not operate a hot plate by yourself. Take care that hair, clothing, and hands are a safe
distance from the hot plate at all times. Use of hot plate is only allowed in the presence of the
teacher.
2. Heated glassware remains very hot for a long time. They should be set aside in a designated
place to cool, and picked up with caution. Use tongs or heat protective gloves if necessary.
3. Never look into a container that is being heated.
4. Do not place hot apparatus directly on the laboratory desk. Always use an insulated pad. Allow
plenty of time for hot apparatus to cool before touching it.
5. If leaving a lab unattended, turn off all ignition sources and lock the doors.

Ended the Experiments

1. At the end of the laboratory sessions, you should;
Shut-off main gas outlet
Turn-off the water inlet
Desk top, floor area and sink are clean
All equipment is cool, clean and arranged
2. All equipment use should be flushed using deionized water.

6
 SAFETY DECLARATION FORM
The Dean/Head of Campus
Universiti Kuala Lumpur
Malaysian Institute of Chemical and Bioengineering Technology
Lot 1988, Vendor City Industrial Area
Taboh Naning, 78000 Alor Gajah
Malacca

Dear Sir,

SAFETY DECLARATION

I ...ID No. .
declare that I have read and understood the safety rules and regulations in UniKL MICET. I hereby
agree to abide by all the rules and regulations stated in the safety guidelines.

I hereby understood the contents and will disciplinary action will be taken against me, if I do not abide
by the stated rules.

I am fully responsible for all my actions during laboratory sessions.

Thank you.

Yours faithfully,

.
Name:
Matrix No:
Subject: NKB 10402 Chemical Engineering Laboratory 1
Date:

7
Demonstrators: Technicians:
Dr. Ng Law Yong & Ir. Zaimul Khalil Mustaffa Exp. 1 & 5: Mr. Mohd Fadil Md. Amin
Exp. 2: Ms. Nurahzlinda Ahmad
Exp. 3 & 4: Mr. Mohd Sukri Rahmat
Exp. 6: Mr. Azam
Exp. 7 & 8: Mr. Sulaiman Othman, Mr.
Khairul Azmi Abdul ghani and Mr. Mohd
Fauzi Rosli

Please remember:
All lab report MUST be handed in to the lecturer-in-charge not later than one week after the practical
session.

8
 REPORT PREPARATION AND MARKING

Writing up experiments

Report-writing is an essential part of the engineer's craft. It is the formal means by which ideas and
information are transferred to others. You must therefore be able to write and present your information
sufficiently clear and ensure that it can be easily understood.

Experiments should be written up in the way traditionally used in scientific literature. All experiments must
be written as a full-length report. If you are at all in doubt about the style and layout of scientific papers, go
to the Library and look at academic research journals such as Combustion & Flame, Chemical Engineering
Science, etc.

Your laboratory reports must be word-processed. If you think or know that you cannot typeset equations or
graphs properly, then you should talk to a fellow student, demonstrator or your personal tutor. Remember
that the Department's computing resources are limited and that lack of access to a computer terminal will
not be accepted as a valid excuse for the late submission of a report.

A Typical Laboratory Experiment Report

My Name

Date of experiment

Summary

Even though it comes at the beginning you would write this section last. It is a brief statement of what you
did and what you found. It should directly address the original aims of the experiment. If you have
calculated a numerical constant give its value and comment on its validity. It will be mainly based on your
conclusions so will not repeat theory, experimental method etc. The length of the summary will reflect the
st
volume of work done. For a PhD Thesis the summary may be up to 300 words whereas for a 1 year
laboratory experiment it will normally be less than 100 words, a typical example being as follows:

Pressure drop was measured across a section of horizontal pipe for a range of flow rates. By calculating
Reynolds number the data was seen to cover both laminar and turbulent flow regimes. Calculated values
of friction coefficient were compared with established theory. Excellent agreement was found in the laminar
flow region, but agreement in the turbulent region was poor. This may be because the assumed pipe
roughness was incorrect.

Aim(s)

A simple statement of what it is you plan to do in the experiment. Point form is preferable. For example:

The aim of the experiment is to determine the friction coefficient of a horizontal pipe for both laminar and
turbulent flow and to compare the values with established theory.

Introduction

This is another brief section. You should introduce the experiment by providing background information to
put the topic in an engineering or scientific context. For example the importance of friction factor in the
design of flow systems.

9
Theory

Before you write this section you will have studied any theory given in the laboratory manual, perhaps
supplemented by text books and lecture notes. You should not attempt to reproduce all of this here. The
level of detail of theory should typically be only that required for the processing, analysis and discussion of
your data. The derivation of the equations would not normally be of direct relevance to the aims of the
experiment so would not be included.

What you must include are any equations that you are going to rely upon in analysing your data. This will
include any equations needed to process your measurements (for example calculating a pressure drop
from a measured height on a manometer) and any equations or theoretical data which you are going to
compare with your data. The theory should be briefly introduced, for example stating any main limitations
to its use. Each equation should be given a number, so that you can easily refer back to them later in the
report, and all variables should be defined and units given, as typically your original measurement will be in
a different unit.

For example the pipe flow experiment would require an equation for Reynolds Number
VD
Re (1)

where:
V = Average velocity of fluid in pipe (m/s)
D = Internal pipe diameter (m)
= Fluid density (kg/m )
3

= Fluid dynamic viscosity (Ns/m 2)

information would also be needed on how Re can be used to determine laminar and turbulent flow
regimes. Other equations needed would be those to predict friction factor for both laminar and turbulent
flow, an equation to calculate friction factor from the data measured and equations to convert the
manometer reading to a pressure drop in the appropriate units and the flowrate measurement to an
average velocity.

Note above the convention of symbols being written in italics (Microsoft equation editor will do this
automatically).
Note also that as with the Aims and the Introduction sections, much of the Theory section could, in
principle, be written before you actually conduct the experiment.

Experimental Method

This is a description of what was done. It will normally start by briefly describing the experimental system
used, with reference to a diagram, followed by an outline of the method.

The diagram of apparatus is a key part of the report. It should have a figure number and title, and include
all the main parts of the equipment, with suitable labels so that you can easily refer to it in your method
description. Computer drawing packages are available but a carefully hand drawn and labelled diagram is
acceptable, and can often convey more information. You should sketch out you diagram during the
experiment.

In describing the method include all the main steps. Use the past tense and avoid using the first person.
For example valve 2 was adjusted until the required flowrate was indicated on the rotameter is clear and
correct, whereas I twist the valve whilst my lab partner reads the flowrate is wrong is many respects.

Another important aspect of the apparatus can be its dimensions, for example a pipe length and diameter,
which you need to perform your calculations. Make sure you record all these during the experiment and
include them in the report. From the theory section it may also be apparent that certain system properties
are needed, for example fluid density and viscosity, which may depend on conditions during the
experiment, such as temperature. Again make sure that the necessary data is obtained during the
experiment and detailed in the report.

The accuracy to which you do the experiment is a key factor, and can often be the limiting factor in gaining
agreement between your data and theory. Your description should include details of the type of
10
measurement instruments being used and, where possible, an indication of their accuracy. For example
flowrate was measured on a 2 l/min to 20 l/min rotameter with a reported accuracy of 1% of full scale.
The demonstrator should be able to give details of how instruments work and their accuracy. Details of
estimating errors are given in the laboratory handbook and would typically form part of the data analysis,
but instrument accuracy should be recorded in the method section.

Experimental Results

This is simply a record of the data recorded during the experiment. Normally it would be given in one or
more Tables, which would include units and numbers reported to an appropriate accuracy, typically
consistent with the instrument accuracy. Remember that a report is read and so the text must refer the
reader to all Tables, Figures, Graphs, Equations, Appendices etc. which otherwise could be missed,
especially in a large report. So this section would typically start The data obtained is given in Table X and
then give further detail as required of how the data is presented. It is important that all the raw data is
presented in the report, that is before any changes of unit or other calculations have been done

Analysis and Discussion

In this section you will apply to the data the theory and equations detailed in the Theory section. At this
stage you can check to make sure the Theory section contains all but only equations necessary here.
Typically you may need to change raw data to another form, or use it to calculate other variables, and then
perform some comparison with theoretical values, either calculated from theoretical equations or extracted
directly from the literature. You should give an example of each of the main calculations performed,
sufficient that any errors can be easily detected, but avoid unnecessary repetition. The final results of the
calculations are often best presented in a Table, which may be an extension of the original data Table if
convenient, and then plotted on one or more graphs.

The illustration of data in graphical form is a key skill which will be of value throughout both your course
and your career, so time spent developing this skill is very worthwhile. Basic graphs can be produced in
EXCEL, but note that the basic default x-y scatter format with grey background and single set of grid lines
needs to be re-formatted. More advance packages such as SIGMAPLOT can produce very professional
results. In designing your graph you should think carefully about what you are trying to illustrate. Avoid
unnecessary detail which can obscure the main aim of the graph. Remember that if you are comparing
your measured data points with a theoretical equation, it is often best to present your data simply as
discrete points, with no associated line, whilst the theory equation is represented by a line, with no points.
Appropriate selection of symbols and line styles, together with a legend, then enables several sets of data
and theoretical predictions to be included on a single graph. Alternatively you may be trying to match a
best-fit line to the data, and computer packages have facility for this. Each graph should have a Figure
number and title and be referred to within the text of the report. Axes should be suitably labelled including
units.

Often it is only after the results have been plotted that the main findings of the experiment become
apparent, so you are advised to plot out your results before writing the discussion. Remember that any
claim you make about your experiment must be justified by your results, and a clear graphical
representation often provides such justification.

The discussion is perhaps the most critical part of the report, in that it enables you to put the results in the
context of established theory and to demonstrate your depth of understanding of the topic.

The discussion should focus on the aims of the experiment. It should typically identify any significant trends
arising from the data analysis and compare results obtained with established theory. Specific discussion
points are sometimes also identified in the laboratory manual, and these should also be addressed. You
should be critical in your discussion and try to explain any disagreement with theory in a logical and
constructive way. The impact of errors or uncertainties on your results should also be considered. Error
bars can sometimes be usefully incorporated on graphs.

If you are conducting an extended or open-ended laboratory, the discussion may also identify and define
further experiments required to be done, which would then be reported in subsequent sections of the
report.

11
Conclusions

This should only draw upon the analysis and discussion included in the body of the report. It should not
introduce new material. It can often be well presented in the form of bullet points, but this is not necessary.
It will typically contain more detail than given in the summary. For example, for the sample summary given
earlier, the conclusions may have been as follows:
The pressure drop measured across a length of horizontal pipe was found to increase with
increasing flow rate.
The Reynolds number for the flow was calculated and found to vary from 1100 to 7500, indicating
flow in both the laminar and turbulent regimes.
The pipe friction factor was calculated and found to show excellent agreement with theory
throughout the laminar flow regime.
In the turbulent flow regime the agreement between measured and predicted friction factor was
relatively poor. The disagreement was much greater than the estimated uncertainty of the
measurements, but it was shown that excellent agreement could be obtained by assuming the pipe
to have a surface roughness of 0.1 mm, indicating that the assumption of a smooth pipe as
indicated in the handout may be incorrect.

Alternatively, in the context of writing a laboratory report, the following may be concluded:
Writing a laboratory report is a significant task which cannot be satisfactorily done in a last minute
panic.
The report has a formal structure which must be followed.
Writing a good report is a valuable skill which needs to be developed through practice.
An understanding of the background theory of the subject needs to be developed.
Whilst conducting the experiment details of equipment need to be recorded as well as carefully
recording the raw data.
The presentation and discussion of the results is a key aspect of the report.

References

This is a vital part of the report. If you fail to properly acknowledge and refer the work of others which you
have cited some way in writing the report you will normally be assumed to be trying to cheat by claiming
their work as your own, and be reported for plagiarism. For further information on plagiarism and unfair
means you should refer to the Department Undergraduate Handbook, the notes on MOLE and specific
guidance issued by module leaders.

References should be given in the text with name and year, e.g. (Levenspiel, 1999). Give sufficient details
to identify the source, including year and page numbers. For example:

Book:
Billmeyer, F. W. (1984). Textbook of Polymer Science. (6th ed). Toronto: John Wiley & Sons.

Journal article:
Toshihiro Hirotsu, Ketelaars, A.A.J., and Kazuo Nakayama (2000). Biodegradation of Polycarbonate/ABS
Blend Sheets. Polymer Degradation and Stability. 68, 311-316. Elsevier.

Website:
Sulco Chemical Ltd. (2001). www.sulcochemicals.com/proc.html: Plant Process and Diagrams.

Note that much of the information on the Internet should not be regarded as part of established scientific
literature, so should not form the main basis of your references.

Within your report you would not normally reproduce chunks of text from references, but if you do these
should appear in quotation marks and would not normally be longer than about 30 words. You are
expected to be able to extract the key meaning from references. Data and equations do not have to be
given in quotation marks, but the source must be given clearly.

You may wish to illustrate your Introduction or Theory section with a figure reproduced directly for a
reference (this is not encouraged and such reproduction is unlikely to be appropriate elsewhere in the
report). If this is done the reference must appear as part of the Figure title in addition to being listed at the
end of the report.
12
Some things to bear in mind:

(i) Do not leave your report writing until the night before the deadline. If you have a problem you
may not be able to resolve it in time (see Penalties for late submission below).
(ii) Do not reproduce large chunks of the handout verbatim. The handout will contain a certain
amount of background information, but is not always written in a style that is appropriate to a
scientific report.
(iii) Make sure you write in the third person and use the past tense. Write in English (no text
message-style abbreviations) remember: this is a scientific report.
(iv) Pay great attention to the accuracy of your data. Do not quote data to 7 significant figures
unless it is justified. If you use a computer spreadsheet (e.g. Excel), make sure that you
format your columns to give an appropriate number of significant figures. Markers have been
instructed to deduct marks for inappropriate presentation of data.
(v) When drawing graphs (this must be by computer), show all your data points with clear
symbols. Do not be embarrassed by scatter of data. Scatter of data may be telling you
something important about the accuracy of the experiment. Consider data points carefully
before drawing a best curve. This may not always be a straight line.

All reports must be submitted using the form available on E-learning. As explained in the introduction,
please fill in the top of the first page (remembering to sign the form before submission) and generate the
report from page two using the guidance notes. Please remember to delete the guidance notes before you
submit the report! The form is reproduced on the next page.

13
 UniKL-MICET Laboratory Report Submission Form

To: (Name of lecturer-in-charge for that particular experiment) Exp. No.:

From:(Student Name, Student ID)
1.
2.
3.
4.
5.
We agree / disagree that the attached is our own work, except where specifically stated.

TITLE OF EXPERIMENT Date of Experiment

Due Date: Office use only: RECEIVED Office Use only RECEIVED BY
Time Date

Section Note Max Marks Comments by Marker

Summary
150 words maximum 10

Aims
50 words maximum 5

Introduction
Half page maximum 5

Theory
One or two pages 10

Experimental Methods One or two pages 10

Apparatus diagram By Hand only 10

Experimental Results Tables and explanation 15

Analysis and Discussion With graphs, calcs 20

Conclusions
Principal outcomes 10

References
According to format 5

Marker: Final Mark:

Total
100

14
Summary (maximum 150 words)

1.0 Aims:

A simple statement of the purpose of the experiment, in one or two sentences.

2.0 Introduction

Explain in your own words the scientific or engineering context, in no more than half a page. Copying from
the handout or elsewhere is not acceptable. State the reasons to carry out the experiment
3.0 Theory

Give any equations (using Equation Editor function) or principles you will use in the analysis. You may
quote briefly (up to 30 words) from textbooks, but should not include derivations. Refer to your sources by
name and year, e.g. (Seider, Seader & Lewin, 2003) and give full details in your reference section.

4.0 Experimental Methods

A drawing of the main apparatus, and a brief description, followed by what was done with it. Use what is
called the passive voice. That is, write the temperature was measured.. instead of I measured the
temperature.. or we measured the temperature.

5.0 Experimental Results

Present the measurements you actually made, and possibly any direct calculations in the form of tables
which are clearly labelled and explained. For example, you may have columns showing the measured
values of mass and volume, and the calculated value of density. Note that the calculated value cannot be
to greater precision than the experimental measurement.

6.0 Analysis and Discussion

This will normally included properly formatted graphs, and calculations based on the underlying theory.
Include any relevant observations and comparisons with literature. Do not assume you are wrong just
because your results are different, but note this fact. For example: this is about 30% less than the value
given in Hanson (1985), but this may have been due to the higher temperature.

7.0 Conclusions

This should be limited to what the evidence of the experiments tells you, not what you read elsewhere. For
example:
7.1 The electrical current through Carbon speciment A increased linearly with voltage (within an
experimental uncertainty of 4%) so it follows Ohms Law.
7.2 Carbon specimen B followed Ohms law up to 5.2 V then its resistance tended to increase, limiting
the current, so it is a non-ohmic resistor.

8.0 References

Give the names (Surname, Initials) of the authors, the year of publication, the title of the journal or book
and the pages referred to. The Internet can be used for general reading, and for accessing printed
publications online, but only printed material can be given as a reference.

15
 Experiment 1: Ester Saponification

Safety Note: This experiment uses acid and alkali solutions. Protective gloves and glasses MUST
be worn at all times.

Aim

To measure the rate constant of the reaction between ethyl acetate and sodium hydroxide under batch
conditions.

NOTE In this session, each group member will carry out their own batch reactor experiment.

Introduction

Chemical engineering processes can be broadly divided into two types: batch processes and continuous
processes. In a batch process, input materials are placed in a vessel or reactor, and product is withdrawn
some time later, e.g. when the reaction has finished. This is typical of what is normally done in chemistry
laboratories. In a steady-flow continuous process, such as is often used in large chemical plant, there is a
continuous flow of material in and a continuous flow of material out. No separate filling and emptying
operations are required.

You will be studying under both batch conditions the reaction between an ester (ethyl acetate or ethyl
ethanoate) and sodium hydroxide.

CH3COOC2H5 + OH CH3COO + C2H5OH

- -

[This type of reaction is called a saponification because of its importance in the manufacture of soap.]

MEASUREMENT UNDER BATCH CONDITIONS

NOTE You should work individually for this work.

The reaction is relatively slow and the changing ester concentration can be followed quite easily by
analysing samples from the reaction mixture every few minutes. The second-order rate constant for the
reaction can then determined in two different ways.

(1) Integrated rate law method

Assuming the reaction to be a simple, irreversible, second-order process, then the rate law for a batch
process may be written

d[ester]
Rate = = k[ester][OH ]
dt
Suppose that the concentrations of the ester and hydroxide are equal at the start of the experiment and
equal to co mol/dm3, and that at some time t later, both the ester and hydroxide concentration have fallen
to c. Then we can write:

16
 dc
= k[ester][OH ] kc2
dt

Separating the variables and integrating with appropriate boundary conditions:

c t

dc
= k dt
c2
co 0

1 1
kt
c co (1)

So, a plot of 1/c, i.e. 1/[ester], against t should give a straight line with gradient k.

(2) Half-life method

Equation (1) can be rearranged to give:

1 co c
k
t coc

Let t1/2 be the time taken for the concentration of ester to be halved, i.e. c = co/2. Then

1
k
t1 2 co

i.e. the time taken to halve the concentration of ester is inversely proportional to the initial concentration.
From a plot of the ester concentration (c) against time, it is possible to determine t1/2 and hence the rate

Experimental Method

Pipette 250 cm3 of 0.1M ethyl acetate solution into a clean dry conical flask, and 250 cm3 of 0.1M sodium
hydroxide solution into a large beaker. Label six clean conical flasks 1-6 and pipette 25 cm3 of 0.1M HCl
into each of them. Place the mechanical stirrer in the sodium hydroxide solution. Turn on the stirrer, and
quickly pour all of the ethyl acetate into the beaker, starting the stopwatch at roughly the mid-point of
addition. After about 5 minutes, withdraw by pipette 25 cm3 of the reacting mixture, and run into Flask 1,
noting the time at the mid-point of delivery. Record the temperature of the reacting mixture in the beaker.
Titrate the contents of Flask 1 against 0.1M sodium hydroxide, using two or three drops of phenolphthalein
as indicator. Withdraw further samples at roughly 10, 20, 30, 50 and 75 minutes, and repeat the
procedure.

Results & Analysis

17
First note what you are measuring in this experiment. Sodium hydroxide is gradually consumed as it
reacts with the ester. When a sample is withdrawn and run into the acid, any sodium hydroxide in the
sample reacts instantly with the acid, thereby stopping any further reaction of the ester. The excess acid is
then titrated against sodium hydroxide. This determines how much excess acid remains, which can be
related to the sodium hydroxide and ester in the original sample using the method below.

Let titre of NaOH = y cm3.

Then the number of moles of 0.1M NaOH used in the titration = 0.1y/1000 mol = Acid neutralised in
titration.

Original quantity of 0.1M acid = 0.1*25/1000 mol.

So, acid neutralised by sample = 0.1(25 - y)/1000 mol = moles of NaOH present in the sample
withdrawn from the reactor.

Thus, NaOH concentration in 25 cm 3 sample from the reactor = ester concentration (c)

Determine the rate constant, k, using both the methods outlined above. In the half-life method, note that
you do not have to restrict yourself to just the very start of the experiment. Initial concentration can be
interpreted very liberally. For example, if you know the concentration at, say, t = 10 minutes, then from the
graph you can see how long it takes for that concentration to be halved, and hence obtain a value for k.
Repeat this procedure for at least five other times during the experiment to check that k is indeed constant.

Important note: The reaction being studied is an equilibrium reaction, but the kinetics equations assume it
to be a one-way (irreversible) process. The effect of the reverse reaction can be seen particularly in the c
vs t plot, where the concentration is flattening out to a constant non-zero value; the concentration of
reactant in a one-way reaction would asymptote to zero. This reverse reaction affects your determination
of k: you may see some curvature in the 1/c vs t plot, and you may get some variation in values of k
obtained from the half-life method. You will need to think about how to obtain the most reliable estimate of
the real value of the rate constant. [Hint: think about where/when in the experiment the reverse reaction is
least significant.]

References
On Chemical Kinetics:
Atkins, P.W.: Physical Chemistry (various eds), OUP, 1976 onwards 541
Frost, A.A. & Pearson, R.G.: Kinetics and Mechanism (2nd ed.), Wiley, 1961 541.394
Smith, J.M.: Chemical Engineering Kinetics (3rd ed.), McGraw-Hill, 1981 541.39
Stevens, B.: Chemical Kinetics (2nd ed.), Chapman Hall, 1970 541.39
plus any general text-books on physical chemistry.

18
 Experiment 2: Synthesis and characterizationof Alkane, Alkene and
Alkyne

Aims
o To synthesize methane, ethane and ethyne
o To characterize the prepared methane, ethane and ethyne

Introduction

Saturated Aliphatic Hydrocarbon

Alkane

Methane is first member of the family of hydrocarbons. It can be prepared in the laboratory by the reduction
of any halogenated derivatives of alkane. This type of reaction involves the replacement of one or more
atoms of halogen . The generalized scheme is:

RX HX
reduction

The chemical properties of methane are characteristic of the alkanes as groups. A convenient test for
alkanes which distinguishes them from unsaturated aliphatic hydrocarbons consists of treatment with
bromine in carbon tetrachloride. If it is an alkane; almost no reaction occurs in the dark. In bright artificial
light or in sunlight, the bromine colour is gradually discharged as the substitution reaction proceeds and
hydrogen bromide (HBr) is evolved.
To test for HBr, blow you breath gently across the mouth of the reaction tube. HBr, if present, will dissolve
in the moisture of your breath to form a cloud of droplets.

Unsaturated Aliphatic Hydrocarbons

Unsaturated aliphatic hydrocarbons have one or more multiple (double or triple) carbon-carbon bonds per
molecule.

Alkenes

The distinguishing feature of the alkene hydrocarbons is the carbon-carbon double bond. The synthesis of
alkene can be accomplished by elimination of atoms or groups from two adjacent carbon atoms. The
production of 2- methyl -2- butane from t amyl alcohol is an example of the acid catalysed dehydration of
alcohols.

Two tests can be carried for an alkene i.e:

19
 a. Bromine, dissolved in carbon tetrachloride , adds rapidly to alkenes at room temperature to
form dibromides H H

3RHC CHR + Br2 R C C R

Br Br

Evidence for the reaction is the disappearance of the bromine colour, even in the dark
with no evolution of hydrogen bromide

b. Baeyer Test. Alkenes react with neutral permanganate solution to form glycols.

OH OH

+ 2MnO4 + 2 KOH
4H2O 3 R C C R
3RHC CHR + 2 KMnO4 +
H H Dark Brown
Purple Precipitate

Alkynes

The distinguishing features of an alkynes is a carbon-carbon triple bond. Alkynes give positive Baeyer Test
for unsaturation with aqueous potassium permanganate.

This experiment contains two parts:

In Part A, you will synthesize methane, ethane and ethyne

In Part B, you will characterize prepared methane, ethane and ethyne.

Experimental Method (Part A)

Preparation of Methane by reduction of chloroform

1. Add 10 g of zinc dust into a 50 ml round bottomed flask mounted in a ring stand
2. Add 10 ml of ethanol and 10 ml of water
3. Fit the flask with a rubber stopper and a delivery tube for collection of the gas over water (see Figure
1.1)
4. Add to the mixture 5 ml of chloroform and 1 ml of 10 % copper sulfate solution.
5. The reaction may require several minutes to start. If it becomes too rapid, cool the flask in a pan of cold
water.
6. After the air in the flask has been displaced, collect (over water) at least 6 test tubes of methane by
keeping the bottles (or test tubes) inverted over the water.

20
 Figure 2.1 Apparatus for the Synthesis of Methane by the Reduction of Chloroform

Preparation of Ethene

1. Place Rocksil wool at the bottom of test tube. Drop 8 10 drop of ethanol until the rocksil wool has
been soaked up with ethanol.
2. Place about 1 g of aluminium oxide halfway along the tube ( see Fgure 2.2)
3. Fit a cork and delivery tube to the test tube and heat the aluminium oxide with a gentle flame
4. Collect at least 6 test tubes of ethene by displacement of water.

Figure 2.2: Apparatus for the Synthesis of Ethene

Preparation of Ethyne

1. Place 2 or 3 small pieces of calcium dicarbide in the a test tube (Figure 2.3) and arrange the
apparatus for collection of ethyne
2. Add 2 or 3 drops of water at a time.
3. Collect at least 6 test tubes of ethyne by displacement of water

21
 Figure 2.3 Apparatus for the Synthesis of Ethyne

Experimental Method (Part B)

Characterization tests for Methane, Ethene and Ethyne

1. Prepare FIVE sets of tubes, each set consist of 3 test tubes containing methane, ethene, and ethyne),
2. To set 1A and 1B, add 1 ml of a 4% solution of bromine in carbon tetrachloride. Stopper all the test
tube. Place one set of tubes (set 1A) containing methane, ethene and ethyne in your drawer for 15
minutes. Leave the other the other set (set 1B) in bright light (preferably sunlight).After 15 minutes,
observe the results. Open the stopper and blow your breath across the mouth of each tube. Note and
record any difference.
3. To set 2A, swirl about 2 ml of a 0.3 % solution of potassium permanganate in test tubes containing
methane, ethene and ethyne. Record your observations.
4. Set 2B; shake the tubes containing methane, ethene and ethyne with alkaline potassium
3
permanganate solution (made by dissolving about 0.1 g of anhydrous sodium carbonate in 1 cm of 1
% potassium permanganate solution). Record your observations.
3 3
5. Set 2C; add about 1 cm of acidified potassium permanganate (by adding 1 cm of sulphuric acid to
0.5 ml of 1% potassium permanganate solution). Record your observations.

22
 Results & Analysis

Observation

No Test
Methane Ethene Ethyne

SET 1A

1 Tubes left in darkness

SET 1B

2 Tubes left in a bright light

SET 1A & 1B

3 Blowing across the mouth

of each of the test tubes

SET 2 A

4 2 ml of 0.3% potassium
permanganate solution

SET 2 B

5 1 ml Alkaline potassium
permanganate

SET 2 C

6. 2 ml Acidified potassium
permanganate solution

NOTE: GIVE REASON FOR EACH OBSERVATION.

23
Points for discussion

1. What do 'saturated' and 'unsaturated' mean when applied to hydrocarbons? Give examples of a
saturated hydrocarbon and an unsaturated hydrocarbon.
2. Give Five (5) sources of methane.
3. Describe reactions that are characteristics of alkanes, alkenes and alkynes.
4. Write a balanced equation for the reaction which methane was obtained by the reduction of
chloroform.
5. Provide 2 (TWO) other methods of collecting gas that can be used in this experiment.

24
 Experiment 3: AAS: Determination of Cooper (Cu) in water by flame
atomic absorption spectroscopic technique

Aims
o To prepare a serial dilution and generate a standard calibration Curve

o To determine amount of cooper (Cu) in sample

Introduction

Atomic absorption spectroscopy is the elemental analysis that widely used in analyzing samples from
environment, metal, food, pharmaceutical and chemical industries. For measurement, sample must be
converted into free atom.
Figure below is the schematic diagram of atomic absorption spectrometer. Hollow cathode lamp will emit
the line spectrum of the element to be analyzed. Samples are then atomized in the flame. Selection of
wavelength of interest is done by the monochromator.

Figure 3.1 Basic AA spectrometer

The sample must be introduced in the aerosol form. When the samples enter the flames, the metal ions
inside the samples are then converting into free atoms and evaporate all the solvent. The common flames
used are air-acetylene and nitrous oxide-acetylene.
A premix burner is commonly used with the flame. Sample aspirated through the capillary tube, sprayed
into the spray chamber in a fine mist by a nebulizer and mixed with oxidant-air mixture. Samples are then
introduced into the flame. Large droplets of sample flow to waste and only a small amount of samples with
the smallest droplets remained.
Optimization of atomic absorption spectroscopy requires the several conditions such as to make sure the
unit is operating correctly, flame conditions is correct for the element, alignment of the burner system and
proper integration time. In order to achieve optimization, we need to check few items in the system; lamp,
nebulizer, gas flows and burner position condition. Setup element is needed to assess instrument
performance which should have the following characteristic;

o Should not be sensitive to slight changes in flame conditions

25
 o Wavelength should be greater than 250 nm (minimizes potential interferences).

o Standard solution should be easy to prepare.

o Standard solution should produce a signal of about 0.200 absorbance.

In this experiment, the ideal setup element used is copper which have a wavelength at 324.8 nm and
aspiration of solution of 4.0 mg/L should produce of 0.200 absorbance.
Characteristic concentration is the concentration of analyte that gives 1% absorption or 0.0044

absorbance (as shown in checking the Performance part). Characteristic concentration is very useful
in assessing instrument performance by showing a low characteristic concentration value which
indicates a higher sensitivity.

Experimental Method

A. Preparation of copper standard solution (* Standard solution has been prepared by

technician, student should perform dilutions starting from step 3)

1. Pour about 10 mL of 1000ppm copper standard solution into a small beaker and prepare 100ppm
copper standard solution in 100ml volumetric flask using the following equation;
MV =MV
1 1 2 2

Where;
M = Initial concentration in ppm
1

V = Initial volume in ml (volume of solution required)

1

M = final concentration in ppm

2

V = final volume in ml (volume of volumetric flask used)

2

2. Add 1% (v/v) of concentrated nitric acid (1% = 1ml) into the

100ml volumetric flask and mark up to the volume using
deionized water.

WARNING! Concentrated nitric acid is highly corrosive! Please use a glove

for protection when you are dealing with the corrosive chemicals!

26
 3. By using the freshly prepared 100ppm copper standard solution above , prepare 2.0 ppm and
4.0 ppm of copper standard solution using 100ml volumetric flask (calculate the volume of
solution required using the above equation).
4. Prepare the 0.5ppm, 1.0ppm, 1.5ppm and 2.5ppm copper standard solution using
100ppm copper standard solution. Add 1% v/v of concentrated nitric acid (~ 20 drops) to each
of the standard solution and mark up to the volume.
5. The standards solution prepared are now ready to be analyzed.

B. Operating the instrument

Please refer to the Appendix. Step 1 until 5 and then do the following order as below;

1. Optimizing the Burner System.

a. Prepare a blank solution.

b. Aspirate the known standard using 2ppm and 4ppm.

c. Adjust the burner position using the horizontal adjustment knob and the nebulizer
adjustment nut until a maximum absorbance is displayed on the screen.
d. Check the absorbance of blank solution again. It should be zero.

2. Checking the Performance

a. In the Analyses menu, click on Characteristic Concentration.
b. Enter the sample concentration and instrument reading (the maximum absorbance).
c. Press the Tab key.
d. The Measured Characteristic Concentration should be within 20% of the
Comparison Characteristic Concentration value.
e. Close the Characteristic Concentration window. The characteristic concentration
value can also be calculated using the following equation;

0.0044 X known conc. used

Characteristic Conc. Value = ___________________________
Absorbance for known conc. used

3. Creating a Calibration Curve and Analyzing Samples.

a. Creating a calibration curve.

i. Immerse the nebulizer tube into blank solution. In the Manual Analysis Control window,
click on Analyze Blank.

ii. Select the calibration standard you want to analyze from the drop-down list. The software
completes the concentration entry according to the value entered in the method.

27
 iii. Click on Analyze Standard. Repeat this step for every calibration solution; 0.5ppm,
1.0ppm, 1.5ppm, 2.0ppm and 2.5ppm.
iv. Check the calibration curve. If any of the standards appear to be off the calibration curve,
then you may wish to edit the calibration curve.

b. Analyzing the samples.

i. Immerse the nebulizer tube into sample solution.

ii. Click on Analyze Samples.

4. Shut down the instrument by following step 7 in the Appendix.

Results & Analysis

Standard solution concentration (ppm) Absorbance (mean)

0.5
1.0
1.5
2.0
2.5
Unknown 1
Unknown 2

Comparison characteristic concentration value (2ppm) = ________________ mg/L

Measured characteristic concentration value (2ppm) = ________________ mg/L
Comparison characteristic concentration value (4ppm) = ________________ mg/L
Measured characteristic concentration value (4ppm) = ________________ mg/L
% RSD (mean) = __________________
Correlation coefficient (final) = __________________

Points for discussion

1. What is the function of monochromator?

2. You are given a 100 ppm mercury stock solution. What is the volume needed in mL to prepare a
15 ppm standard stock solution in 50 mL volumetric flask?
3. How would you determine the performance of the atomic absorption spectrometer?
4. Calculate the Characteristic Concentration Value for 2 ppm copper standard that has the
absorbance value of 0.194 absorbance.

28
 Experiment 4: HPLC: Determination of caffeine in soft drink

Aims
o To Identify the presence of caffeine in soft drink sample

o To determine amount of caffeine in soft drink sample.

Introduction

High Performance Liquid Chromatography (HPLC) is a chemistry based tool for quantifying and
analyzing mixtures of chemical compounds. It can be used to separate compounds that are dissolved
in solution. HPLC instruments consist of a reservoir of mobile phase, a pump, an injector, a
separation column, and a detector. Compounds are separated by injecting a plug of the sample
mixture onto the column. The different components in the mixture pass through the column at different
rates due to differences in their partitioning behavior between the mobile liquid phase and the
stationary phase.

The area of this peak (in relation to the area of other peaks) is proportional to the concentration of that
particular species in the sample. The identity can also be found by comparing the sample peaks to
standards. Identical substances (peaks) will have identical retention times.

Experimental Method

1. Preparation of caffeine 1000 ppm standard (stock solution) (* Standard solution has been
prepared by technician, student should perform dilutions starting from step (iii))

(i) Dissolve 1.000 g of caffeine in 50 mL of HPLC solvent in a 100 mL volumetric flask with
gentle heating (in the hood). Cool to room temperature and dilute to the mark with HPLC
solvent.

(ii) Dilute 10.00 mL to 100.00 mL with HPLC solvent in a volumetric flask to obtain 1000 ppm of
caffeine.

29
 (iii) Prepare a series of dilution for caffeine standards; 20 ppm, 40 ppm, 60 ppm, 80 ppm and 100
ppm with distilled water.

2. Preparation of soda samples (*Student should only perform step (iii))

(i) Obtain a soft drink sample.

(ii) Degas the sample by placing it in a vacuum flask and connecting the flask to a vacuum pump
or water aspirator. Leave it under vacuum until no more bubbles appear in the soda sample.
(If no vacuum is available, allow the soda to stand open overnight.)

(iii) Filter the degassed soda through #42 filter paper.

Instrument set-up

1. Obtain the degassed 60:40 methanol : water solvent for the mobile phase (This has been set up in
the instrument).
2. Place solvent tube with attached metal filter into the solvent bottle the filter must be submerged.
Place the thin tube with attached black trap into the waste bottle. Place the short thin tube with no
attachment into another waste bottle.
3. Turn on the HPLC. (The switch is at the right rear above the power cord.) Prime the pump by
attaching a 60 mL plastic syringe to the nozzle at the right front of the prime/purge valve. Open the
valve by turning the knob to the left. Bring the flow of solvent up to 1.50 mL/min by using the
up/down arrows on the front display. Make sure the valve is open before pushing the prime
button. If it is not, the column could be damaged. Push the prime button and pull solvent into
the syringe until no air bubbles are observed in the solvent tubing or the syringe. Stop the pump,
close the valve, and remove the syringe. Press the run button and let the HPLC run approximately
15 minutes before injecting your sample. (Make certain that waste is collecting in the waste bottle.)
Discard the solvent in the syringe in the waste bottle.
4. Turn on the computer and double click on the Peak Simple program. Once the computer and HPLC
have communicated for awhile, Standby will appear in the upper right corner of the display.
5. Set the range to 0.020 absorbance by pressing up/down range arrows.
6. Press the Autozero button.
7. Make sure all bubbles are removed from the tubing and detector.
8. Clean the syringe by rinsing several times with the solution to be injected.
9. Rinse the 100 L syringe several times with your sample. Draw up sample to the 100 L mark, and
expell down to 80 L; make sure that there is no air in the syringe.
10. Make sure the injector lever is in the LOAD position, and insert the sample with the syringe.
11. Move injector lever to inject position. The display in the upper right corner of the computer screen
will change from standby to running in red letters. If it doesnt, press the spacebar, or click on
acquisition, then run.

30
12. The run may be stopped by pressing the end key on the keyboard or clicking on acquisition, then
stop and postrun. Be sure to note the number of your run. This can be observed by looking at
the upper left line of the computer.
13. Return injector lever to LOAD position.
14. Print or save any runs if instructed to do so.
15. Repeat steps 7 - 13 for each sample (standards and sodas).

Results & Analysis

1. Use standard benzoic acid /caffeine retention time to identify the benzoic acid/caffeine peak
and then record their retention time.
2. By using above information, clarify and justify the present of benzoic acid/caffeine in the soda
sample.
3. Record different concentration of standards peaks area and construct a standard calibration
curve (concentration vs peak area).
4. Measure the caffeine peak in the soda sample chromatograph, and use standard calibration
curve (concentration vs peak area) to determine the concentration of Benzoic acid/ caffeine in
the soda sample.
Note: All raw data must be record in table form.

Instrument shut-down

1. Clean syringe with methanol (HPLC grade).

2. Run 100% methanol (HPLC grade) as a solvent for 5-10 minutes.

3. Turn off pump, detector, and computer.

Note: Failure to clean the column may result in a clogged column. Please clean after each
class.

Points for discussion

1. Why does the syringe have to be carefully rinsed before each use?
2. Retention of caffeine in standards. How could you be identify a peak in the soda was caffeine and
not another substance by using retention time?

Reference
Gas Chromatography (Analytical Chemistry: an introduction- 7th edition, Skoog et al., chapter 25A)

31
 Experiment 5: Activation Energy of an Ionic Reaction

Safety Note: This experiment uses strongly oxidizing solutions. Protective gloves and glasses
Must be worn at all times. Place any waste solutions in the large beaker provided, so that the
technicians may safely dispose of them after the practical session. Do not pour strongly
oxidizing solutions into the nearest sink.

Aim
=
To investigate the rate of reaction of peroxydisulphate ions (S2O8 ) with large excess of iodide at a
o o
number of temperatures between 30 C and 70 C, and determine the activation energy of the
reaction.

Introduction

Peroxydisulphate ions (also known as persulphate) are powerful oxidizing agents, and react with
iodide ions to form iodine via the overall reaction:

S2O8 + 2I 2SO4 + I2
= - =

The rate of reaction is dependant on the concentrations of the peroxydisulphate and iodide ions. If
iodide is present in much higher concentration than peroxydisulphate , then the concentration of
iodide will hardly change during the experiment. The rate of reaction will then appear to depend only
on the concentration of peroxydisulphate ions. The rate law can be written:

where k , which includes any dependence on iodide concentration, is known as the pseudo first
order rate constant for the reaction.

Consider such an experiment, where the iodide ion concentration is in excess. Suppose that the initial
=
concentration of S2O8 is ao and that by time t is has fallen to a. We can use these boundary

conditions to integrate the rate law:

Integration of this equation leads to:

( ) (1)

32
 =
In principle, if we can monitor the change in concentration of S2O8 with time, then the rate constant
can be calculated. In your experiment, you will not be measuring the rate constant directly, but you
will use an indicator to show how fast the reaction is proceeding. suppose that is the time taken for
a fraction of the S2O8= to be used up. i.e. the concentration of S2O8= will fall from aO to aO (1- ).
Substitution into Equation (1) gives:

Which tells us that the rate constant is inversely proportional to the time for a fraction of the
reaction to occur. Thus if we vary the reaction conditions (e.g. temperature) and monitor the time
taken for a fixed amount of peroxydisulphate to react,we can infer how the rate constant changes.
The rate constant (k) for any reaction varies with absolute temperature (T) according to Arrhenius
Equation:

(2)

Where E is the activation energy of the reaction, R is the molar gas constant (8.314 j/mol.k). and A is
known as the A- factor, which is related to the frequency of collision between the reacting molecules.
We have al ready shown that k is proportional to 1/ , so if the arrhenius Equation holds, a plot of in
against 1/T will give a straight line of slope (E/R), from which E may be readily determined.

Experimental Method

5 thermostatically controlled water baths are used in this experiment. The temperature of the water
in each water bath is controlled by the control knob located on the right hand side of each bath. A
more accurate measurement of water temperature is obtained using a mercury thermometer
immersed in the water.

3 3
Place 10 cm of 0.5 M potassium iodide (KI) and 5 cm of 0.01M sodium thiosulphate (Na2S2O3) in a
O
boiling tube and place the tube in the plastic rack in the 30 C water- bath. Place in second tube 10
3
cm of 0.02 M potassium peroxydisulphate (K2S2O8) and add to it a small amount of iodine indicator.
Allow the crystals to dissolve, and place the tube in the rack in the water bath next to the first. Allow
the contents of the tubes to reach the temperature of the thermostat, using a thermometer to monitor
the temperature. (N.B.: take care not to contaminate your solutions. Do not transfer the thermometer
from one tube to the other.) Record the temperature of the water bath, quickly pour the contents of

33
one tube into the other, and start the stopwatch. Stir the reactant and time how long it takes for the
colourless solution to turn blue. Adjust the thermostat setting and repeat the procedure in roughly 10
o o
C steps to 70 C. You may save time by using several water- baths simultaneously.

Results & Analysis

In this experiment peroxydisulphate ions start to oxidise to the iodide and to liberate iodine as soon as
the solutions are mixed. The thiousulphate immediately reacts with (and removes) the generated
iodine, so no colour is seen for as long as there is thiousulphate in solution. When all the
thiousulphate has reached any futher iodine generated gives aclour change. Because the same
volumes of the reagents are used at each temperature, the same fraction of the original
peroxydisulpahte has reacted each time when the colour appears. Thus the equations derived above
can be used to determine the activation energy of the reaction.
Plot ln K against 1/T (remembering that T is absolute temperature). Hence determine the activation
energy for the reaction.

Points for Discussion

How good is the approximation that the iodide concentration remains constant? Use evidence both
from the experimental method and from your results to justify your argument.

References:

Atkins, P.W.: Physical Chemistry (various edns),OUP, 1976 onwards 541

Atkins,P.W. & Beran, J.A.: General Chemistry, Sci Am books, 1992 540
Frost, A.A. & Pearson, R.G.: Kinetics and Mechanism ( 2 nd ed.)wiley, 1961 541394
rd
Smith,J.M,: Chemical Engineering Kinetics (3 ed),mcgraw hill, 1981 541.39
nd
Steven, B,; Chemical Kinetics (2 ed). Chapman hall, 1970 541.39

Note: you will probably have difficulty tracking down kinetic data for the specific reaction studied here.
However, you should be able to use the literature to find the range of typical activation energies for
ionic reactions in solution.

34
 Experiment 6: Refrigeration cycle

Aims
o To determine the coefficient of performance of a refrigeration unit.

o To study the effect of evaporating and condensing temperature on the refrigeration rate
and condenser heat output.

o To investigate the effect of compressor pressure ratio on system performance.

o To determine the overall heat transfer coefficient between R141b and water in the
evaporator and condenser.

Introduction

A refrigerator is defined as a machine whose prime function is to remove heat from a low temperature
region. Since energy cannot be destroyed, heat taken-in at a low temperature plus any other energy
input must be dissipated to the surroundings. If the temperature at which the heat is dissipated is high
enough to be useful (for example space heating), the machine is then called a heat pump.
Clausius statement of the Second Law states that heat will not transfer from a cold space to a hotter
region without the aid of an external agency. Thus a refrigerator requires a compressor to operate.
The most common type of refrigerator operates on a vapor compression cycle. The components of a
vapor refrigeration system are:

i. Compressor which uses work input to increase the pressure of the vapor being
transferred to the condenser

ii. Condenser where the high pressure vapor condenses, rejecting heat to its surroundings

iii. expansion device controls the flow of liquid refrigerant and reduces the pressure

iv. evaporator heat is taken from low temperature region as the liquid evaporates at low
pressure

Condenser

Expansion device

Compressor

Evaporator 35
Figure 1: Refrigeration Demonstration Unit

36
The refrigeration cycle can be plotted on a Pressure-Enthalpy diagram

P
3
2

4 1

The Coefficient of Performance (COP) is an indicator of the performance of a refrigeration cycle:

Refrigeration effect, Q c
COP =
Compressor work, W
h1 h 4

h 2 h1

Experimental Method

1. Start the unit and ensure that the unit is air free by venting air from the condenser.

2. Set the evaporator water flow to a mid range value and allow the unit to run approximately 15 -
20 minutes.

3. Record all system parameters.

4. Repeat the experiment for 5 different condenser pressures by adjusting the condenser water flow
rate from 50 g/s to 10 g/s.

37
Analysis

Test No. 1 2 3 4 5

2
Gauge Evaporator Pressure, Pe (KN/m )

2
Absolute Evaporator Pressure, Pe (KN/m )

o
Evaporator Temperature, T5 ( C)

Evaporator Water Flow Rate, ms (g/s)

o
Evaporator Water Inlet Temp, T1 ( C)

o
Evaporator Water Outlet Temp, T2 ( C)

o
Condensed Liquid Temp, T8 ( C)

2
Gauge Condenser Pressure, Pc (kN/m )

2
Absolute Condenser Pressure, Pc (kN/m )

o
Condenser Temp, T6 ( C)

Condenser Water Flow Rate, mc (g/s)

o
Condenser Water Inlet Temp, T4 ( C)

o
Condenser Water Outlet Temp, T3 ( C)

o
Compressor Discharge Temp, T7 ( C)

Compressor Power Input, W (watts)

38
Points for discussion

a) i. Plot the cycle on the P-h diagram for different condenser pressures to determine the enthalpy
values.
ii. Determine the COP for different condenser pressures.

b) i. Calculate the heat transfer in evaporator for different condenser pressures.

ii. Calculate the heat transfer in condenser for different condenser pressures.
iii. Calculate the compressor pressure ratio (Pc/Pe).
iv. Plot graph of heat transfer in evaporator and condenser vs. pressure ratio.
v. Calculate the overall heat transfer coefficient in evaporator and condenser at different
condenser pressures.

Additional Information:

2
a) Water Coil Surface Area of Condenser = 0.032 m
2
b) Water Coil Surface Area of Evaporator = 0.032 m

c) Specific Heat Capacity of Water, Cp = 4.18 kJ/kg.K

d) Refrigerant Used: R141b or 1,1-dicholoro-1-fluoroethane

39
40
 Experiment 7: Method of Flow Measurement

Aims
o To demonstrate typical flow measurement devices for incompressible fluids: (1) venturi
meter, (2) orifice plate and (3) rotameter.

o To determine the head loss incurred by each of these device.

Introduction

In engineering and industrial practice, fluid measurement of many of the variables and properties,
such as density, viscosity, pressure, velocity, flow rate and etc is one of the problems most frequently
encountered by engineers. It is therefore essential for engineers to be well equipped with knowledge
of the fundamentals and existing methods of measuring various fluid properties and phenomena. This
apparatus is specially designed to obtain the flow rate measurement by utilizing three basic types of
flow measuring techniques, which are float-type flow meter, venturi meter and the orifice meter.

Experimental Method

1. Connect measurement lines.

2. Open all valves at pipe section and the six tubes manometer.

3. Switch on the pump and let the water flow for one minute or until all air has been expelled
from the pipe work, then switch off the pump.

4. Close both the inlet and flow control valves. Let the vent and drain valves of the six tubes
manometer opened.

5. Now immediately close vent and drain valves.

6. Adjust the height of the manometer tubes by slightly opening and closing vent and drain
valves until the height of the manometer become 150 mm.

7. Switch on the pump and open inlet valve slowly.

8. Adjust the height of the water in the manometer tubes with the help of flow control valve until
you get the difference in levels between each manometer.

9. Record the flow rate shown by the rotameter.

10. Without adjusting any valves, convey the water outlet hose into a container whose capacity is
known and record the time taken for the water to fill it up.

11. Record manometer readings in the sample reading table.

41
12. Record the volume of water collected in the catch tank V in time t.

13. Repeat step 8 to 11 for other flow rate.

Figure 7.1: Flowmeter Apparatus

42
Analysis

Manometer Reading (mm)

Flow rate calculated

Rotameter Rotameter Manometer Flow rate using Bernoullis Eq. Head loss
(L/min) (L/hr) Reading Vol. Time Q (L/min) (L/min) hL (m)
(mm) (L) (min)
1 2 3 4 5 6 Venturi Orifice Venturi Orifice
200 20
300 20
400 20
500 20
600 20

43
 Points for discussion

1. Determine the flow rate of Q as given by (1) venturi meter, (2) orifice plate

2p
Q = Ad k p

Where:

p = hg with h = h1 h2 for orifice meter

h = h3 h4 for venturi meter

litre
For venturi meter :k= 240
hr mbar

litre
For orifice meter :k= 293
hr mbar

2. Determine the head loss incurred by each of these devices.

Venturi meter : hf34 = h3 h4

Orifice meter : hf12 = 0.83(h1 h2)

3. What are the limitations of Bernoullis Theorem?

4. What are the primary considerations when selecting a flow meter to measure the flow rate of a
fluid?

5. Explain how flow rate is measured with obstruction-type flow meters. Compare orifice meters
and venturi meters with respect to cost size, head loss and accuracy.

References

th
1. Robert L. Street, Gary Z. Walters, John K. Vennard. Elementary Fluid Mechanics. 7 Ed.
John Wiley & Sons Inc.
2. Anthony Esposito. Fluid Mechanics with Applications. Prentice Hall International Inc.
th
3. Robert L.Mott. Applied Fluid Mechanics 5 Ed. Prentice Hall International Inc.

44
 Experiment 8: Drag coefficient

Aims
o To analyze the phenomena of free-falling body in any fluid.
o To determine the terminal velocity.
o To measure the drag coefficient of spheres over several decades of particle Reynolds
number.

Introduction

Any solid object moving through a viscous fluid will experience a resistance or 'drag force'. This is one
of the most important aspects of fluid mechanics and it must be remembered that common fluids like
air and water must be considered viscous in this context. An understanding of fluid drag forces is
therefore essential to the proper design of aircraft, trains, automobiles, ships, submarines, tall
structures, jetties and off-shore structures of all kinds. It is equally relevant to the mechanics of
particles falling under gravity; raindrops and parachutes in air, sand grain in air or water and the
settlement of kinds of all suspended solid particles in water. The drag force depends on a number of
variables and one of the more important is the shape of the moving body. In this experiment, only
spherical objects are used. This enables the relationships between more easily described parameters
such as velocity, fluid viscosity and body density to be explored experimentally. For spherical objects,
the radius is a sufficient description of the object although the specific weight of each material used
must be determined as well.

Experimental Method

1. Fill the two transparent vertical cylinders with clear liquids of different viscosities.

2. The spheres provided of various sizes and material, are dropped ONE AT A TIME from the top of
the cylinders and allowed to fall to the bottom. Their passage between the 1m marks on the wall
of the cylinders being timed with a stopwatch and recorded.

3. When each sphere has arrives at the recess in the base of the cylinders, it is removed by turning
the valve through 180, by rotating the knob, then sliding the valve outwards by pulling the knob.

4. After ejecting the sphere, the valve should be returned to the operating position (the knob should
be pushed in with the indicator mark uppermost).

5. Repeat the whole process with other different sizes and material of sphere.

6. It is important to remove each sphere as it reaches the valve, as two or more larger spheres will
prevent the valve from operating.

45
 inlet

1m

Bottom
valve
Figure 8.1: Two transparent vertical cylinders

7. Values of D and therefore r should be obtained using a micrometer gauge. Care must be
taken not to over tighten the gauge on the plastic spheres as this may result in flats, which will
spoil their shape.

Note:
Liquid should be drained from the equipment after use and the cylinders cleaned /
flushed with water.

To obtain reasonable accuracy with the larger spheres it is advisable to average a

number of t values obtained over repeated drops.

Results & Analysis

Table 1: Diameter and mass of the spheres

Sphere Diameter, D (cm) Mass, m (g)

46
 Table 2: Time taken by the spheres from top line to the bottom line (1 m)

Liquid 1 Liquid 2
Sphere Time, t (s) Time, t (s)
1 2 1 2

Table 3: Viscosity and specific gravity of the liquids

Liquid Viscosity (cP) Weight, f

Calculation

1. The specific weight of the sphere should be determined by first finding the mass of a large
sphere of each material (in kg) and then calculating the specific weight from the relationship:

s mg / Volume
4
mg / r 3
3
2. The terminal velocity of a sphere V is calculated as 1/t, where t is the time taken by the sphere to
fall between the 1 m marks.

3. The drag coefficient for a sphere can be shown to be:

8 r s f
CD
3 V 2

4. The total drag force can be expressed as:

u 2
FD C D .A
2

47
5. Stokes law can be used to find the viscosity of the fluid.

2 s f
r2
9 u

6. The Reynolds number can be calculated from:

ud u
Re 2r

and if the Re value is less than 1 the value of calculated from (5) is valid.

List of Abbreviations

Constant
Symbol Description Unit
Value
F Drag force N
CD Drag coefficient -
2
A Cross section area of solid object m

3
Fluid density kg/m
V Relative velocity of sphere through fluid m/s

2
Coefficient of dynamic viscosity Ns/m
s
3
Specific weight of solid object N/m
f Specific weight of fluid (f = g)
3
N/m
r Radius of sphere m
D Diameter of sphere m
Re Reynolds number of solid object -
t Time for solid object to fall through 1m s
m Mass of solid object kg
2
g Gravity acceleration 9.81 m/s

(mm /s @ cSt)
2
Liquid SG
NaCl 1.19 2.4
Hydraulic oil 1.25 28

48
 Points for discussion

1. Plot CD and 1/Re values obtained experimentally on a graph. Stokes Law may be shown as
24
CD and represented as a straight line.
Re

2. Comment on the agreement between the experimental points and the Stokes Law.

3. Discuss whether the liquids used are Newtonian or Non-Newtonian.

4. What is the factor that might be cause error to the calculation of the viscosity?

5. What is the relationship between CD and the Reynolds number?

6. Briefly describe the following terms:

a. terminal velocity

b. drag coefficient

References

1. Fay, J. A. Introduction to Fluid Mechanics, MIT Press, Cambridge, 1994.

2. Debler, W. R. FluidMechanics Fundamentals, Prentice-Hall, London, 1990.

3. Bertin, J. J. Engineering Fluid Mechanics, Prentce-Hall, London, 1984.

th
4. McCabe, W. L Smith, J. C. and Harriott, P. Unit Opemtions of Chemical Engineering, 5 Ed.,
McGraw-Hill, New York, 1993.

49