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NKB 10402

Chemical Engineering Laboratory 1

Laboratory Manual

1

Contents

INTRODUCTION

3

LABORATORY SAFETY GUIDELINES

4

SAFETY DECLARATION FORM

7

NKB 10402-LABORATORY SCHEDULE

8

REPORT PREPARATION AND MARKING

9

Student number

Error!

Bookmark not defined.

Experiment 1: Ester Saponification

15

Experiment 2: Synthesis and characterizationof Alkane, Alkene and Alkyne

18

Experiment 3: Activation Energy of an Ionic Reaction

24

Experiment 4: AAS: Determination of Cooper (Cu) in water by flame atomic absorption spectroscopic technique

28

Experiment 5: HPLC: Determination of caffeine in soft drink

31

Experiment 6: Multi Pump Test Rig

34

Experiment 7: Method of Flow Measurement

45

Experiment 8: Demonstration of Bernoulli’s Theorem in Fluid Flow

49

2

INTRODUCTION You are required to carry out eight experiments during the first year. Eight (8)
INTRODUCTION
You are required to carry out eight experiments during the first year. Eight (8) experiments must be
written up and handed 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 three/four and details of working arrangements are
given on the laboratory sheets together with the timetable. All reports must be submitted in group.
If you are unable to attend a practical class for a valid reason, please meet Miss Yuhanees Mohamed
Yusof 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 in the designated area and must not be left on benches or on
the floor between benches.
 You must wear a lab coat 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 and will not appreciate being bumped into!
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 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 happy with the data analysis that is required. Demonstrators
will help you if there is anything in the handout that is unclear. Carry out some of the calculations in the
laboratory. Then any problems can be sorted out while the demonstrators are present.
Laboratory reports must be written up and handed in to Miss Yuhanees Mohamed Yusof within one
week after your laboratory class. Late work is not acceptable (see below).
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.

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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 instructor’s 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 ………………………………

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.

……………………………………………….ID

No. ……………………….

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:

Date:

7

Thank you. Yours faithfully, ………………………………. Name: Matrix No: Subject: Date: 7
NKB 10402-LABORATORY SCHEDULE JULY 2017 Semester Technicians: Exp. 1 & 3: Ms. Juhaida Exp. 2:
NKB 10402-LABORATORY SCHEDULE
JULY 2017 Semester
Technicians:
Exp. 1 & 3: Ms. Juhaida
Exp. 2: Ms. Nurahzlinda Ahmad
Exp. 3 & 4: Mr. Mohd Sukri Rahmat/ Mr. Mohd Fadil Md. Amin
Exp. 6,7 & 8: Mr. Khairul Azmi Abdul ghani and Mr. Mohd Fauzi Rosli
*Lab venues and technicians involved are subject to change
8
REPORT PREPARATION AND MARKING Writing up experiments Report-writing is an essential part of the engineer's
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 volume of work
done. For a PhD Thesis the summary may be up to 300 words whereas for a 1 st 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. 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.
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Theory Before you write this section you will have studied any theory given in the
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.
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The accuracy to which you do the experiment is a key factor, and can often
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 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
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

Few 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

Summary (maximum 150 words) 1.0 Aims: A simple statement of the purpose of the experiment,
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
called the passive voice. That is, write “the temperature was measured
drawing of the main apparatus, and a brief description, followed by what was done with it. Use what is
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 Ohm’s Law.
7.2 Carbon specimen B followed Ohm’s 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.
14
Experiment 1: Ester Saponification Safety Note: This experiment uses acid and alkali solutions. Protective gloves
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
15
Suppose that the concentrations of the ester and hydroxide are equal at the start of
Suppose that the concentrations of the ester and hydroxide are equal at the start of the experiment and equal
to c o mol/dm 3 , and that at some time t later, both the ester and hydroxide concentration have fallen to c.
Then we can write:
 dc
=
k[ester][OH  ]
kc 2
dt
Separating the variables and integrating with appropriate boundary conditions:
c
t
dc
=
k
dt
2
c
c
0
o
1
1
kt
c
c
o
(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
 c o  c
k
t
c o c
Let t1/2 be the time taken for the concentration of ester to be halved, i.e. c = c o /2. Then
1
k
t 1 2 c o
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
constant.
Experimental Method
Pipette 250 cm 3 of 0.1M ethyl acetate solution into a clean dry conical flask, and 250 cm 3 of 0.1M sodium
hydroxide solution into a large beaker. Label six clean conical flasks 1-6 and pipette 25 cm 3 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 cm 3 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 every 10 minutes, and repeat the procedure.
16
Results & Analysis First note what you are measuring in this experiment. Sodium hydroxide is
Results & Analysis
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.
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
Smith, J.M.: Chemical Engineering Kinetics (3rd ed.), McGraw-Hill, 1981 541.39
541.394
Stevens, B.: Chemical Kinetics (2nd ed.), Chapman Hall, 1970
plus any general text-books on physical chemistry.
541.39
17
Experiment 2: Synthesis and characterizationof Alkane, Alkene and Alkyne Aims o To synthesize methane, ethane
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.
18
Two tests can be carried for an alkene i.e: a. Bromine, dissolved in carbon tetrachloride
Two tests can be carried for an alkene i.e:
a.
Bromine, dissolved in carbon tetrachloride , adds rapidly to alkenes at room temperature to form
H
H
dibromides
R
C
C
R
3RHC
CHR
+
Br 2
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
2MnO 4
3
R
+
C
C
R
3RHC
2 KMnO 4
+
4H 2 O
CHR
+
H
Dark Brown
H
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. Prepare the apparatus as shown in Figure 2.1
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.
19

+

2 KOH

Figure 2.1 Apparatus for the Synthesis of Methane by the Reduction of Chloroform Preparation of
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 in the tube ( see Figure 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
20
Figure 2.3 Apparatus for the Synthesis of Ethyne Experimental Method (Part B) Characterization tests for
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. Put stopper in all the
test tubes. 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 permanganate
solution. Record your observations.
5. Set 2C; add about 1 cm 3 of acidified potassium permanganate. Record your observations.
21
Results & Analysis Observation No Test Methane Ethene Ethyne SET 1A 1 Tubes left in
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
ml Alkaline potassium
permanganate
1
SET 2 C
6.
2
ml Acidified potassium
permanganate solution
NOTE: GIVE REASON FOR EACH OBSERVATION.
22

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.

23

Experiment 4 : AAS: Determination of Cooper (Cu) in water by flame atomic absorption spectroscopic
Experiment 4 : 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
24

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.

25

Experimental Method

A. Preparation of Copper Standard Solutions 1. Prepare the 0.5ppm, 1.0ppm, 1.5ppm. 2.0 ppm, 2.5ppm and 4.0ppm copper standard solutions. Add 1% v/v of concentrated nitric acid (~ 20 drops) to each of the standard solution and mark up to the volume. 2. 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.

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

=

Correlation coefficient (final) =

% RSD (mean)

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.

Experiment 5: 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.

between the mobile liquid phase and the stationary phase. The area of this peak (in relation

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 standard solutions

(i) 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 doesn’t, press the spacebar, or click on acquisition, then run.

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)

Experiment 3: 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 number of temperatures between 5 o C and 35 o 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:

d S 2 O 8 =  k’S 2 O 8 =  =
d S 2 O 8 = 
k’S 2 O 8 = 
=
dt
dt

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:

d a S 2 O 8 =  t = k’ dt S 2 O
d
a
S 2 O 8 = 
t
= k’
dt
S 2 O 8 = 
a
O
o

Integration of this equation leads to:

a O ln = k’t (1) a
a
O
ln
=
k’t
(1)
a

31

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-

(1) gives:

). Substitution into Equation

1 1 = ln k’ 1-
1
1
=
ln
k’
1-

Which tells us that the rate constant is inversely proportional to the time

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:

for a fraction

of the reaction

E RT
E
RT

k = A exp

E RT
E
RT
ln k = ln
ln k = ln
(2)
(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

Five thermostatically controlled water – baths are used in this experiment ranging from 30 O C to 70 O C. 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.

Place 10 cm 3 of 0.5 M potassium iodide (KI) and 5 cm 3 of 0.01M sodium thiosulphate (Na2S2O3) in a boiling

tube and place the tube in the plastic rack in the 30 O C water- bath. Place in second tube 10 cm 3 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 waterbath 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 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 30 o C steps to 70 o C.

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

Smith,J.M,: Chemical Engineering Kinetics (3 rd ed),mcgraw – hill, 1981

541.39

Steven, B,; Chemical Kinetics (2 nd 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.

Experiment 6: Multi Pump Test Rig

Aims



Determine the operating characteristic of different pumps in a contained unit.

Understand the types of pumps in principle and design, and the selection of the appropriate pump for a particular application for optimal operation.

Introduction

Pumps are of a major concern to most engineers and technicians. The types of pump vary considerably in

principle and design, and the selection of the appropriate pump for a particular application is essential for

satisfactory operation. This experiment allows students to measure the operating characteristic of different

pumps in a contained unit. This training unit incorporates appropriate pipe work and tanks to make the

operation self-contained. The manually operated valves and pipe work are arranged for rapid and safe

selection of any one-test pump. All necessary instrumentation for measurement of flow, pump head, speed

and power are included. In the experiments, students are able to operate three types of pump namely a

Horizontal Single Stage Centrifugal Pump, a Positive Displacement Plunger Pump and a Positive

Displacement Gear Pump.

Experimental Method

General Start - Up Procedures

Before conducting any experiment, it is necessary to do the following checking to avoid any misuse and malfunction of equipment.

1. Make sure that the water tank is filled with water up to at least 50%.

2. Make sure that the oil tank is filled with oil up to at least 50%.

3. Make sure that the RS 232 data cable is connected to the computer.

4. Switch on the main power supply located on the control panel. The instruments should light up.

5. Select the appropriate pump and flow meter according to the following combination.

6. Switch on the computer and monitor if you are using them to collect data and generate the characteristic

curve.

Table A

Pump

Indication

Flow Meter

Flow rate

Diff.

Pump Head

Pressure

P1/P2

0 -100%

FT 1

0 – 113.56 L/min

DPT 1

0 – 3 bar

Table B

Types of

Pump

Process

Hand Valve OPEN

Hand Valve CLOSE

Pump

Selection

Selection

Switch

Switch

Horizontal

       

Single

Stage Pump

P1

Water

HV2, HV3, HV4

HV1, HV5, HV6, HV7, HV8

Plunger

P2

Water

HV2, HV5, HV6

HV1, HV3, HV4, HV7, HV8

Pump

Important:

i. Never operate the pumps when there is no liquid in the pipeline. It will cause serious damage to the pumps.

ii. Always watch out for the direction of the motor impeller, it should follow the direction of the arrow on the pump.

Data Acquisition System

1. Power the pump Test Rig first.

2. Ensure that the cable between the computer and the Pump Test Rig is correctly connected.

3. Switch on the power to the computer.

4. Under Windows click on the Pump Test Rig icon. The program wills startup

automatically.

5. The table consists of fifteen entries and a final entry at the bottom labeled 'live'- this is the

live reading at that moment in time (online data).

6. During an experiment, if you wish capture these data, click on the 'Record' button.

7. The recording mechanism will capture at maximum 15 entries. After which it will try to

replace the closest old entry found.

8. These captured data could be saved in the form of a file. It could also be loaded later for

review or to add a new entry.

9. It is important that the user selects the correct pump before recording the data, as live data

will be represented differently for each pump.

Experimental Procedures Experiment 1 : Rotational Speed Vs Volumetric Flow rate. Performance Curve for a Centrifugal Pump

Experimental Procedures 1 for P1 Please refer to the general start - up procedures (Table B) before conducting this experiment.

1. Press the START push button to start the pump.

2. Set the motor speed to about 2800rpm using the speed control beside the speed indicator.

3. Open HV2 fully so that the flow rate is at its maximum.

4. Record the flow rate once the readings are stable. (Refer Table 1)

5. Repeat steps 2 and 4 for the following speed readings of 2600, 2400, 2200, 2000, 1800, 1600,

1400, 1200, 1000, 800 and 600rpm.

6. The data collected using above procedure will enable you to plot the following

characteristic curve:

i. Rotational speed (N) Vs. Volume Flow (Q)

At the end of experiment:

i. Adjust the potentiometer (speed control) to its minimum setting (fully anti clockwise).

ii. Please switch off the pump by pressing the stop push button at the end of experiment.

Experiment 2 : Other Performance Curve for a Centrifugal Pump

Experimental Procedures 2 for P1 Please refer to the general start - up procedures (Table B) before conducting this experiment.

1. Press the START push button to start the pump.

2. Set the motor speed to maximum (2800rpm) using the speed control beside the speed

indicator.

3. Set HV2 at full opening (50% of flowrate) so that the output flow rate is maximum and

record the readings for the flow rate, the differential pressure, the power and speed once the readings are stable. (Refer Table 2)

4. Repeat step 3 with the following flow rate of output 40%, 30%, 20%, 10%. You can try any

other intermediate reading.

5. The data you have collected will enable you to analyze the following characteristic curve:

i. Motor Input Power (PMi) Vs Volume Flow rate (Q)

ii. Pump Total Head (H) Vs Volume Flow rate (Q)

iii.

Pump Power Output (Po) Vs Volume Flow rate (Q)

iv. Pump Power Input (Pi) Vs Volume Flow rate (Q)

v. Pump Efficiency (ETA) Vs Volume Flow rate (Q)

vi. Overall Efficiency (ETAgr) Vs Volume Flow rate (Q)

At the end of experiment:

i. Adjust the potentiometer (speed control) to its minimum setting (fully anti clockwise).

ii. Please switch off the pump by pressing the stop push button at the end of experiment.

Experiment 3 : Rotational Speed Vs Output Pressure Performance Curve for a Positive Displacement Pump

Experimental Procedures 1 for P3

Please refer to the general start-up procedures (Table B) before conducting this experiment.

1. Press the START push button to start the pump.

2. Adjust the potentiometer beside the speed indicator, set the motor speed to its maximum

(About 1500 rpm for P3)

3. Slowly adjust the HV11 so that the pump head (pressure) is at 70%.

4. Record the flow rate once the readings are stable.(Refer Table 3)

5. Repeat steps 2 and 4 for the following motor speed readings of P3 = 1300, 1200, 1100, 1000,

900, 800, 700, 600, 500 and 400 rpm.

6. The data you have collected will enable you to plot the following characteristic curve.

i. Rotational Speed (N) Vs. Volume Flow Rate (Q)

At the end of experiment:

i. Adjust the potentiometer (speed control) to its minimum setting (fully anti clockwise).

ii. Please switch off the pump by pressing the stop push button at the end of experiment.

Warning: Do not close the HV11 completely when P3 is running. This may cause serious damage to the instrument.

Experiment 4 : Other Performance Curve for a Positive Displacement Pump

Experimental Procedures 2 for P3 Please refer to the general start-up procedures (Table B) before conducting this experiment.

1. Press the START push button to start the pump.

2.

Adjust the potentiometer beside the speed indicator, set the motor speed to its maximum

(About 1500 rpm for P3).

3. Slowly adjust the HV11 so that the pump head (pressure) is at 70%, record the flow rate,

differential pressure, power and speed once the readings are stable (Refer Table 4).

4. Repeat step 3 with the following pump head readings of P3 = 65%, 60%, 55%, 50%, 45%,

40%, 35%, 30%, 25%, 20%, 15% and 10%. You can try any other intermediate reading but never try to close the HV11 fully. This is to ensure that the existing pressure develop in the

pipeline doesn’t exceed the limit.

5. The data you have collected will enable you to plot the following characteristic curve;

i. Motor Input Power (PMi) Vs Output Pressure (Pr)

ii. Volume Flow (Q) Vs Output Pressure (Pr)

iii. Pump Power Output (Po) Vs Output Pressure (Pr)

iv. Pump Power Input (Pi) Vs Output Pressure (Pr)

v. Pump Efficiency (ETA) Vs Output Pressure (Pr)

vi. Overall Efficiency (ETAgr) Vs Output Pressure (Pr)

vii. Volumetric Efficiency (ETAv) Vs Output Pressure (Pr)

At the end of experiment:

i. Adjust the potentiometer (speed control) to its minimum setting (fully anti clockwise).

ii. Please switch off the pump by pressing the stop push button at the end of experiment.

Warning: Do not close the HV11 completely when P3 is running. This may cause serious damage to the instrument.

39
40
41
41
42
42
Points for discussion 1. Define pump. 2. What is the difference between dynamic pump and
Points for discussion
1. Define pump.
2. What is the difference between dynamic pump and positive displacement pump?
3. List down three factors which influence the choice of pump for a particular operation.
4. Plot the characteristic curves which have been stated in experiment 1 and 3.
Comments the plotted graphs in terms of their relationships between the y – axis and
the x – axis.
5. Plot all the characteristic curves which have been stated in experiment 2 and 4 in one
graph paper for i) P1 and ii) P3 . Comments the plotted graphs in terms of their
relationships between the y – axis and the x – axis.
43

References

1. White, F.M. Fluid Mechanics 4th Ed. McGraw Hill

2. McCabe, W.L., Smith, J.C and Harriot Unit Operations of Chemical Engineering 5th

Ed. McGraw Hill

3. Anthony Esposito. Fluid Mechanics with Applications. Prentice Hall International Inc.

4. Debler, W.R. Fluid Mechanics Fundamentals. Prentice Hall International Inc.

44

Experiment 7: Method of Flow Measurement Aims o To demonstrate typical flow measurement devices for
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 compare the difference in flow rate 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. Check the measurement line to ensure all lines are connected.
2. Open all valves at pipe section and the six tubes manometer except for the inlet valve.
3. Switch on the pump and open the inlet valve slowly to let the water flow for one
minute. Ensure all air has been expelled from the pipe work.
4. Close the outlet valve, vent valve and drain valve. Then switch off the pump.
5. Adjust the height of the manometer tubes to 150mm by opening vent valve 3 to 4
round & opening drain valve slightly.
6. Switch on the pump and open inlet valve slowly.
7. Adjust the height of the water in the manometer tubes with the help of inlet valve
until you get the difference in levels between each manometer.
8. Set the rotameter reading at 200L/hr.
9. 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 to 20L in Table 1.
10. Record manometer readings in Table 1.
11. Repeat step 8 to 11 for other flow rate (300, 400, 500 and 600 L/hr).
45
Figure 7.1: Flowmeter Apparatus 46
Figure 7.1: Flowmeter Apparatus
46
Analysis Manometer Reading (mm) Rotameter Rotameter Manometer Flow rate Difference % (L/min) (L/hr) Reading Vol.
Analysis
Manometer Reading (mm)
Rotameter
Rotameter
Manometer
Flow rate
Difference %
(L/min)
(L/hr)
Reading
Vol.
Time
Q (L/min)
Flow rate calculated
using Bernoulli’s Eq.
(L/min)
(mm)
(L)
(min)
1
2
3
4
5
6
Venturi
Orifice
Venturi
Orifice
Rotameter
200
20
300
20
400
20
500
20
600
20
47
Points for discussion 1. Determine the flow rate of Q as given by (1) venturi
Points for discussion
1.
Determine the flow rate of Q as given by (1) venturi meter, (2) orifice plate
2 
Q = Ad
p 
k
p
Where:
p = hg
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
: hf34 = h3 – h4
Orifice meter
: hf12 = 0.83(h1 – h2)
3. What are the limitations of Bernoulli’s 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
1. Robert L. Street, Gary Z. Walters, John K. Vennard. Elementary Fluid Mechanics. 7 th Ed.
John Wiley & Sons Inc.
2. Anthony Esposito. Fluid Mechanics with Applications. Prentice Hall International Inc.
3. Robert L.Mott. Applied Fluid Mechanics 5 th Ed. Prentice Hall International Inc.
48
Experiment 8: Demonstration of Bernoulli’s Theorem in Fluid Flow Aims   To determine the
Experiment 8: Demonstration of Bernoulli’s Theorem in Fluid Flow
Aims

To determine the fluid velocity using the Bernoulli’s theorem and the Continuity
equation.
 To obtain the hydraulic grade line and the total energy line.
Introduction
The Bernoulli effect is simply a result of the conservation of energy. The workdone on a
fluid (a fluid is a liquid or a gas), the pressure times the volume, isequal to the change in
kinetic energy of the fluid. In a real flow, friction plays alarge role - a lot of times you must
have a large pressure drop (decrease inpressure) just to overcome friction. This is the case
in your house. Most water pipes have small diameters (large friction), hence it is called
"water pressure" – itis the energy from that pressure drop that goes to friction.
Experimental Method
1. Fill water into the volumetric tank of the hydraulic bench until it isapproximately 90%
full.
2. Open the outlet flow control valve fully at the right hand end of the apparatus.
3. Close the inlet flow control valve then start the pump.
4. Gradually open the inlet flow control valve and allow the pipework (Venturi and
manometer) to fill with water until all air has been expelledfrom the pipework.
5. Check that all manometer tubing is properly connected to th corresponding pressure
taps and are air-bubble free. If needed press airbleeds screw slowly to flush the air-
bubbles.
6. After ensure that air is being expelled from the pipework, close the inlet valve fully
and stop the pump.
7. With the outlet valve open, press the air bleed screw slightly until the manometer
levels reach mid height (if the height of manometer is 34 mm, then the mid height is
approximately 17 mm). Wait for some time for the level in manometer tube to stabilize
(it takes some time for it to reach steady state).
49
8. Start the pump and slowly adjust the inlet valve so that you get the
8. Start the pump and slowly adjust the inlet valve so that you get the difference in levels
between tapping point 7 and 8.
9. Wait for some time for the level in manometer tube 8 to stabilize (it takes some time
for it to reach steady state).
10. After the steady state is achieved, redirect the water outlet hose into a container
whose capacity is known (20 liter, for example) and record the time taken for the water
to fill it up to 20 liter. Take at least 3 measurements and record the timings in Table A1
(Table A2 and A3 to be filled in for the other flowrate) in order to calculate (average)
flow rate.
11. Gently push the Pitot (total head measuring) tube, connected to manometer 8, so that
its end reaches the cross section of the Venturi tube at A, for example. Wait for some
time and note down the readings from manometer 8 and A. The reading shown by
manometer 8 is the sum of the pressure and velocity heads, i.e. the total (or stagnation)
head (h*), because the Pitot tube is held against the flow of fluid forcing it to a stop (zero
velocity). The reading in manometer A measures just the pressure head (h) because it is
connected to the Venturi tube pressure tap, which does not obstruct the flow, thus
measuring the flow static pressure.
50
12. Repeat step 11 for other cross sections (B, C, D, E and F). 13.
12. Repeat step 11 for other cross sections (B, C, D, E and F).
13. Repeat step 8 -12 for other flowrate (another two different flowrate) by adjusting the
inlet valve.
14. Record all the measurements acquired in Table B1, B2 and B3.
15. Calculate the velocity, ViB using the Bernoulli’s equation where:
16. Calculate the velocity, ViC using the continuity equation where:
17. Determined the difference between two calculated velocity and the percentage differ
of it.
18. Calculate the total energy head using the following equation:
19. Fill in Table C1, C2 and C3.
51
Results & Analysis 52
Results & Analysis
52
53
53
54
54
Points for discussion 1. Determine the difference between two calculated velocity and the percentage differ
Points for discussion
1.
Determine the difference between two calculated velocity and the percentage differ of
it.
2.
Plot the hydraulic grade line and the total energy line for all the readings. What do
these plots tell you about the interchange of different types of energy flow passed
through the different configurations?
3. What are the three major assumptions used in the derivation of the Bernoulli
equation?
4. Express the Bernoulli equation in three different ways using (a) energies, (b) pressures
and (c) heads.
5. What is stagnation pressure? Explain how it can be measured.
6. What is the hydraulic grade line? How does it differ from the energy grade line?
55

References

1. Joseph B. Franzini. Fluid Mechanics. 10th Ed. McGrawHill (2002).

2. John F. Douglas. Fluid Mechanics with Engineering Applications. 4th Ed. Prentice

Hall (2001).

3. Noel de Nevers. Fluid Mechanics for Chemical Engineers. 2nd Ed. McGraw Hill

(1991).

4. McCabe, W.L., Smith, J.C. and Harriot. Unit Operations of Chemical Engineering. 5th

Ed., Mc Graw Hill (1993).

56