1

CEM 2005W

INTRODUCTION TO THE LABORATORIES

PRACTICAL COURSE AND SCHEDULE

The practical courses extend over 25 weeks, during which students must complete all
experiments, practical exams, attend tutorials and complete tutorial tests. The experiments
will be allocated to students according to the timetable which will be posted on the notice
board outside the laboratories and on Vula. No departure from this schedule can be
allowed.

LABORATORY HOURS

Practicals will be held on Tuesdays and Thursdays starting at 13h30 and ending at 17h00.
Students must start clearing up by 16h30. A register will be taken and students arriving
late will be classified absent. Students will not be allowed to do practical work outside
these hours due to COVID-19 safety measures. No student may use an analytical
instrument (e.g. a spectrophotometer) without a demonstrator present.

PRECEDING THE LABORATORY

Students are expected to acquaint themselves with the experiment to be performed before
coming to the class. This involves reading the instructions and the recommended
references on Vula, and completing a flow diagram, a hazard data sheet and any pre-
practical questions. You will not be allowed to do the practical if you have not done
this. An example of a flow diagram follows (see pages 2 and 3).

Flow diagrams

It is well recognised that students can be so immersed in the details of a practical exercise
(especially syntheses) that they lose sight of what is happening and the reasons for the
various procedures they are required to implement. Construction of a flow diagram can
help to define the purpose of each step. In addition, the flow diagram can be used as a
substance audit to keep track of what species are present in the reaction mixture at each
stage of the procedure.

Flow diagrams will be checked and stamped and students failing to complete these will be
asked to leave. As it will not be possible to reschedule the experiment, failure to comply
with these requirements will result in a student being awarded zero for the practical. Any
relevant books may be used.
 2

A SAMPLE FLOW DIAGRAM:

THE OXIDATION OF BENZYL ALCOHOL TO BENZOIC ACID

O
KMnO4
CH2OH C OH

Benzyl alcohol Benzoic acid

Method

Place 4 g of potassium permanganate and 1 g of sodium hydroxide into a 250 cm 3 round

bottomed flask. Add 50 cm3 of water, attach a reflux condenser (remember to grease the
joint after adding all reagents). Clamp the apparatus above a burner and add a few boiling
chips. Take 2 cm3 (2.09 g) of benzyl alcohol and, using a dropper, add the alcohol slowly
(dropwise) to the gently boiling potassium permanganate solution. The addition should
take 5-10 minutes (longer addition times can be a disadvantage). Rinse the residue of the
benzyl alcohol down the condenser with a few cm 3 of water and allow the boiling to
continue until the reaction appears complete (10-15 minutes). Cool the reaction mixture in
an ice bath and filter off the manganese dioxide using a Büchner funnel (wet the filter
paper first with a little water to make sure it's seated correctly in the funnel). Wash
the manganese dioxide on the filter funnel with two 5 cm 3 portions of water to remove
adsorbed sodium benzoate. (Note: when filtering with the water pump, always
disconnect the tubing to the Büchner flask before turning off the water, otherwise
the water will suck back into the flask). Transfer the filtrate to a conical flask, add
enough sodium metabisulphite (one spatula at a time) so that the solutions become clear
and colourless, and then acidify with dilute sulphuric acid. After cooling the solution, filter
off the precipitated benzoic acid and recrystallise it from the minimum amount of water i.e.
the hot solution should be almost saturated with benzoic acid. (Caution: benzoic acid is
volatile in steam, and some may be lost if the solution is boiled for too long).

The flow diagram should:

(i) summarise the purpose of each stage
(ii) keep track of what species are present
 3

SAMPLE FLOW DIAGRAM

3
KMnO4 (4g) H2O (50 cm ) NaOH (1 g)

attach condenser

(1) add boiling chips (3) rinse benzyl alcohol

boil gently down condenser

3
(2) using a dropper add 2 cm (4) reflux gently 10-15 min
benzyl alcohol over 5-10 min

MnO4-, OH -, Na+, MnO2,

sodium benzoate

cool mixture in ice bath

MnO2
3
filter off MnO2, wash with 2 x 5cm
water and discard MnO2

sodium benzoate
in filtrate

MnO4-, OH -, Na+,
sodium benzoate

transfer filtrate to flask

(1) add sodium metabisulphite (2) acidify with dilute

until soln is clear and sulphuric acid
colourless

cool the soln

filter off the crude benzoic

acid

recrystallise benzoic acid from minimum amount of hot water

 4

Marking scheme for flow diagrams

Item Mark (%)

Structure

Completeness All sections present, all steps present, 40

includes subroutines where applicable
All sections present, steps missing 30
Sections missing, all steps of sections drawn 20
are present
Sections missing, steps missing 10
No sections or steps 0
Sequencing Logical 10
Some logic 5
No logic 0

Features of diagram

Representation (pictures or Correct representation 10

diagrams)
Some elements correct 5
Not correct 0
Idea of how apparatus Good idea 10
works
Some idea 5
No idea 0
Quantities indicated Yes 10
No 0
Attention to detail (shows Some evidence 10
drops or shaking)
No evidence 0

General aspects

Use with the manual Can be used in place of the manual 5

Manual required 0
Relevance of information Relevant 5
Long; irrelevant information included, steps 0
repeated instead of indicating a subroutine

Total (for all items in bold) 100

 5

LABORATORY HAZARD ANALYSIS

Look up MSDS material safety data sheets for all the chemicals you are using for your
experiment. Use the information found on them to complete the table. Sigma and Merck
are good sites to look at to find MSDSs.

SEE THE EXAMPLE BELOW:

CEM2005W LABORATORY HAZARD ANALYSIS

Chemica Chemical/physical Hazard/toxic- Action/perso First aid applicable Waste
l characteristics ological nal protection Disposal
information
methanol Colourless liquid with May form explosive Don’t inhale. If inhaled seek fresh air, Specify into
pungent odour. mixture with air. Risk Work under apply artificial respiration which waste
Boiling point 64.5 C. of explosion, ignition, hood. Avoid if breathing stops. category you
Flash point 9.7 C. and exothermic heat or ignition Remove contaminated will discard
reaction. Oral and sources. Wear clothing and rinse skin. the chemical
inhalation toxicity. safety glasses, Remove contact lenses (non-
Viton gloves, and rinse eyes. If halogenated,
and anti-static swallowed drink ethanol halogenated
flame-retardant and call doctor. or aqueous
protective (inorganic)
clothing. waste

caffeine Odourless while solid. Risk of explosion of Ensure proper If inhaled seek fresh air. Organic non-
Melting point 235- dust. Strong oxidizing ventilation. Wear Remove contaminated halogenated
239C. agents can cause safety glasses, clothing and rinse skin.
violent reactions. nitrile gloves, Remove contact lenses
Toxic orally. protective and rinse eyes. If
clothing. swallowed drink water
and call a doctor.

DURING THE LABORATORY CLASS

It is important not to follow experimental procedures blindly as one might do a recipe. A

little extra effort will greatly enhance the insights gained from the experiment, will make it
much more interesting and may save time in the long run. Ensure before you leave that
you have all your results and know exactly what is required of the writeup.

Rough graphs should be plotted during the course of the experiment where necessary.
These graphs are to be neatly redrawn for the report. All graphs must be fully labelled.
The department cannot supply graph paper - students are therefore requested to
purchase a pad of graph paper or square-ruled paper which they must bring with them.
Graph paper can also be purchased from the dispensary. Students should also supply
their own drawing equipment (ruler, eraser, pencils, etc).

Stopwatches are provided and must be signed for.

NOTE
Marks will be deducted for apparatus left dirty on completion of the class.
 6

DEMONSTRATORS

Demonstrators are there to help and guide you with both the theoretical and practical
aspects of the experiment. Ask a demonstrator if help is required but they are not there to
give you the answers to all the questions, rather to lead you to the answers.

INSTRUMENTS AND BALANCES

You will have access to delicate and expensive instruments. All instruments and
accessories must be handled with great care and responsibility. Read the instructions
carefully. If you are in any doubt concerning the operation of an instrument, consult Ms
Lawrence-Naidoo or Dr Jappie. Any breakage must be reported immediately to the
lecturer or technician in charge. Use the analytical balances to determine all masses.
KEEP THE BALANCE PANS CLEAN; use the brushes provided for the analytical
balances.

CELL PHONE POLICY

The use of cell phones in the laboratories is prohibited. Please ensure that they are
switched off before you enter the laboratory. Any cell phones that ring during the practical
session will not be tolerated. Ensure that your cell phone is switched off during the
practical session, only to be switched on after the practical session.

PRACTICAL REPORTS

Through his experiments Henry Cavendish, the eighteenth-century British physicist, came
to a deep understanding of electrical phenomena. He had, however, one serious fault - he
rarely took the trouble to write up his findings. The result was that for many years people
continued working on problems he had long ago solved. For example, he discovered
Ohm's Law of electrical resistance fifty years before Ohm did. The law is quite rightly
ascribed to Ohm though, because it was the German schoolmaster who made the
information available to others. Moral: you may get personal satisfaction from doing good
experimental work but, if you wish to get credit for it and to benefit the community at large,
you have to develop an ability to communicate your findings to others. Moreover you must
do this in sufficient detail so that others may decide for themselves whether to believe your
result or not. This is the purpose of asking you to submit a report for each experiment.
This report is not to be confused with your own laboratory notes - they are part of your
own private diary. The final report is your showpiece - it is on this that you are judged.
 7

Time management and submission of reports

Practical reports are to be submitted one week after the practical was performed via Vula
under the Assignments tab. Submission dates and times for each practical report will be
clearly indicated on Vula.

One week after handing in a report, a mark for that particular experiment will appear on
Vula. Assessment slips will also be returned via Vula. Students obtaining a low mark are
advised to consult the supervisor in charge of the practicals so that they may attempt to
improve in future work. Copies of assessment slips are available on Vula.

NOTE
Failure to hand in reports on time will result in a student being penalised 10% per day
which could jeopardise the granting of a D P certificate.

The primary purpose of the practical reports is to communicate your experimental results
and your analysis of them to your instructors. The second purpose is to provide training in
effective written communication of technical information. Since report writing is a vital part
of scientific effort, it is important that students gain experience and obtain feedback on this
writing (see instructions below).

Instructions for the writing and layout of reports

Presentation of your practical report is an extremely important aspect, since it is this

document that is used to evaluate your performance. It is obvious then that you should
pay careful attention to its preparation.

Questions and assignments given in the manual must be answered; these are often a
guide to discussion of results.

Flow diagrams must be submitted with reports as they will be marked.

Labelled samples of compounds prepared must be handed in at the end of the practical
session Samples will be checked and students handing in samples which are not
authentic will be deemed to have committed fraud. This will be dealt with in terms of the
standing rules at UCT.

Templates will be provided for certain practicals and will be submitted instead of a full
report.

The following overall layout is suggested

 8

a. Aim
Clear statement of the objectives to be achieved in this practical.

b. Method
i) A concise and accurate account, in your own words, of your experimental
procedure. Include relevant equations. Note any departures from the
method given in the practical manual. Record any significant experimental
observations.
(ii) Should you perform any additional experiments, briefly describe the overall
method(s) used.

c. Results
Record yields obtained in preparations and any measurements made. Data and
results may be best presented in a table.

d. Calculations
i) Include enough steps in your calculations so that a reader can easily follow
the logic of your analysis.
ii) Use algebraic symbols and units to outline each type of calculation used.
iii) Substitute numbers and complete one sample calculation of each type.
iv) Show how units are derived.
v) Summarise all calculated results in a table.
vi) Include any appropriate plots.

A high mark will be awarded if:

i) Experimental data are well organised and easy to read.
ii) Data are complete and of high quality.
iii) No major errors are present in calculations.
iv) Calculations are presented in the format required and are clear and easily
read.
v) Questions are answered correctly and completely.
vi) Good interpretation of spectral data provided. See appendix for an example
of how to set out the assignment of spectral data.
vii) Evidence of original or creative thought can make up for minor deficiencies
in any of the above areas.

e. Discussion and conclusions

(i) Your experimental results should be evaluated, interpreted and discussed.
Any significant result should be highlighted. An understanding of the
chemistry involved must be shown; this is an important part of the write-up.
Should your results be poor, in your opinion, you should indicate clearly the
reason.
(ii) Included in your discussion should be an assessment of the method used to
achieve your stated aim. Again only brief comments are necessary.
 9

(iii) In conclusion state whether you have achieved your stated aims, and draw
any other relevant conclusions you may feel appropriate.
(iv) Answer any further questions given in the practical.

f. Bibliographic references
The references will be put on Vula. Other relevant books may be found on the
shelves in the library.

How to write a bibliography (list of references)

Note that all references consulted should be listed at the end of the report in the
style used in the Journal of the Chemical Education:

Journals: All authors' names including initials, journal, year, volume, page(s).

Example: Barton, T. J. and Groh, B. L. J. Am. Chem. Soc., 1985, 107, 7221-
7225.

Books: All authors' names including initials, title, publisher, place, year,
page(s).

Example: Greenwood, N. N. and Earnshaw, A. Chemistry of the Elements,

Pergammon Press, Oxford, 1984, pp. 142-146.

NOTE
Rough results must be written in ink and date-stamped ON THE DAY the practical is
performed.

The sheet must include the following:

- Your name
- Your locker no
- Expt no

The data sheet must be handed in with the report. Failure to do so will result in a
deduction of 10%.

No Tippex® is permitted on rough data sheets.

D P REQUIREMENTS

One of the requirements for a D P certificate is the completion of all the practicals and
tutorials (i.e. attending all practicals and handing in all reports). Exemption from a
practical will only be granted on presentation of a VALID medical certificate or a
note from a warden of a residence. Failure to hand in a report will jeopardise the
awarding of a D P certificate.
 10

EXAMINATION

There will be two examinations during the course. The practical course is also treated as
an examination. Consultation with class members is expected and encouraged before
and during the time devoted to laboratory work. AFTER THE EXPERIMENTAL WORK
HAS BEEN COMPLETED, ALL FURTHER PREPARATION (INCLUDING
CALCULATIONS AND ANALYSES) IS TO BE DONE INDIVIDUALLY. Students who
copy reports will be given zero and disciplinary action will be taken.

SAFETY INSTRUCTIONS IN TEACHING LABORATORIES

YOU MUST READ THE FOLLOWING SAFETY INSTRUCTIONS BEFORE STARTING

THE PRACTICAL COURSE.

Chemists’ work, like many other professions, can be dangerous if not carried out properly.
However, the chemical hazard can be minimised, and in most cases eliminated, by taking
a few simple precautions and following a few simple rules, always based on common
sense. No set of safety regulations can cover all the possible situations which can be
potentially dangerous. The instructions given below will help you to carry out your
practical work without endangering yourself and your colleagues. But, apart from these
more detailed instructions, the best advice for safe chemical work is: USE YOUR
COMMON SENSE. If you are not sure, think again. If you are still not sure, NEVER
hesitate to ask your lecturer, supervisor or demonstrator. Now familiarise yourself with the
following safety precautions in your laboratory.

I. GENERAL

1. SAFETY GLASSES MUST BE WORN AT ALL TIMES IN THE LABORATORY.

Safety glasses which will be supplied to all students, must be worn even if students
wear prescription glasses. Failure to comply with this rule will lead to expulsion from
the laboratory. Note: Due to covid-19 regulations you will be issued with a visor
instead of safety glasses and will be required to wear your visor at all times in the
laboratory.

2. Laboratory coats and closed shoes (not sandals) must be worn at all times.
Students will not be permitted to carry out experiments unless they are wearing
personal protective clothing. A limited number of laboratory coats and overshoes
are available for hire from the dispensary.

3. Long hair must be tied back and scarves tucked into laboratory coats.

4. No eating, drinking or smoking is allowed in the laboratory.

5. First-aid boxes, fire extinguishers and safety shower are available in each
laboratory. Acquaint yourself with their location.
 11

6. DO NOT LEAVE AN EXPERIMENT UNATTENDED.

7. Report any accident immediately to the lecturer, demonstrator or Scientific Officer

in charge.

8. Broken glassware must be placed in the bins provided. In some cases it may be
possible to repair apparatus; check with the practical supervisor before discarding
broken glassware.

II. USE OF SOLVENTS AND CHEMICALS

1. Replace lids after using a solvent or chemical.

2 Be very careful not to contaminate solvents or chemicals. Clean spatulas and

weighing boats between weighing of chemicals.

3. Do not throw solvents down the sink - use the solvent waste bottles provided in
the waste fumehood.

4. Do not put pipettes into bottles; pour out the required amount into a beaker.

5. Several reagents can be found on the side-shelves, DO NOT waste them or pour
any excess back into the bottle. Ethanol is available at the dispensary as are some
of the solid reagents which have been pre-weighed.

III. TOXICITY OF CHEMICALS

1 Some of the chemicals and solvents that you will be using may be toxic, corrosive
and/or cause chemical burns. They have to be handled with care. All reactions
involving such substances have to be performed in a fume cupboard. Use gloves
when weighing these compounds.

2 When pipetting toxic liquids (e.g. methanol) a pipette filler bulb must be used. It is
necessary to take certain precautions, however, because the bulbs are expensive
and their valves are delicate. The bulb will irreversibly be destroyed if liquid is
allowed to come into contact with the valves. Therefore, LIQUID MUST NEVER
BE ALLOWED TO ENTER A FILLER BULB AND WET A VALVE. Thus a pipette
must NEVER be OVERFILLED. Further, after delivering an aliquot of liquid, the
 12

FILLER BULB MUST BE REMOVED before the pipette is laid horizontally on the
bench.

3 Try not to allow any chemical to come into contact with your skin.

4 Protect yourself and your colleagues. NEVER point a test tube of boiling liquid at
your neighbour or at your face. NEVER keep it stationary in the flame - it may
bump and the contents shoot out. Sway it slowly from side to side over the flame.

5 If you get corrosive or poisonous chemicals on your skin or in your eyes, wash this
area immediately with large quantities of water, while you call for a demonstrator or
Scientific Officer to assist with the first aid treatment.

6 NEVER dispose of any chemicals in a sink.

IV. WASTE DISPOSAL

1 Organic solvents must be discarded into the residue bottles provided. DO NOT
MIX CHLORINATED SOLVENTS WITH OTHER ORGANIC SOLVENTS.

2 Mercury residues, including broken, thermometers, must be placed in the residue

bottles provided.

3 Do not mix aqueous and organic wastes.

4 Consult your demonstrator or Scientific Officer if you are not sure of the waste
disposal procedure for a particular chemical or solution.

V. FIRE

1. Most organic substances are inflammable; but organic solvents are especially
dangerous. Diethyl ether, petroleum ether, and benzene introduce the
greatest fire hazard due to their low flash points. In the event of a fire – do
not panic. Call your demonstrator immediately!

2. Bunsen burners (and any other open flame) can be used only after making sure
that no flammable solvents are in the vicinity.
 13

3. Ether extractions should be carried out in a fume cupboard.

4. Recrystallisation from an organic solvent must be carried out carefully. Heat must
be applied from a steam bath or from an electrically-heated hotplate

5. Sodium residues, even very small fragments, must be dissolved VERY

CAREFULLY in absolute alcohol before discarding.

VI. BURNS

The best first aid treatment for heat burns is to immediately immerse the burned
area in cool water and KEEP it in the water or under running cold water for 10-15
minutes. Do not smear grease or oily substances on the burned area. Ask the
demonstrator or another student to inform the Scientific Officer or the
lecturer in charge about the burn as Burnshield is available in the dispensary.