Laboratory rules

These rules will be strictly enforced. Non-compliance may result in disciplinary

action.

1. Closed in, non-slip footwear must be worn in the laboratory at all times.
Students with bare feet, thongs, or open-toed shoes will be ejected from the
laboratory.

2. Properly fastened laboratory lab coats must be worn in all laboratories where
chemicals, radioactive substances and biohazardous substances are being used,
or if directed to do so by the academic in charge of a class.

3. No horseplay or running is permitted in the laboratories.

4. Under no circumstances are unauthorized experiments to be conducted in the

laboratories.

5. No smoking, drinking, eating, handling of food or application of cosmetics is

permitted in the laboratories.

6. Safety glasses must be worn at all times.

7. No mouth pipetting is permitted at ANY time.

8. Disposable gloves must be worn when handling toxic and radioactive

substances, or if your hands contain open wounds.

9. No unauthorized human venepuncture is to be performed by an undergraduate

student.

10. Sitting on laboratory benches is not permitted.

11. ALWAYS WASH YOUR HANDS BEFORE LEAVING THE

LABORATORY.

12. All safety instructions given by the academic in charge of a class must be
followed.

General Safety Information

• When in the laboratory, never adopt a casual attitude – always be conscious of

potential hazards.

• Always take note of instructions given by your academics, demonstrators or

by laboratory staff.

• Never drink from laboratory taps.

 • Regard all substances as hazardous unless there is definite information to the
contrary.

• Report all accidents – no matter how slight – to a demonstrator or laboratory

staff.

• Familiarize with the locations of all fire exits and with the safety facilities
available in the laboratory:
o There are first-aid kits available in each laboratory and emergency eye-
wash bottles located above or on each sinks.
o Emergency gas cut-off switches are located near the main entrances in
each laboratory.

• If you notice any faults with any equipments, or a hazardous situation in the
laboratory, please report it immediately to a demonstrator or laboratory staff.

• On completion of your practical session you are required to ensure that your
work areas are left clean and tidy. If biohazardous materials have been used
the benches must be wiped down with disinfectant.

• Do not attempt to adjust the instrumentation or microscopic light sources if

you are not familiar with them. Always ask the laboratory staff for assistance.

• All dirty glassware (including test tubes) is to be RINSED and placed in the
tubs provided. See special instructions for biohazardous material.

• All dirty graduated and volumetric pipettes are to be placed TIPS DOWN in
the buckets provided. See special instructions for biohazardous material.

• All Pasteur pipettes are disposable and should be placed in the specially
labeled ‘GLASS ONLY’ bins located in the laboratory. See special
instructions for biohazardous material.

Waste disposal

General: paper, plastic and non contaminated material etc, can be placed in the plastic
lined garbage bins.

Glass: broken glassware, uncontaminated Pasteur pipettesand serology tubes, etc, are
to be disposed of in the ‘Glass Only’ bins located in each laboratory. A dustpan and
broom is located next to the glass bins for cleaning up broken glass. Under NO
circumstances should broken glass be picked up with your hands.

Hazardous chemicals: Waste bottles are placed in the fume hoods for organic, heavy
metal and other wastes that are not to be disposed down the sink. If you are not sure,
ask a demonstrator or the laboratory staff.
Radioactive waste: use in designated areas only and follow instructions given.
Immediately report all spills and contaminations to a demonstrator or the laboratory
staff. Dispose of wastes in appropriate vessels in your work area. If you have ANY
doubts, always ask a demonstrator or the laboratory staff.
Preliminary reading and activity

Before commencing practical work, the following must be studied carefully.

The terms ‘Accurately weigh about…’ and ‘Accurately weigh say 0.2-0.3g…’ are
frequently encountered. What do these terms mean and what apparatus should be used
in complying with them?
_____________________________________________________________________
_____________________________________________________________________
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_________

Explain how a solid and a solution can be quantitatively transferred from one
container to another.
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1. DRYING AND STORAGE OF SAMPLES

The need for drying of samples, primary standards (and in some cases the weighing
vessel) must be considered. It is usually achieved by heating in an air oven at 105ºC-
110ºC for 1 hour, removing the object from the oven, cooling to room temperature in
a controlled atmosphere and weighing. The heating, cooling, weighing process is
repeated until constant weight is achieved and hence the term ‘dry to constant
weight’. Obviously, the variation in mass permissible for the object to be considered
at constant weight will depend on the circumstances.

For example, let us consider the following two situations.

i. Drying to constant weight a sample of mass10.000g, and

ii. Drying to constant weight a sample of mass 100mg.

What is the allowable variation in consecutive mass readings before these can be
considered at ‘constant weight’?

We stated above that the object was cooled in a controlled atmosphere with no
indications as to how this was to be achieved. The usual approach to this is to use a
dessicator containing a drying agent or dessicant. Typical dessicants in order of
effectiveness are granular calcium chloride, silica gel, porous calcium sulphate
(Drierite) and anhydrous magnesium perchlorate (Dehydrite). Note that the dessicant
requires periodical changing.
2. CLEANINGOF APPARATUS

It is your responsibility to ensure that the apparatus you use is clean and fit for
purpose.

What is clean depends on the circumstances. For example, the presence of phosphate
in glassware (from detergents) will interfere in the determination of phosphate in a
sample but not interfere in the determination of copper in the same sample. Again,
how the cleaning is achieved will depend on the circumstances. For example, less
stringent cleaning will be required for the analysis of copper in a sample containing of
the order of 30% copper than the analysis of copper at the ppb level.

Thorough rinsing with tap water followed by rinsing with small successive portions of
distilled water generally will be sufficient to ensure cleanliness of your apparatus.
This will not always be the case, however, (eg. Determination of sodium at the trace
level) and you should give this matter some thought whenever commencing analysis.
If in any doubt, consult the laboratory staff.

3. USE OF VOLUMETRIC APPARATUS

A pipette or burette must be used in the same way that it was calibrated; ie. The
matter of delivery must be the same, the same period of drainage and the same
temperature used. When liquids other than water are pipetted, the volumes of liquid
delivered may be considerably different from the volume found in calibration, owing
to differences in viscosity, density, and surface tension. With dilute (1M) aqueous
solutions of salts, acids, and bases, the differences are so small that it may be
disregarded.

Volumetric flasks are used in the dilution of solutions and in the preparation of
standard solutions. This will involve weighing the sample (analytical balance),
quantitative transfer of the weighed sample to a beaker followed by dissolution of the
sample.

The resulting solution is transferred quantitatively to the volumetric flask and diluted
until the level of the solution has risen nearly to the neck of the flask. The flask is now
swirled to ensure mixing. The final adjustment to the mark is made by adding liquid
(often distilled water) dropwise from a pipette. Time must be allowed for the liquid to
drain down the sides of the neck if the latter has been wetted. Finally, the clean, dry
stopper is inserted and the solution mixed thoroughly by inverting the flask several
times with a simultaneously rotary motion. If the solution is not to be used
immediately, it must be transferred to a clean flask which has been with 3 or 4
aliquots of the solution. The temperature of the solution must be noted and recorded.
4. WEIGHING ERRORS

On the basis of origin, weighing errors may be classified as:

i. Due to the balance and weights.

• Inherent errors due to factors such as imperfections in knife edges and
corroded weights,
• Environmental factors such as temperature changes, vibration, and
gathering of dust may cause weighing errors;

ii. Due to changes in condition of the weighing vessel, the substance weighed or
the atmosphere.
• Absorption of water by either the weighing vessel or the sample will
cause errors,
• Electrification of glass containers, especially in a low humidity
atmosphere, may have to be guarded against. A buildup for static
electricity on the weighing vessel will produce an erroneous weight on
account of the attraction of the charged container for the walls or the
floors of the balance,
• Differences in temperature of the sample /weighing vessel and the
balance may cause serious errors. Thus the apparent weight of an
object warmer than the balance will be less than the true weight
because the rising convection currents will buoy it up. Moreover, if the
warm body is hollow (eg. A covered crucible) the air within will be
less dense than the air in the balance case, and the buoyancy will result
in a negative error. For example, a 25ml covered crucible at 1ºC above
the balance case temperature will weigh 0.1mg less than when at the
same temperature. If the subject is colder than the balance, it will
appear to be heavier.
• Where temperature is no problem, then the errors due to the buoyancy
of air are usually insignificant. (See, for example, Quantitative
Chemical Analysis by LM. Kolthoff, E.B. Sandell, et al. the Macmillan
Co. London, 1969, p. 496);

iii. Due to the analyst as a result of carelessness.

5. PRACTICAL REPORTS AN ASSESSMENT OF PRACTICAL WORK

In doing the practical work and preparing your reports, you should pay particular
attention to the following:
• Correct storage of sample/standards
• Cleanliness of apparatus
• Quote the correct units with your results
• Quote the final answer for the concentration of a component in the original
sample and not in some diluted aliquot
• All quantitative results must be accompanied by an associated error, i.e. mean
± error estimate
• Recording of all raw data must be done in laboratory workbook. Please bring a
suitable book to the residential school.