Basic laboratory procedures

p26,27:
• Why must the clamp holder be positioned (when clamped to the support stand) that the open
“slot” is pointing upwards?
• Where do you clamp a conical flask and why?
• What is a ground glass joint?
• Why must the clamp be positioned with the movable joint at the top?
• How would you determine which layer in a separating flask is which?

p27:
• Why is the separating funnel (Fig 5.3) not clamped in the middle of the funnel?
• When do you use gravity filtration and why?
• When do you use vacuum filtration and why?
• Why can plastic funnels not be used with organic solvents?
• When is hot filtration used?
• Why can slow filtration lead to disaster with hot filtration?

p28:
• Why is the support stand in Fig 5.4 positioned wrong?
• Why does one used a fluted filter paper?
• Can you use a fluted filter paper with vacuum filtration?

p29:
• When do you use a Buchner funnel and when a Hirsch funnel?
• Why can you not use a Buchner or Hirsch funnel with gravity filtration?
• Why should you not use a sintered glass funnel for removing activated charcoal from a
solution?
• When an organic product in an organic solvent is treated with activated charcoal, what is the
most practical way to filter the solvent? (using a sintered glass funnel – not in text books –
also see p31).
• Why should a Buchner or Hirsch funnel (mostly made of porcelain) not be used for
recovering a solvent?
• What is the principal of a waterjet pump? (not in book). How is the vacuum created?
• Why does one use thick wall tubing for vacuum?
• Can you use any type of Buchner (filter) flask?
• What can go wrong when you are using suction filtration with a hot solution (during
recrystallization)?
• Why does one use a water trap with suction filtration (Fig 5.7)?

p30:
• Why is point 8 required?
• Why is point 12 required?

p31, 32:
• How do propose to clean a sintered glass funnel?
• What is the principal of boiling stones?
• Why can a glass rod be used to avoid pumping?
• Name 3 types of laboratory glass? (not in book).
• Name applications of each type of glass?
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• Which of these types of glass can be heated? Explain why or why not.
• What is a magnetic “flea”?
• What will happen if you add anti-bumping granules to a hot solution?
• When does one use a micro burner?

p33:
• Why should one use medium wall tubing for gas burners?
• What is the difference between a constant temperature (thermostat) bath and a water bath?
• What is the difference between a water bath and a steam bath?
• When will you rather use a water bath?
• When will you use a steam bath?
• Modified steam bath (UKZN model).
• Why are steam burns more extensive than hot water burns? (not in book).
• What are the advantages of using a steam or water bath? Disadvantages?

p34, 35:
• Why should a round bottom flask never be heated on a hot plate?
• What precaution should be taken with water tubing and the electrical cable when you are
using a hot plate?
• Why is an oil bath used in a fume hood?
• Can you use sunflower oil or peanut oil for an oil bath? (not in book)
• During a heating experiment (reflux, distillation etc.) the setup can sometimes over heat.
What precautions should one make to quickly remove the source of heat (hot plate, oil bath,
mantle)? Name two precautions (see p28 and p35).
• What is the ideal level of the liquid in side the reaction flask in terms of the level of liquid in
the oil bath? (not in book). And with a mantle?
• You forgot to put the thermometer (mercury) in the oil bath and the temperature has reached
150 degrees C. What is the danger and how do you overcome that? (hint: the thermometer
is made of soda glass).
• How would you know if the water inlet an outlet to a condenser was connected the wrong
way around?
• What do you do when the thermometer breaks and spill the mercury?

p36
• A heat gun can be used with TLC? explain?

p37, 38
• Why can an ice bath maintain temperatures of say -20 degrees C or lower?
• Why can dry ice mixtures maintain temperatures of down to -100 degrees C?
• What is a potential risk when you want to measure the temperature of a dry ice bath?
• How do you prevent condensation of wet air inside the reaction glassware setup when you
are working in a dry ice bath?

p39
• Two methods to clean glassware for ultra sensitive conditions? (not in book).
• What solids can be dried in an oven?
• Why should organic solids in general not be dried in an oven?
• Can you use a vacuum desiccator with water jet pump to dry a solid?
• When you are using a vacuum desiccator, there is a possibility that the solid shoots up and
spill all over the inside of the desiccator. How is this risk minimized? (not in book).
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• One gets four main types of vacuum pumps: (a) membrane, (b) rotary (oil) (c) dispersion
(oil or mercury) and turbine vacuum pumps. Read up about the principles behind these
pumps and applications for each one.
• How do you prevent your sample from being blown all over the inside of the desiccator
when you want to open the dessicator?
• You have dried a sample over the weekend. On Monday morning the desiccator does not
want to open (the paraffin grease was old and it is very sticky). What do you do (not in
book)? (hint: from what type of glass is the desiccator made of?)
• When you want to switch the rotary (oil) vacuum pump off, what precautions must you take
and why?

p43:
• In organic research (less than 300 mg of starting material) one NEVER uses paraffin grease
(or any other grease). Why not? (not in book)
• Why could “dry” joints be used with distillations or reflux experiments? (not in book).
• Alternative for grease is Teflon socks (see Aldrich catalogue).

p44:
• Where can a joint clip be used with a distillation or setup and why?

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Distillation:

P107, 106:
• What is the difference between a take-off adapter and a distillation adaptor (see p42)?
• What is the purpose of various types of fractional distillation columns?
• When distillation is performed in a fume cupboard, one sometimes observes that the vapour
is not reaching the top of the still head. Name two methods to ensure that the vapour is
distilled over.

p109:
• How could you ensure that the receiver flask and take-off adaptor do not fall off and
break/spill the product?
• Where is the correct position of the thermometer?
• Can you use an oil bath or mantle for heating?
• Why is a thermometer used to measure the temperature of the oil bath (see p35).
• Why should the temperature not vary too much when distilling different fractions off (see
Box 15.2, point 3).
• Why should you NOT use grease for organic synthesis – not in book (see Box 15.1, point 8
and 12)?
• Why is gentle heating required for fractional distillation? (See Box 15.3, point 2, 3, 5 as well
as Key point on p108).
• Why should one not use flat bottom flasks (including conical flasks) for vacuum distillation?
• Why can one use a Buchner flask (flat bottom) for vacuum filtration? (see p29).
• Why should one use an “anti-suck-back” trap with vacuum distillations?
• How would you prevent excessive bumping when you perform vacuum distillation?

p111, 112:
• What is the most crucial point when using an Anshutz manometer?
• What is the most critical point when using a Vacustat® manometer?
• If the mercury spills, how would you suggest to clear the mess up? (not in book).
• You are using an Anshutz manometer with a vacuum distillation. When would you use the
tap on the manometer? (not in book).
• The distillation is completed. How would you ensure that the manometer is not damaged
when the vacuum is broken? (see page 113)
• Why is a three way tap used between the manometer and the vacuum pump?
• When you want to switch the rotary (oil) vacuum pump off, what precautions must you take
and why? (also see p113)
• Name two applications for Kugelrohr distillation (find additional applications)
• How would you ensure that you remove all sample from a specific bulb in a Kugelrohr
apparatus?

p116:
• Why is round bottom flasks and pear shape flasks preferred for distillation and reflux
experiments?
• When would you use a double surface condenser?
• When would you use a normal dropping funnel and when a pressure-equalizing funnel?
• What is the difference between a dropping funnel and a separating funnel?
• When would you use a magnetic stirrer and when would you use a mechanical stirrer?

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