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- Chemistry (CH382)
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- The University Of Kent (UKC)
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CH382 Fundamental Laboratory Techniques CH382Technique 6: Separation by Distillation
Surname Xavier Grade
Initials FX Date: 29/10/19 Marker
Safety Data: For the experiment the following chemicals were used listed below are the
hazards:
Hexane – Flammable, environmental hazard, irritant, Health Hazard
Toluene – Flammable, Health hazard, Irritant
The experiment was conducted in a fume cupboard to avoid all risks, no ignition was
required at any stage.
, CH382 Fundamental Laboratory Techniques CH382
Method: For the experiment the liquid mixtures which consists of hexane and toluene
was supplied as a 1:1 mixture by volume of the two components assuming the starting
mixture to have a density of 0.76g ml-1 .
Within the apparatus a 250ml round bottom flask is used and never be more than two
thirds full of the liquid mixture, which also should be pre-charged with about 20ml of
toluene and some anti-bumping granules.
For the distillation transfer 60ml of the liquid mixture to the round bottomed flask using a
measuring cylinder, making sure the apparatus is secure and that all the QuickFit joints
are flush once the transfer is complete. Separate the mixture into two main fractions by
distillation about 20ml for each fraction and an additional intermediate fraction about
10ml. note the volumes of each distilled fraction collected using the graduated test tube.
Discard the first few millimetres of the distillate and thereafter start collecting the first
fraction which will be pure hexane. The thermometer holds a steady reading around the
boiling point of hexane which is set up for a liquid/vapour reflux around the bulb. The
second (intermediate) fraction will be a mixture of hexane and toluene which will distill
over a temperature range around 75 degrees celsius and the final fraction distilled will be
pure toluene. To avoid cracking the glassware do not boil to dryness, at least 5 – 10ml of
solvent should remain in the round bottomed flask.
Purity analysis (Abbe refractometer): the purity of the three distilled fractions can be
obtained by using an Abbe refractometer where the refractive index of each fraction can
be attained and used to compare it with literature values.
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