BIOM1007 – Chemistry for the Biosciences 2020-

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Practical 1 – Separation and Purification

Method Notes

Vacuum filtration
1. Uses a Buchner (or Hirsch) funnel with filter paper placed into the funnel.
2. Buchner funnel is placed onto a specialised flask with a vacuum inlet using a rubber
ring.
3. The conical flask must be supported with a retort stand and clamp to prevent tipping
and loss of sample.
4. A vacuum line is connected to the buchner flask
Note – before you begin filtering any samples, add solvent to the filter paper so it
“sticks” to the buchner funnel. Start the vacuum and then pour your sample into the
funnel.

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Recrystallisation
1. Helps purification of a compound of interest as the recrystallisation process excludes
contaminants from the formation of the crystal lattice of the required compound.
2. he contaminants usually remain within the solvent used and can be disposed.
3. The compound to be purified is dissolved in a minimum amount of hot solvent
(solvent to be used depends on the chemical being recrystallised) and then the
mixture is allowed to cool to room temperature before placing in an ice bath.
4. The crystallisation process is aided by low temperature and high concentration of
solute hence uses minimal volumes of solvent.
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Vacuum drying oven

This device works, as the name suggests, by applying a vacuum to a heated chamber (oven)
that enables samples to be dried. The vacuum lowers the vapour pressure facilitating
evaporation of a solvent, whether that be water or another solvent.

Melting point determination

1. Aids in the identification of a compound with or without standards.
2. Melting point apparatus is provided in the laboratory and instructions on use are
noted on the instrument and on accompanying instruction cards.
3. Thin walled capillary tubes are used which are usually sealed at both ends. These
should be carefully broken (in a piece of tissue) in the middle before use – be careful
not to penetrate your skin with sharp pieces of glass.
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4. To fill the capillary tubes, the test compound needs to be powdered or in a very fine
granular form. Dip the open end of the capillary in the powder and tap sealed end on
the bench carefully to get the powder into the bottom of the tube. Repeat as
necessary and only a couple of millimetres of test compound are needed in the tube
to perform the test.
5. Once the plateau temperature is reached careful observation of the material in the
tube is needed. It may help to rotate the capillary tube to help see what is
happening. Record the temperature at which the compound begins to melt and then
again when melted. Melting temperature should be recorded over a span of three
degrees e.g. if your compound begins melting at 125 °C and is completely melted at
127 °C, then you would report the range as 125-127 °C or 126±1 °C.

Thin walled capillary tubes

Melting point apparatus