Recrystallization: Experiment

Experiment 2
RECRYSTALLIZATION
Solid organic compounds when isolated from organic reactions
are usually impure; they are usually contaminated with small
amounts of other compounds that are produced along with the
desired compound. The purification of impure crystalline
compounds is usually done by recrystallization from a suitable
solvent or a mixture of solvents.
Liquids are customarily purified by distillation , while solids are
purified by recrystallization (sometimes called simply
crystallization). Insoluble impurities and colored impurities can
be removed from hot solvent through the us of activated carbon
and filtration .
Choosing a solvent for recrystallization:
The proper choice of a solvent is an important part of the art
of crystallization. The ideal solvent should:
1.Be chemically inert toward the solute.
2.Dissolve the solute readily at its boiling point but
sparingly at low temperatures (0 – 25 0C).
3.Dissolve impurities either very easily or not at all.
4.Be highly volatile so that it can readily be evaporated
from the crystals.
5.Not be flammable, of low cost, and of low toxicity.

Practically, to choose a good solvent take about (0.1 gm) of the
compound to be purified (a pure sample) and try to dissolve it in (1
ml) of the solvent;
1- if it dissolves in the cold solvent, the solvent will not be good
for recrystallization
2- if it dissolves in the solvent with heating, the solvent will be
good for recrystallization
3- if it does not dissolve in the solvent even with heating, the
solvent will not be good for recrystallization.
Solvents extensively used for recrystallization include water,
ethanol, chloroform, ether, acetone, and benzene.
Decolorizing charcoal:
Frequently, samples to be purified may contain soluble colored
impurities that may cause the solution and the crystals to be
colored when they should be colorless; they dissolve in the
boiling solvent and are adsorbed on the crystals produced upon
cooling.
These impurities can be removed by treating the colored sample
with decolorizing (activated) charcoal that is composed of fine
carbon particles with a large active surface on which the colored
impurities will be adsorbed.
Charcoal is added to the hot solution before boiling and the
solution is kept hot at or near the boiling point for about 3-5
minutes with shaking to wet the charcoal. The solution is then
filtered through a fluted filter paper. No more charcoal than
actually needed should be used because any excess amount will
cause the desired compound to be adsorbed on the charcoal.
Charcoal is not added at the boiling point of the solvent because
its particles function as thousands of boiling chips causing the
solution to boil over and foam.

Recrystallization using mixed solvents:
This is applied when your compound is readily soluble in a
solvent at room temperature, and at the same time is not soluble in
another solvent. The two solvents must be completely miscible
with each other such as alcohol and water, ether and pentane, and
glacial acetic acid and water. So the compound is dissolved in the
solvent that it is soluble in, charcoal is used if required, and the
solution is filtered to get rid of the insoluble impurities. Then the
over solvent (in which the compound is insoluble) is added to the
filtrate gradually until turbidity appears. The mixture is then left
aside to facilitate crystallization.

Notes:
1- If crystallization does not take place scratch the sides or the bottom of the
container below the surface of the solution with in glass rod, add a small crystal of the
pure compound, or evaporate some of solvent to induce the crystallization process.

2- The funnel, filter paper, and the container of the solution should be kept hot
through out the filtration process to prevent the deposition of the crystals on the filter
paper or on the neck of funnel. Therefore, it is recommended to wash the filter paper
after completing the filtration process with a small amount of the hot solvent.

3- Use a minimum volume of the solvent to prevent the loss of the compound because
large volumes of the solvent will keep most of the compound dissolved in it.

Recrystallization: Experiment

Uploaded by

Copyright:

Available Formats

Recrystallization: Experiment

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Recrystallization: Experiment

Uploaded by

Copyright:

Available Formats

Experiment 2

You might also like