Recrystallization
The technique is a physical process. Used to purify solids based on their
different solubility, in this technique, an impure solid compound is dissolved in
a solvent and then allowed to crystallize out as the solution cools slowly. As the
compound crystallizes from the solution, the molecules of the other compounds
dissolved in solution are excluded from the growing crystal lattice, of a pure
solid. There are two types of impurities: those more soluble in a given solvent
than the main component and those less soluble. (If there are any impurities that
have the same solubility as the main component, then a different solvent needs
to be chosen.)
A suitable recrystallization solvent should also be partially volatile to easily
remove from the purified crystals. The solvent should not react with the
compound being purified and it should have a boiling point below the melting
point of the compound being purified because the solid melts before dissolves
(oiling out). In selecting a good recrystallization solvent one should also
consider flammability, toxicity, and expense. In selecting a solvent consider that
like likes like. Polar compounds dissolve polar compounds and non-polar
compounds dissolve non polar compounds. The most commonly used
recrystallization solvents are presented in the following table.
The steps in the recrystallization of a compound are:
1- Find a suitable solvent for the recrystallization.
2- Dissolve the impure solid in a minimum volume of hot solvent.
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3- Remove any insoluble impurities by filtration.
4- Slowly cool the hot solution to crystallize the desired compound.
5- Filter the solution to isolate the purified solid compound.
Note :-Crystallization of a solid is not the same as precipitation of a solid. In
crystallization, there is a slow, selective formation of the crystal framework
resulting in a pure compound. In precipitation, there is a rapid formation of a
solid from a solution that usually produces an amorphous solid containing many
trapped impurities within the solid's crystal framework. For this reason,
experimental procedures that produce a solid product by precipitation always
include a final recrystallization step to give the pure compound.
Equipment and chemicals :
1- acetanilide or benzoic acid 2-conical flask 250 ml 3- hot plate 4- Stirring rod
5- filter paper 6- small stirring bar 7- funnel 8- 50 mL beaker
Procedure :
1- Boil approximately 200 ml of DI water, slowly add the hot water to ---- grams
of acetanilide or benzoic acid in a 250 ml conical flask with constant stirring
until it is dissolved in the minimum amount of boiling solvent. If needed, place
the flask in a hot water bath to keep the solution hot and prevent
recrystallization.
2- Using a minimum amount of solvent will return a greater yield of acetanilide
or benzoic upon cooling. Also, remember that the solid may dissolve slowly. Do
not add the hot solvent too rapidly.
3- Allow the solution to slowly cool to room temperature. Crystals will begin to
form as the solution cools. It is recommended to leave the solution standing
overnight. If the solvent is volatile, cover it a watch glass. In this experiment, we
will just wait until room temperature.
4- Place the flask into an ice bath and allow cooling.
5- Filter the cold solution by vacuum filtration using aBüchner funnel.
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6-wash the collected crystals with cold solvent.
7- Remove the crystals and allow drying covered with watch glass.
8- Weigh and calculate % yield.
.Recrystallization apparatus
Schematic protocol of drug recrystallization for further purification.
