Many solid organic compounds are often contained undesirable impurities. If the compound has solubility considerably different from that of the impurities, crystallization from a soluble solvent (or solvent mixture) provided a useful and simple method of purification. Note that the term crystallization and recrystallization are often use interchangeably by practicing chemist.
Crystallization is a valuable technique because it is one of the methods used for purification of solids. The process of crystallization involves dissolution of the solid in an appropriate solvent at an elevated temperature and the subsequent re-formation of the crystals upon cooling. It means that any impurities are still remains in the solution.
Almost all solids are more soluble in a hot than in a cold solvent, and solution crystallization takes advantage of this fact. Thus, if a solid is first dissolved in an amount of hot solvent insufficient to dissolve it when cold, crystals should form when the hot solution is allowed to cool. Even after a solid has been recrystallized, it may still not be pure. Thus, it is important to determine the purity of the sample, and one of the easiest methods to do this is by determining the melting point of the solid.
Standard crystallization techniques
1. Selection of an appropriate solvent.
2. Dissolution of the solid to be purified in the solvent near or at its boiling point.
3. Decolouration with an activated form of carbon (charcoal), if necessary, to remove colored impurities and filtration of the hot solution to remove insoluble impurities and the decolorizing carbon.
4. Formation of crystalline solid from the solution as it cools.
5. Isolation of the purified solid by filtration.
6. Drying the crystals.
7. Melting point determination.
Solvent selection
The choice of an appropriate solvent for crystallization, polar or non polar solvent, must be basically a trial-and-error process. A crystallization solvent should have a relative low boiling point (e.g. less than 100 C) so it can easily and quickly concentrate and so that the isolated crystals will dry quickly. Because it is often desirable to cool solvent in ice to force more crystals from the solution the freezing point should be < 0 C. Some of more the commonly used crystallization solvent and some of their properties are listed in Table 1. Notice that the listing is in approximate order of decreasing polarity.