Impurities often contaminate organic compounds that have been synthesized in the laboratory or isolated from natural sources. Recrystallization is a purification process used to remove impurities from organic compounds that are solids at room temperature. This process is based on the premise that the solubility of a compound in a solvent increases with temperature. Conversely, the solubility of the compound decreases as the solution cools, and that’s when the crystals are formed.
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.