Crystallization - Purification of organic compounds

Crystallization:

It is the most widely used method for the purification of solid organic compound. This process is carried out in by the follow-ing step

(i) Selection of solvent:

Most of the organic substances being covalent do not dissolve in polar solvents like water, hence selection of solvent (suitable) becomes necessary. Hence the powdered organic substance is taken in a test tube and the solvent is added little by little with constant stirring and heating, till the amount added is just sufficient to dissolve the solute(ie) organic compound. If the solid dissolves upon heating and throws out maximum crystals on cooling, then the solvent is suitable. This process is repeated with other solvents like benzene, ether, acetone and alcohol till the most suitably one is sorted out.

(ii) Preparation of solution:

The organic substance is dissolved in a minimum quantity of suitable solvent. Small amount of animal charcoal can be added to decolorize any colored substance. The heating may be done over a wire gauze or water bath depending upon the nature of liquid (ie) whether the solvent is low boiling or high boiling.

(iii) Filtration of hot solution:

The hot solution so obtained is filtered through a fluted filter paper placed in a funnel.

(iv) Crystallization:

The hot filtrate is then allowed to cool. Most of the impurities are removed on the filter paper, the pure solid substance separate as crystal. When copious amount of crystal has been obtained, then the crystallization is complete. If the rate of crystallization is slow, it is induced either by scratching the walls of the beaker with a glass rod or by adding a few crystals of the pure compounds to the solution.

(v) Isolation and drying of crystals: 

The crystals are separated from the mother liquor by filtration. Filtration is done under reduced pressure using a Bucher funnel. When the whole of the mother liquor has been drained into the filtration flask, the crystals are washed with small quantities of the pure cold solvent and then dried.