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PURIFICATION of Organic Compounds

The common techniques used for the purification of a particular compound are based on its nature and also on the nature of the impurities present in
it. The various methods used for this purpose are:
1. Crystallization 2. Sublimation 3. Differential extraction 4. Distillation 5. Fractional distillation 6. Distillation under reduced
pressure 7. Steam distillation 8. Chromatography.
1. Crystallization is a process of solidification of a pure substance from its dissolved state. This is the most common way of purifying organic solids.
This method is based upon differences in their solubility in a given solvent or a mixture of solvents. Solvents such as alcohol, acetone, chloroform,
ether, etc., are also commonly used for this purpose. The process involves the steps given below:
The impure substance is powdered and heated with the solvent. The hot saturated solution prepared is then filtered. The hot filtrate is allowed to cool
slowly and crystallizing. In this way, large and beautiful crystals are obtained. The crystals are separated from the mother liquor by filtration
Selection of the Solvent: A suitable solvent is one in which:
(a) The substance dissolves on heating readily and crystallises out on cooling. (b) The solvent must not react chemically with the substance.
Examples: Ethanol can be used for purification of sugar containing impurities of common salt. Common salt does not dissolve in ethanol. Similarly, a
benzoic acid containing impurities of naphthalene can be purified by using hot water which dissolves only benzoic acid but not naphthalene.
2. SUBLIMATION: Sublimation is a process of conversion of a solid into gaseous state on heating without passing through the intermediate liquid state
and vice versa. This process is used for the separation of volatile solids, which sublime on heating from the non-volatile solids. The impure substance
is heated. The Vapours of the solid, which sublime, pass through condensation on the cooler. The non-volatile impurities are left behind in the dish.
Examples: Iodine, camphor, naphthalene, benzoic acid, etc., are purified by this method.
3. DIFFERENTIAL EXTRACTION: Organic compounds, whether solids or liquids, can be recovered from aqueous solutions by shaking the solution in a
suitable organic solvent which is immiscible with water but in which the organic compound is highly soluble. This process is known as extraction or
solvent extraction. Some commonly employed solvents are, Ether, benzene and chloroform.

The process is carried out as follows: The aqueous solution is mixed with a small quantity of the organic solvent and its contents shaken for some
time. When the organic solvent dissolves out the solute. The mixture is now allowed to settle and in this way solvent and water from two separate
layers. The lower aqueous layer is run out and the solvent layer is collected separately. The whole process may be repeated to remove the solute
completely from the aqueous solution. The solute is finally recovered from the organic solvent by distilling off the latter.

4. DISTILLATION: Distillation is a process of conversion of a liquid into vapours by heating followed by condensation of vapours so produced by
cooling. The method is used for the purification of liquids which boil without decomposition and are associated with non-volatile impurities. The
impure liquid is boiled and the vapours, thus, formed are condensed to get the pure liquid.

This process is used to separate mixture of two or more miscible liquids having different boiling points. It can be carried in two ways as under.
(a) Simple distillation: When the two liquids have their boiling points wide apart, say about 40° or more, the mixture may be separated by using simple
distillation. The more volatile liquid (low b.p.) distils over first and is collected. The less volatile liquid distils over and is collected. The two fractions
thus obtained are redistilled separately, a number of times, to ensure complete purity of the liquids.
(b) Fractionational Distillation
When the boiling points of the two liquids are quite close (difference less than 30°) the separation is effected by fitting the distillation with a
fractionating column. A fractionating column is a long tube provided with obstructions to the passage of the vapours upwards and that to liquid
downwards. On heating the mixture, the vapours obtained consist of more volatile (low b.p) rise up the fractionating column, they condense partially·
and the condensed liquid flows down. This process is repeated throughout the length of fractionating column. Consequently, the vapours which
escape from the top of the column into the condenser consist almost of more volatile component. Whereas the liquid left behind in the flask is very
rich in low volatile component. This process may be repeated to achieve the complete separation of liquids. Fractional distillation has found
remarkable application in modern industry especially in the distillation of petroleum, coaltar and crude alcohol.
Principle: A liquid boils when its vapor pressure becomes equal to the applied pressure or external pressure. If applied pressure is decreased, the
same liquid will now, boil at a lower temperature. Thus, this process is employed if the liquid has a tendency to decompose near its boiling point.
Under reduced pressure, the liquid will boil at a low temperature and the temperature of decomposition will not be reached. Glycerol, for example,
boils with decomposition at 563 K but if the pressure it reduced to 12 mm, it boils at 453 K without decomposition. . The desired pressure is
maintained by vacuum pump.
7. STEAM DISTILLATION: The process of steam distillation is employed in the purification of a substance from non-volatile impurities provided the

substance itself is volatile in steam and insoluble in water. This method is based on the facts that:
(i) A liquid boils at a temperature when its vapor pressure becomes equal to the atmospheric pressure. (ii) The vapor pressure of a mixture of two
immiscible liquids is equal to the sum of the vapor pressures of the individual liquids.
In the actual process, steam is continuously passed through the impure organic liquid. Steam heats the liquid. After some time, the mixture of the
liquid and water begins to boil because the vapor pressure of the mixture becomes equal to the atmospheric pressure. Thus in steam distillation the
liquid gets distilled at a temperature lower than its boiling point and condensed for separation from condensed water. Any chances of decomposition
organic liquids are avoided.
8. CHROMATOGRAPHY: The method is used for the separation of colored substances into individual components. Chromatography in general, may
be described as the technique of separating the constituents of a mixture by the differential movement of individual components through the
stationary phase under the influence of mobile phase. Different types of chromatographic techniques are employed depending upon the nature of
stationary and mobile phases.
(A) Adsorption chromatography: It is based on the principal of differential adsorption of various components of the mixture on a suitable adsorbent.
When the mobile phase is allowed move over the stationary phase (adsorbent), the components of the mixture move by varying distances over the
stationary phase.
(B) Partition chromatography: It is based on the continuous differential partitioning (distribution) components of a mixture between stationary and
mobile phases. The mobile phase is liquid mixture of two or more substances with water as one of the component.