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Practical Organic Chemistry (Poc) : Ones Today Iitians Tomorrow

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8 views33 pages

Practical Organic Chemistry (Poc) : Ones Today Iitians Tomorrow

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manishkumar9112007
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© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Practical Organic Chemistry (POC) 1

Ones Today IITians Tomorrow


METHODS OF PURIFICATION OF ORGANIC COMPOUNDS

The common techniques used for purification are as follows :

(i)Sublimation

(ii) Crystallisation

(iii) Distillation

(iv) Differential extraction and Chromatography


Sublimation
Sublimation

❖ Some solid substances change from solid to vapour state without


passing through liquid state.

❖ The purification technique based on the above principle is known as


sublimation and is used to separate sublimable compounds from
non sublimable impurities.
Crystallisation
Crystallisation

It is based on the difference in the solubilities of the compound and the


impurities in a suitable solvent.

The impure compound is dissolved in a solvent in which it is sparingly


soluble at room temperature but appreciably soluble at higher
temperature. The solution is concentrated to get a nearly saturated
solution.

On cooling the solution, pure compound crystallises out and is removed by


filtration
Distillation
Distillation
This important method is used to separate

(i) Volatile liquids from nonvolatile impurities

(ii) The liquids having sufficient difference in their boiling points.


Distillation

Liquids having different boiling points vaporise at different temperatures.

The vapours are cooled and the liquids so formed are collected separately.

Example:

Chloroform (b.p 334 K) and aniline (b.p. 457 K) are easily separated by the
technique of distillation
Fractional Distillation
Fractional Distillation

❖ Difference in boiling points of two liquids is not much, simple


distillation cannot be used to separate them.

❖ The vapours of such liquids are formed within the same


temperature range and are condensed simultaneously.

❖ this technique, vapours of a liquid mixture are passed through a


fractionating column before condensation.
Fractional Distillation

One of the technological applications of fractional distillation is to


separate different fractions of crude oil in petroleum industry.
Distillation under reduced pressure
Distillation under reduced pressure

➢ This method is used to purify liquids having very high boiling points
and those, which decompose at or below their boiling points.

➢ Such liquids are made to boil at a temperature lower than their


normal boiling points by reducing the pressure on their surface.

➢ Glycerol can be separated from spent-lye in soap industry by using


this technique.
Steam Distillation
Steam Distillation

➢ This technique is applied to separate substances which are steam


volatile and are immiscible with water.

➢ In steam distillation, steam from a steam generator is passed


through a heated flask containing the liquid to be distilled.

➢ The mixture of steam and the volatile organic compound is


condensed and collected. The compound is later separated from
water using a separating funnel.

➢ Aniline is separated by this technique from aniline – water mixture


Differential Extraction
Differential Extraction

When an organic compound is present in an aqueous medium, it is


separated by shaking it with an organic solvent in which it is more
soluble than in water.

The organic solvent and the aqueous solution should be immiscible


with each other so that they form two distinct layers which can be
separated by separatory funnel.

The organic solvent is later removed by distillation or by evaporation


to get back the compound.
Differential Extraction

If the organic compound is less soluble in the organic solvent, a very


large quantity of solvent would be required to extract even a very
small quantity of the compound.

The technique of continuous extraction is employed in such cases. In


this technique same solvent is repeatedly used for extraction of the
compound.
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Chromatography
Chromatography

In this technique, the mixture of substances is applied onto a stationary


phase, which may be a solid or a liquid.

A pure solvent, a mixture of solvents, or a gas is allowed to move slowly


over the stationary phase. The components of the mixture get gradually
separated from one another.

The moving phase is called the mobile phase


Chromatography

Chromatography is classified into different categories.

(a) Adsorption chromatography

(b) Partition chromatography


Adsorption Chromatography

Adsorption chromatography is based on the fact that different compounds


are adsorbed on an adsorbent to different degrees.

Commonly used adsorbents are silica gel and alumina.

When a mobile phase is allowed to move over a stationary phase


(adsorbent), the components of the mixture move by varying distances
over the stationary phase
Adsorption Chromatography

a) Column chromatography

b) Thin layer chromatography


Column Chromatography
Column Chromatography

The mixture adsorbed on adsorbent is placed on the top of the adsorbent


column packed in a glass tube.

An appropriate eluant which is a liquid or a mixture of liquids is allowed to


flow down the column slowly.

Depending upon the degree to which the compounds are adsorbed,


complete separation takes place.

The most readily adsorbed substances are retained near the top and others
come down to various distances in the column

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