ANALYTICAL

CHEMISTRY
(Seperation and Purification
Techniques)
Dr.S.SURESH
Assistant Professor
Email:avitsureshindia@gm
ail.com

Purification of solid organic compounds

Purification
of
organic
compounds is important because,
organic compound made in the
laboratory contains impurities.
The
common
methods
for
purification are crystallisation,
sublimation,
distillation,
chromatography, etc.

Crystallization
Crystallization is the process of forming crystals
Crystallization by Cooling a Hot Concentrated Solution
In this method the impure substance is dissolved in water or
some other suitable organic solvent such as alcohol, petrol, etc.,
The solution is filtered to remove any suspended impurities. The
filtrate is heated over a water bath so that the vapors of the
solvent may not catch fire.
Then the hot solution of the organic compound is cooled, so that
the crystals begin to separate out.
The crystals are removed by filtration and the impurities are
passed on to the filtrate.

Crystallization by Cooling a Hot

Concentrated Solution

Recrystallisation
Recrystallisation: It is a method used
to purify an organic solid.
A small amount of the solvent is
added to a flask containing an impure
solid. The contents of the flask are
heated until the solid dissolves. Then
the solution is cooled. A more pure
solid
separates
out,
leaving
impurities dissolved in the solvent.

Example for recrystallisation:

1.0 g of crude benzoic acid is taken in a 50 ml flask.
Add a little water and boil
Some contaminants will not dissolve
Transfer to a conical flask and cool
Filter the crystals and allow to dry for 5-10 mins

Impure benzoic
acid

Benzoic acid after

recrystallisation

Drying agents
A drying agent is an inorganic salt which readily takes
up water to become hydrated.
Example: LiAlH4, CaCl2, CaSO4, K2CO3, Na2SO4
LiAlH4 : It reacts violently with water
liberating hydrogen and is a powerful
drying agent for organic compounds. It is
widely used for drying ethers. It finds
extensive application in purifying organic
chemical substances by the removal of
water and carbonyl containing impurities.

Use of drying agents and their

properties
S.N
o

Drying
agent

Properties

Uses

Neutral

Good preliminary drying agent.

It has large water absorption
capacity giving the hexahydrate.

Neutral

It has large water absorption

capacity for the absorption of
water forming the decahydrate.

CaCl2

Sodium
sulphate

Barium oxide

Basic

Suitable for drying organic

bases

Sulphuric
acid

Acidic

It is suitable for drying bromine,

saturated hydrocarbons, etc.,

Sublimation
Sublimation is the direct change of
a solid to vapour on heating
without going through the liquid state
Used to separate volatile organic
compounds
from
non
volatile
impurities
e.g.
Naphthalene,
benzoic acid, anthracene, camphor.

Sublimation
The substances that sublime can be purified by
this method, provided the impurities present
does not sublime.
Many organic compounds directly form
vapours, when solid compounds are heated,
without becoming a liquid at any stage. On
cooling the vapours the solid is directly
obtained.

Sublimation

A mixture of two compounds can be

separated by sublimation

Purification of Liquid organic

compounds
Organic compounds in the liquid state are purified by
distillation.
Distillation involves the heating of a liquid to boiling
and then collecting their vapours to condense them in
liquid state.

Simple Distillation
Simple distillation is designed to evaporate a volatile
liquid from a solution of non-volatile substances; the
vapor is then condensed in the water condenser and
collected in the receiver.

 2-Fractional Distillation
If the boiling point of the liquids in the mixture are very
close to each other then such mixtures can be purified
by fractional distillation. The difference in boiling points
of the mixture is usually less than 40C.
e.g. acetone(b.p. 56C)and methyl alcohol(b.p. 65C).
For fractional distillation, a suitable fractionating column
is placed between the flask and the condenser.

Fractional distillation

Distillation under reduced

Pressure (or) Vaccum
distillation

Vacuum distillation- It is used for

organic compounds which decompose
at or below their boiling points.
Example: Glycerol
The boiling point of a liquid is the
temperature at which the total
vapour pressure is equal to the
external pressure. This means that by
lowering the pressure the boiling
point of the liquid can be lowered.

Vaccum distillation
If we have an organic substance
which decompose at its boiling
point, we can make it to boil at a
temperature lower than its boiling
point. All that we have to do is to
create a partial vaccum. Under
reduced pressure, the substance
boils at a much lower temperature
and distils over undecomposed.

Distillation under reduced pressure

Extraction
Extraction is a very common laboratory procedure
used when isolating or purifying a product
In organic laboratory, liquid-liquid extraction is most
commonly used. Liquid-liquid extraction requires two
immiscible liquids known as the organic phase and the
aqueous phase. The aqueous phase is water-based
and the organic phase is an organic solvent.

General extraction procedure

Place the solution to be extracted in the separatory funnel.
As the organic solvent and water are not miscible with
each other, you should be able to see the two layers
(organic and aqueous layers) clearly.
Now, shake the separatory funnel to increase the contact
between these substances and the water. When
finished, the funnel can be returned to
the stand and the layers are allowed to
separate.
You should also have two beakers ready, one labelled
"organic layer" and the other labelled "aqueous layer".

Solvent Extraction
Extraction with solvents is used as
a method of separation of dissolved
substances from solutions.
The common solvent which is used for the
extraction are diethyl ether, benzene, etc.,
A good solvent for extraction should satisfy two
important conditions.
(a) The substance to be extracted should be highly
soluble in the solvent.
(b) After the extraction the solvent should be easily
separable from the solute.

Solvent Extraction
The mixture of urea and benzoic acid can be separated
using solvent extraction process.
The mixtures are taken in a separating funnel, to the
substances(Urea and benzoic acid) which is solid,
diethyl ether is added.
The two mixtures are shaken well to get a solution.
Only benzoic acid is soluble in ether, while urea is not.
Urea is at the bottom of the separating funnel, and it is
collected.
Now the benzoic acid in ether is left, which on heating,
we get benzoic acid.

Solvent Extraction

Criteria and test for purity

The following physical properties are used for
checking the purity of substances
(a) Melting point
(b) Boiling point
(d) Density
These properties have long been utilized in
identification and characterisation of organic
compounds

Melting Point Apparatus

Criteria and test for purity

Melting point: The melting point of a pure
substance is a constant. The presence of
impurities in a substance lowers the
melting point and hence if the melting
point of a substance is correct then the
substance is taken as pure
Boiling Point: The boiling point of a pure
substance under a particular pressure is a
constant and therefore this property can
be used to check the purity of a liquid.

Criteria for purity

The purity of an organic compound can
be checked by the following criteria:
(a) Sharp melting point which does not
change on further purification.
(b) In case of solids, mix the solid with
known sample of pure compound and
its melting point is noted. The m.pt
should remain the same.
(c) Concordant boiling point
(d) Definite crystalline shape.