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Isolation and Purification of Organic Compounds

The document discusses various methods for the purification of organic compounds, including sublimation, crystallization, distillation, and chromatography. Each method is explained in terms of its principles and applications, such as separating compounds based on boiling points or solubility. Additionally, it highlights the importance of checking purity through melting and boiling points.

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danieltofunmi24
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66 views31 pages

Isolation and Purification of Organic Compounds

The document discusses various methods for the purification of organic compounds, including sublimation, crystallization, distillation, and chromatography. Each method is explained in terms of its principles and applications, such as separating compounds based on boiling points or solubility. Additionally, it highlights the importance of checking purity through melting and boiling points.

Uploaded by

danieltofunmi24
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Download as PDF, TXT or read online on Scribd
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The purification of organic compounds is necessary, after its

extraction from a natural source or synthesis in the


laboratory, though complex. The method of purification of
the organic compound depends mainly on the nature of the
compound and the impurities present.
Table of Content
Sublimation
Crystallisation
Distillation
Fractional Distillation
Vacuum Distillation
Steam Distillation
Differential Extraction
Chromatography
Melting and Boiling Points
One easy method to check the purity of an organic
compound is to either melt or boil it. Organic
compounds tend to have sharp melting and boiling
points.
Purification means the removal of unwanted impurities
present in an organic compound.
SUBLIMATION
• It involves the direct conversion of a solid into the gaseous
state oh healing without passing through the intervening
liquid state and vice versa on cooling

• It is helpful in separating sublimable compounds from non-


sublimable ones.

• Camphor, naphthalene, iodine, anthracene, benzoic acid, are


examples of such compounds that can be separated by
sublimation.
The substance is heated in a china dish above which an inverted funnel is
kept to collect the sublimable compounds. The funnel is kept cool so as to
hasten the process. Vapours of the substance solidify on the funnel.
CRYSTALLISATION
For example, crystals of benzoic acid can be crystallised with
water. Benzoic acid is sparingly soluble in cold water and
soluble in hot water.
DISTILLATION

The underlying principle behind distillation is that the mixture of


liquids can be separated by the difference in their boiling points.
The boiling point is defined as that temperature at which the
vapour pressure of the liquid is equal to the atmospheric
pressure. This method separates volatile liquids from non-volatile
liquids. The setup is given below.
SIMPLE DISTILLATION
FRACTIONAL DISTILLATION

This method is employed when the difference between the


boiling points of the liquids isn’t much. Since the vapours of such
liquids might condense together, a fractionating column is fixed
to the mouth of the RB.
FRACTIONAL DISTILLATION
VACUUM DISTILLATION
Since the boiling point is dependent on the atmospheric pressure,
the liquids will boil at a temperature lesser than their boiling
points if they were distilled in an atmosphere having lower
pressure. This is achieved by using a vacuum pump. Since the
atmospheric pressure is reduced, the liquids also boil faster and
hence the whole process of distillation is made fast.
VACUUM DISTILLATION
STEAM DISTILLATION
In this variant, steam is passed into the flask containing the
liquids to be separated. The principle here is that the liquids
will boil faster because of aqueous tension (vapour pressure of
water) helps in equalising the atmospheric pressure.

Total pressure = Aqueous tension + vapour pressure of liquid


components
STEAM DISTILLATION

In the absence of aqueous tension, the process of boiling would have been continued
until it equalises the atmospheric pressure. Now with the addition of steam, that
process is expedited.
DIFFERENTIAL EXTRACTION
This method is used for immiscible liquids, that is, liquids that do
not mix together. For example, oil and water are immiscible.

The immiscible liquids are taken in a separating funnel and left


undisturbed. After a while, they separate out according to their
specific gravities, with the heavier liquid at the bottom. Then
they are later collected.
DIFFERENTIAL EXTRACTION
CHROMATOGRAPHY
Chromatography is of two types:

• Adsorption Chromatography
• Partition Chromatography
Adsorption Chromatography
It is based on the principle that the constituents are adsorbed on an
adsorbent in varying degrees. The adsorbents used are generally silica gel
or alumina. When a mobile phase moves over the fixed phase, different
constituents of the mixture get adsorbed at various distances over the fixed
phase.
Adsorption Chromatography is further classified into:
• Column Chromatography
• Thin Layer Chromatography
Column Chromatography
Here, a mixture is separated over a column of either silica gel or
alumina, packed in a glass column. The constituent with the most
affinity with the fixed phase is adsorbed at the top, and so on. It
is then retrieved by using an eluant. The solvent is then
evaporated to get the constituent.
Thin Layer Chromatography TLC
Here a sheet of alumina is taken ( 0.2 mm thick) over which a small
spot of the mixture is placed and it is kept in a suitable solvent. The
solvent rises due to capillary action and the constituents also rise
with the solvent depending on their differential adsorption, and
thereby, they are separated.

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