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• Is a highly effective method for the purification of organic

substances, provided that the physical properties of a given


compound permits its purification in this manner.
• It involves the process of dissolving the material to form a
saturated solution in a suitable solvent at an elevated
temperature, filtering while hot to remove any suspended
insoluble particles, and letting crystallization proceed.
DESIRABLE SOLVENT FOR CRYSTALLIZATION
1.) dissolves the solute readily at an elevated temperature,
but only sparingly at a lower temperature (room
temperature)
2.) gives no chemical reaction with the solute
3.) sufficiently volatile so that it maybe removed easily from
the purified crystals
3 Consecutive Stages of Crystallization:
1.) removal of impurities
2.) nucleus formation
3.) encouragement of growth of crystals to visible form.

The Factors that affects removal of impurities

1.) Solubility
2.) Volatility difference
2 KINDS OF NUCLEUS FORMATION:
1.) Spontaneous/indirect nucleus formation- usually at the
vicinity of the freezing point of the compound.
- it is caused by the orientation and aggregation of
sufficient number of molecules which may give rise to a
crystal nucleus.
2.) Induce nucleus formation “seeding” – can be induced by
scratching the sides or bottom of the container with a
glass rod.
Growth of the crystals may be encouraged by stirring
or agitation.
In supersaturated solutions, growth of crystals may
be inhibited as a result of restricted motion of molecules.
In this case, crystallization is effected by seeding or by
scratching the sides of the vessel with a glass rod.

Animal Charcoal- the fine carbon particles present a


large, active surface upon which soluble colored
substances may be absorbed, particularly the polymeric,
resinous and reactive by-products.
Less effective at a high than at low temperature.
The direct conversion of a substance from solid to
gas without passing through the liquid state.
It can be applied when the components of a solid
mixture differ appreciably in their vapor pressure.
It involves gentle heating of the mixture is a confined
container until particles of the solid escape into the vapor
phase. When the vapors are condensed on a solid
surface, crystals of the component with high vapor
pressure can be collected, with the component of lower
vapor pressure left in the container.
It depends on differences in volatility, in cases when
the impurities can be volatilized. Less volatile or non-
volatile impurities will remain as residue while the
sublimate is being formed.
Although it is more convenient to apply and requires
less time, its applicability is limited. It cannot be used for
separation of compounds having similar vapor pressures.

This is a picture of
dry ice (frozen CO2)
sublimating.
A frequently used method of withdrawing or
separating a substance from a mixture by the use of
solvents.
The mixture is dissolved in one of two immiscible
solvents and then shaken with other to distribute the
components in each of the 2 solvents will be in direct
proportion to their relative solubilities in each of them.
Water is usually one of the solvents used in an
extraction process, and the other solvent is usually an
organic liquid of a non-polar character.
• Diethyl ether, one of the most important organic
solvents, is used extensively as an extracting solvent.
• It has a high solvent power.
• It is highly volatile (b.p. 34.60) that it is easily removed
from an extract at a low temperature, that even sensitive
compounds are not liable to decompose.
• Ether is slightly soluble in water.
• Its efficiently in use can be improved considerably by the
addition of a small amount of ionizable salt.
• The increase in polar property of the water solution will
cause a decrease in the solubility of the non-polar
compound.
• This reduced solubility of the organic compounds in
water in the presence of an electrolyte (salting-out effect)
• In the presence of an electrolyte is referred to as “salting-
out effect”.
Extraction with water-immiscible solvents is useful
for isolation of natural products that occur in animal and
plant tissues having high water content.
In the soxhlet extractor, solvent vapor rises in the
tube and condensed solvent drops into the solid, leaches
out soluble material and carries it to the boiling flask,
where non-volatile extracted material accumulates.

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