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INTRODUCTION

The most common method of purifying


solid organic compounds is by
recrystallization. In this technique, an
impure solid compound is dissolved in a
solvent and then allowed to slowly
crystallize out as the solution cools. As the
compound crystallizes from the solution,
the molecules of the other compounds
dissolved in solution are excluded from the
growing crystal lattice, giving a pure solid.

Purpose of process
Mainly for the purification of solid
crystalline compounds.
Melting point is one of the ways of
determining the purity of the
compound.

PRINCIPLES OF
RECRYSTALLLIZATION
Based on the difference between the solubilities of
the pure substance and the impurities in the solvent
or mixture of solvents
2 different situations could arise
Either the impurities have greater solubility in the
solvent than the pure substance being recrystallized
In which case the impurities will be retained in the
mother liquor and several recrystallizations will
yield the pure substance
Or the impurities will have less solubility in the
solvent than the substance being recrystallized in
which case the impurities will not dissolve and more
crystals will be obtained

PRINCIPLES OF
RECYSTALLIZATION
At normal laboratory temperatures
the substance being recrystallized is
not soluble. However ,increasing the
temperature results in increased
solubility of the pure substance
At the boiling point of the pure
substance,maximum solubility is
obtained.

PRINCIPLES OF
RECRYSTALLIZATION

After reaching the boiling


point,reduction of temperature
results in precipitation of crystal
nuclei
Presence of crystal nuclei promotes
crystal growth which continues until
the temperature is stabilized at the
normal laboratory temperature

PRINCIPLES OF
RECRYSTALLIZATION
Assumptions made are;
The impurities are present in
comparatively small quantities ie less
than 5%
The effect of either component (ie
the impurity and the pure substance)
on the solubility of the other is
neglected

PRECAUTIONS
The mixture is warmed slowly to
facilitate the crystallization process.
The solution is allowed to cool naturally
to room temperature to aid the
formation of fine crystals.
The filter paper should adhere over the
perforated plate the suction filter.
The filter paper must be moistened
before filtration with the chosen solvent.

PRECAUTIONS(cont)
Suction filtration should be done
gently.
Excess addition of solvent should be
avoided.
When two solvents A and B are used
for a Multi-solvent recrystallization
process, solvents A and B must be
miscible.

CHOICE OF SOLVENT
Substance should be insoluble in
solvent at room temperature but
soluble at elevated temperatures.
Impurities should be either soluble or
completely insoluble in solvent.
Should yield well defined crystals of
required compound.
Should possess low boiling point.

CHOICE OF SOLVENT(cont)
It should not react with the
compound of interests.
Should have similar chemical
properties as the compound to be
recrystallized.
Other factors to be considered
include ease of manipulation,
flammability and cost.

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