Experiment # 07 OBJECT: To Perform Recrystallization of Salicylic Acid. Requirements

EXPERIMENT # 07
OBJECT: To perform recrystallization of salicylic acid.
Requirements:
Theory:
Recrystallization:
The products of chemical reactions can be impure. Purification of your product must be
performed to remove by-products and impurities. Liquids are customarily purified by distillation,
while solids are purified by recrystallization (sometimes called simply crystallization)
Recrystallization of solids is a valuable technique to master because it is one of the methods used
most often for purification of solids. Other techniques for purifying solids include sublimation,
extraction and chromatography. Nevertheless, even when one of these alternative methods of
purification has been used, the solid material thus isolated may still be recrystallized to achieve
the highest possible state of purity.
The process of recrystallization involves dissolution of the solid in an appropriate solvent at an

elevated temperature and the subsequent re-formation of the crystals upon cooling, so that any
impurities remain in solution. This technique, called solution re crystallization. If the impurities
present in the original solid mixture have dissolved and remain dissolved after the solution is
cooled, isolation of the crystals that have formed should ideally provide pure material.
Alternatively, the impurities may not dissolve at all in the hot solution and may be removed by
filtration before the solution is cooled.
Types of recrystallization:
The major classic situation is that a preferred "compound A" is contaminated by a small amount
of "impurity B". There are also various recrystallization techniques that can be used such as:
Single-solvent recrystallization: Basically, the mixture of "compound A" and "impurity B" are
dissolved in the smallest amount of hot solvent to fully dissolve the mixture, thus making a
saturated solution. Saturation is the point at which a solution of a substance can dissolve no more
of that substance and additional amounts of it will appear as a precipitate (formation of a solid in
a solution). The solution is then allowed to cool. As the solution cools, the solubility of
compounds in solution drops. This results in the desired compound dropping (recrystallizing)
from solution. The slower the rate of cooling, the bigger the crystals formed.
Multi-solvent recrystallization: This method is the same as the above, but where two (or more)
solvents are used. This relies on "compound A" and "impurity B" being soluble in a first solvent.
A second solvent is slowly added. Either "compound A" or "impurity B" will be insoluble in this
solvent and precipitate, whilst the other of "compound A"/"impurity B" will remain in solution.
Thus the proportion of first and second solvents is critical. Typically, the second solvent is added
slowly until one of the compounds begins to crystallize from solution and then the solution is
cooled. Heating is not required for this technique but can be used.
Hot filtration recrystallization: Hot filtration can be used to separate "compound A" from both
"impurity B" and some "insoluble matter C". This technique normally uses a single-solvent
system as described above. When both "compound A" and "impurity B" are dissolved in the
minimum amount of hot solvent, the solution is filtered to remove "insoluble matter C". This
matter may be anything from a third impurity compound to fragments of broken glass. For a
successful procedure, one must ensure that the filtration apparatus is hot in order to stop the
dissolved compounds crystallizing from solution during filtration, thus forming crystals on the
filter paper or funnel.
Seeding: Crystallization needs a beginning step. This can be impulsive or can be done by adding
a small amount of the pure compound (a seed crystal) to the saturated solution, or can be done by
simply scratching the glass surface to create a seeding surface for crystal growth. It is thought
that even dust particles can act as simple seeds. A seed crystal is a small piece of single crystal
material from which a large crystal of the same material typically is to be grown.
Application of crystallization:
Some of the applications of Re-crystallization are:

 In more recent times, the fast expansion of the chemical industry has required a thorough
study of the dynamics of crystallization, and this unit operation is now used in many
industrial manufacturing areas: table salt, sugar, sodium sulfate, urea, just to name a few,
are produced by crystallization from solutions.
 Production of sucrose from sugar beet, where the sucrose is crystallized out from an
aqueous solution.
Procedure:
1. Place approximately 0.2gm of salicylic acid in 100ml flask

2. Add 2ml of water Heat the mixture to a gentle boil and continue adding water in 0.5-
mL portions until no more solid appears to dissolve in the boiling solution. Record
the total volume of water used; no more than 10 mL should be required.
3. First cool the mixture at room temperature and then place it on an ice bath for at least
15min.
4. Filter it (weigh the filter paper before use)
5. Wash the filter cake with small portions of cold water.
6. Weigh the final substance
Observation/calculation
Weight of empty filter paper =
Initial weight of substance=
Final weight of substance= final weight-filter paper weight
% recovery= final weight/initial weight × 100
Result:
Precaution:
References:
http://www.innovateus.net/science/what-recrystallization
http://www.chem.utoronto.ca/coursenotes/CHM249/Recrystallization.pdf

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EXPERIMENT # 07

OBJECT: To perform recrystallization of salicylic acid.

The process of recrystallization involves dissolution of the solid in an appropriate solvent at an

Some of the applications of Re-crystallization are:

1. Place approximately 0.2gm of salicylic acid in 100ml flask

Weight of empty filter paper =

Initial weight of substance=

Final weight of substance= final weight-filter paper weight

% recovery= final weight/initial weight × 100

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