Crystallization

The crystallization practice is aimed at the separation of substances in the form of

crystals. Thus a substance can be isolated after a synthesis or purify solid
substances.
For the realization of the practice in the laboratory a dissolution is prepared saturated
with the substance to be purified. Previously, the bibliography should be consulted
variation of the solubility of the salt with temperature

The solid products that are obtained in a reaction are usually accompanied by
impurities that must be eliminated in order to dispose of the desired product in the
highest possible degree of purity. The most suitable method for the elimination of the
impurities that contaminate a solid is by successive crystallisations either in a pure
solvent or in a mixture of solvents. The procedure is given the generic name of
recrystallization. The procedure consists of

• Dissolution of the impure crystalline product in a suitable solvent at or near boiling

temperature
• Filter the hot solution to eliminate insoluble particles such as dust or other impurities
• Allow the solution to cool slowly until the crystallization of the purified product is as
complete as possible
• Separate the crystals obtained from the supernatant liquid (mother liquor) by
filtration
• Drying the solid obtained
• Verification of the purity of the solid obtained through its physical constants (melting
point and spectroscopic data)

The crucial point in the crystallization process is the proper choice of solvent that the
following properties must fulfill
• High dissolving power of the substance to be purified at high temperatures
• Low dissolution capacity of impurities that contaminate the product in any
temperature range
• Generate good crystals of the product to be purified
• Easy to eliminate

A very important factor to consider is whether the solvent is aqueous or organic. In

case of using organic solvents it is always necessary to heat the mixture with the
reflux assembly. If not done in this way flammable vapors are generated that pass
into the atmosphere and that in contact with flames or heat sources lead to a serious
risk of fire and explosions.

Material

 Conical funnel
 Erlenmeyer
 Tumbled beaker
 Büchner
 Kitasatos
 Flased-mouth flask
 Reflux condenser

Folds filter
 Assemblies and equipment
 Suction filtration equipment
 Reflux equipment
 Gravity filtration equipment

Process
A.- Recrystallization of benzoic acid in water
1. Weigh 1 g of benzoic acid, transfer it to a beaker.
 2. Add approximately 20 ml of distilled water and heat the mixture to boiling. Add
portions of hot water little by little, stirring until completely dissolved.
3. Remove the Erlenmeyer flask from the heat source, filter hot with a pleated
filter and a funnel and allow the filtrate to cool to room temperature for a
minimum of 20 minutes.
4. Separate the crystals obtained by filtering by suction.
5. Dry the solid and weigh once dry.
6. Determine the melting points before and after the recrystallization process.

B.- Recrystallization of acetanilide in water

1. Weigh 1g of acetanilide, transfer it to an Erlenmeyer flask.

2. Add 20 ml of water and heat gently. It is observed the appearance of an oil in
the solution that ends up dissolving with the addition of various portions of hot
water.
3. If a colored solution is obtained add a small portion of active carbon
(approximately 0.3 g).
4. Filter into the hot solution with a pleated filter and a conical funnel. Allow the
mixture to cool for 30 minutes and separate the crystals by filtering by suction.
5. Dry the solid and weigh.
6. Determine the melting points before and after recrystallization.

C.- Recrystallization of naphthalene with ethanol (crystallization with a

flammable solvent)

1. Weigh 2.5 g of naphthalene.

2. Transfer the solid to a 50 ml round bottom flask and add 12 ml of ethanol and
a piece of porous plate.
3. Attach a reflux condenser and heat the mixture to boiling. Add with the help
of a Pasteur pipette plus ethanol in 1 ml portions, maintaining the reflux until
the solid is completely dissolved.
4. Filter hot with a pleat filter, with great care avoiding the proximity of heat
sources and vacuuming vapors.
5. Collect the filtrate in a 50 ml Erlenmeyer flask and cover it with a cork.
6. Allow to cool to room temperature for at least 30 minutes and filter in a
Büchner, dry and weigh the solid obtained.
7. Determine the melting points before and after recrystallization