Recrystallization
Recrystallization
Recrystallization
Recrystallization, also known as fractional crystallization, is a procedure for purifying an impure compound
in a solvent. The method of purification is based on the principle that the solubility of most solids increases
with increased temperature. This means that as temperature increases, the amount of solute that can be
dissolved in a solvent increases.
Introduction
An impure compound is dissolved (the impurities must also be soluble in the solvent), to prepare a highly
concentrated solution at a high temperature. The solution is cooled. Decreasing the temperature causes the
solubility of the impurities in the solution and the substance being purified to decrease. The impure
substance then crystallizes before the impurities- assuming that there was more impure substance than there
were impurities. The impure substance will crystallize in a purer form because the impurities won't
crystallize yet, therefore leaving the impurities behind in the solution. A filtration process must be used to
separate the more pure crystals at this point. The procedure can be repeated. Solubility curves can be used to
predict the outcome of a recrystallization procedure.
Note
The slower the rate of cooling, the larger the crystals are that form. The disadvantage of recrystallization is
that it takes a long time. Also, it is very important that the proper solvent is used. This can only be
determined by trial and error, based on predictions and observations. The solution must be soluble at high
tempratures and insoluble at low temperatures. The advantage or recrystallization is that, when carried out
correctly, it is a very effective way of obtaining a pure sample of some product, or precipitate.
Procedure
1. Dissolve the solute in the solvent: Add boiling solvent to a beaker containing the impure
compound. Heat the beaker and keep adding solvent until the solute is completely dissolved. See
Figure 1
2. Cool the Solution: The solution is cooled in open air first, and then cooled in an ice bath. Slow
cooling often leads to purer crystals. Crystals should form on the bottom of the beaker. The process
of "seeding" can be used to aid the formation of crystals- this means adding a pure crystal of the
compound. The pure crystal forms a surface for the solute to crsytallize upon. See Figure 2
3. Obtain the crsytals of the solute: The more pure crystals of the solute are the desirable part of the
mixture, and so they must be removed from the solvent. The process used for isolating the crystals
that remain in the beaker still is called vacuum filtration. Suction is created using an aspirator, and
whatever remains in the beaker is poured though a Buchner funnel. If for some reason there are no
crystals visible, a gravity filtration can be performed. Activated carbon is added to the solution, the
mixture is boiled, and a funnel system is used to transfer the new mixture to a new beaker of boiling
solvent. Filter paper is used in the funnel to remove excess carbon. After this mixture cools slowly
there should be large crystals present.
4. Dry the resulting crystals: The crystals are dried by leaving them in the aspirator and then by
removing them to a glass dish to wait a while longer. The purity of the crystals can be tested by
performing a "melting point determination".