PROG. NO.

: DATE:
CRYSTALLIZATION
(Batch Crystallization)

Aim: To find the yield of crystals in batch crystallizer.

Apparatus: 500ml beaker, measuring cylinder, weighing machine, hot plate.
Chemicals: Copper sulphate powder.
Theory: Crystallization is the unit operation that involves the separation of solute from its solution in
the form of crystals. It is normally carried out in process industries, from solution in the form of almost pure
crystals. Crystallization usually involves concentration of solution and cooling of solution until the solute
concentration becomes greater than its solubility at that temperature then the solute comes out of the solution
in form of pure crystals. The performance of the process is evaluated in terms of size, shape, yield and purity
of crystals. A saturated solution is defined as the one, which is in equilibrium with excess of solid solute of a
given temperature. Supersaturation is the quantity of the solute present in the solution in which crystals are
growing as compared with the quantity of the solute that is in equilibrium with the solution. The amount of
crystals formed depends upon the difference in saturation concentration, since once the crystallization
begins, the extra solute held in the solution due to supersaturation also comes out of the solution in the form
of crystals. There are two steps involved in crystallization.
1) Nucleation
2) Crystal growth
The generation of solid phase is called nucleation while growth is the increase in the size of this nucleus with
the layer-by-layer addition of solute. Supersaturation is the common driving force for nucleation and crystal
growth. The number of nuclei and the rate of growth of crystals does not depend upon the temperature of
operation and of less number of nuclei and hence large size crystals are formed whereas rapid cooling results
into the formation of large number of nuclei, giving yield containing large number of tiny crystals. In
crystallization supersaturation is obtained by
1) Adding the solute
2) Evaporating part of solvent
3) Cooling the saturated solution

Mier's supersaturation theory

There is definite relationship between the solubility curve and super solubility curve. Both the curves are
approximately parallel to each other as shown;
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If the solutions having composition and temperature indicated by point C is cooled in the direction shown by
arrow, it first crosses the solubility curve AB and crystal formation will not begin until the solution is super
cooled considerably past the curve AB. According to Mier's theory, crystallization will start in the
neighborhood of point D and concentration of the solution then follows roughly along curve DE for an
initially unseeded solution. Curve PQ represents the limit where this spontaneous crystal formation starts.
According to Mier's theory under normal conditions, nuclei can not form and crystallization can not occur in
area between solubility curve and super solubility curve i.e., at any position short of point D along line CD.

Procedure :

1) Take 60 gm of CuSO4 powder in 500 ml beaker.

2) Add 200 ml water and stir well.
3) Heat the solution gently until all the powder dissolves in it. This will be the saturated solution.
4) Continue heating and evaporate nearly half of the solution so that the solution becomes super
saturated.
5) Cool the beaker slowly.
6) After two hours the crystals of CuSO4 forms. Remove the mother liquor.
7) Dry the crystals and weigh it.
Observations:
Weight of CuSO4 powder taken = 60 gm
Weight of crystals obtained =

Calculations :

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The yield of the crystals can be calculated as
% yield = Weight of crystals obtained
________________________________
 100
Weight of crystals in feed

Result : The %yield of the crystals _____________

Precautions : Cooling should be slow.

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