CHEM-102 Spring2016 EXP-2 Manual Crystallization

Ko University
Spring 2016
CHEM 102 GENERAL CHEMISTRY LABORATORY
EXPERIMENT 2
Super-cooled Solution and Crystallization
OBJECTIVES
The objective of the experiment is to demonstrate super saturated
solution, super-cooling, crystallization, and heat release of the process.
INTRODUCTION
Super-cooling is the process of lowering the temperature of a liquid or a
gas below its freezing point without it becoming a solid. The condition of
super-cooling alone is not sufficient reason for a system to begin
crystallization. Before crystals can develop in solution there must be
many nuclei (or seeds) which act as centers of crystallization. Nucleation
may occur spontaneously or it may be induced artificially. Nucleation can
be induced by agitation, mechanical shock, friction, electrical discharge
and light or sonic irradiation. It is also known that scratching the container
vessel of super-cooled solution cause nucleation.
Sodium acetate can exists in liquid form below its usual melting point.
When a supersaturated solution is prepared, then the Gibbs energy for
further solution is unfavorable. Instead, the reverse process occurs:
sodium acetate tends to crystallize out and produces heat. In order for the
crystallization to occur, very small particles of crystalline sodium acetate
must form, and then aggregate into larger crystals. But when a particle
forms it leaves behind a quantity of solvent which is less concentrated and
so those ions near the surface have a tendency to redissolve immediately.
This is not a problem for large particles (which have relatively little surface
area), but it makes it difficult for a small particle to survive long enough to
grow and past the critical size where the heat gain outweighs these
surface effects. Small particles therefore face a large energy barrier
against crystallization. The solution is trapped in the metastable,
supersaturated state.
Addition of a foreign object helps because particles forming on the surface
of the object can only redissolve away from it. Thus the effective surface
area of the particle is halved (or reduced even more if the foreign object
has cavities). This allows the small particles to grow to a size where
surface effects can no longer prevent the formation of the crystal. Once
1
this has happened, the crystal can continue growing and releasing heat
until the solution is merely saturated, and the processes of solution and
deposition are at equilibrium.
MATERIALS
Solution bottles
Beaker
Wash bottle
Magnetic
stirring bar
retriever
Magnetic stirring bar
Heating
magnetic
stirrer
Spatula
Glass
stirring rod
Thermometer
Laboratory
balance
EXPERIMENTAL PROCEDURE
SAFETY PRECAUTIONS: Acetic acid is irritant. Safety glasses must be
worn at all times during this experiment. Also perform all experiments in
hood.
WASTE DISPOSAL: All waste from this experiment should be poured into
the WASTE containers in the fume hood.
NaHCO3 (s) + CH3COOH (aq)
CH3COONa (s) + H2O (l) + CO2 (g)
(MWNaHCO3=84.01 g/mol; MWCH3COOH=60.05 g/mol; dCH3COOH=1.049 g/ml).

1. Measure 15 ml acetic acid (CH3COOH) into a beaker.
2. Dilute your solution with 10 ml of water
3. Add 16 g of sodium hydrogen carbonate (NaHCO 3) in small potions
while constant stirring between additions. NaHCO3 and CH3COOH
react to form sodium acetate (CH 3COONa) and carbon dioxide gas. If
the NaHCO3 is not added slowly essentially sodium hydrogen
carbonate-acetic acid volcano occurs which would overflow the
beaker.
4. Now sodium acetate solution is prepared, but it is too dilute
(solubility of sodium acetate is 46.4 g / 100 ml H2O), therefore most
of the water should be removed. Boil the solution to concentrate the
sodium acetate until a crystal skin or film starts to form on the
surface. (There might be some discoloration!)
5. Pour the solution into a separate container and cover it with plastic
wrap. Once sodium acetate solution is removed from heat it should
be immediately covered to prevent any further evaporation. The
solution should not contain any crystals. If there is any crystal, stir a
very small amount of water or acetic acid into the solution, just
sufficient to dissolve the crystals.
6. Place the covered container of sodium acetate solution in ice bath to
cool for 15 min. DO NOT DISTURB YOUR SOLUTION DURING COOLING
PROCESS. Cooled sodium acetate solution in the beaker is an
example of a super-cooled liquid. That is, the sodium acetate exists
in liquid form below its usual crystallization temperature.
7. The crystallization can be initiated by adding a small crystal of

sodium acetate or possibly even by touching the surface of the
sodium acetate solution with a glass rod. The crystallization is an
example of an exothermic process (heat is released).
Data Sheet
Date:
Name & Surname:
Please read results & discussion part of report writing guide before
performing your experiment and note any necessary data for answering
that questions.

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Ko University

Magnetic stirring bar

NaHCO3 (s) + CH3COOH (aq)

CH3COONa (s) + H2O (l) + CO2 (g)

(MWNaHCO3=84.01 g/mol; MWCH3COOH=60.05 g/mol; dCH3COOH=1.049 g/ml).

7. The crystallization can be initiated by adding a small crystal of

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