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CRYSTALLIZATION

G.A.N Obligado

BS Chemistry, College of Arts, Sciences and Education


Aquinas University of Legazpi, Rawis Legazpi City, Philippines
DATE PERFORMED: August 7, 2014

ABSTRACT
Purification of benzoic acid from a mixture containing benzoic acid,
sodium chloride and congo red was performed by crystallization. The addition
of charcoal and the techniques utilized such as heating, stirring and cooling
aided the steps on the way to crystallization which are the following:
elimination of impurities, nucleus formation and promoting the growth of
crystals. The color of the filtrate, the color, size and shape of the crystals
formed were observed as well as the appearance of the dissolved purified
crystals after adding the nitric acid and the silver nitrate. The recovery
percentage was 48.3% .
INTRODUCTION
Purification
of
organic
compounds
is
performed
to
eliminate impurities. Impure liquid
is usually purified by distillation
while impure solid can be purified
through
crystallization.
Crystallization is a technique which
involves
the
following
steps:
removal of impurities, nucleus
formation, and encouragement of
growth of crystals.
In case of colored impurities,
adsorption
by
the
use
of
decolorizing carbon is usually
employed. A common way to
remove impurities is to dissolve the
organic compound in a heated
mixture of solvent and adsorbent.
The solvent must not react with the
solute, can dissolve the solute
readily at a raised temperature but
cautiously at a lower temperature
and
suitably
volatile.
Excess
amount of decolorizing carbon can
be a cause of loses for the reason

that it may adsorb some of the


sample.
Nucleus formation can be
spontaneous or induced while
promoting the growth of crystals
can be done by stirring or
agitation.

METHODOLOGY
One gram each of benzoic
acid, sodium chloride and congo
red were weighed and combined in
a 150-ml beaker. Few amounts of
the mixture were used as sample.
In that case, 50 ml of distilled
water was added in the sample and
was heated. When the benzoic acid
dissolved, 0.5 gram of charcoal was
put. Stirring was continuously done
during the heating. The solution
was filtered right after it boiled.
Equal amounts of the hot filtrate
were collected separately in two
test tubes. One test tube was

covered and set aside while the


other one was put into an ice bath
for about less than three minutes.
Then, the contents of the two test
tubes were combined and filtered.
The crystals were washed with cold
water. The crystals on the filter
paper were placed on a watch
glass and covered letting it to
become dry.
Small
amounts
of
the
purified crystals were dissolved in a
test tube with 1 ml hot distilled
water. One drop of nitric acid and
two drops of silver nitrate was then
added.

crystals in the slow cooling set-up.


Hence, formation of crystals was
greatly induced when the set-up
was put in a lower temperature.
After the drops of nitric acid
and silver nitrate, the crystals have
settled down. However, there were
floating substances which were
little
amounts
of
impurities,
perhaps.

Percent Recovery =
Amount of solid recovered
100
Amount of solid
Percent Recovery =

RESULTS AND DISCUSSION


The color of the filtrate was
clear but somehow it has minute
amounts of crystal-like white
substances possibly due to the
hastily formation of the crystals
during the filtration.
The crystals in the slow
cooling set-up were less than in the
rapid cooling set-up. The color of
the crystals in the two set-ups was
just the same, which is white. The
size of the crystals in the rapid
cooling set-up was larger than the

1.4 g
100
3.0 g

Percent Recovery = 48.3%

REFERENCES
1) Skoog, D.A.; West, D.M;
Holler, F.J.; Crouch, S.R.;
Chen, S.C.; Introduction to
Analytical Chemistry, Eighth
Edition; Cengage Learning
Asia Pte Ltd: Singapore.