SUBLIMATION AND MELTING POINT DETERMINATION

Patricia L. Chua, Julienne Chua, Eunice M. Cruz

Alessandra S. Chavez and Myrielle Co
Group 4 2A Medical Technology Organic Chemistry Laboratory

ABSTRACT
The study ought to perform a successful sublimation procedure for benzoic acid and determine the difference between
melting points of purified, impure and an equal proportion of both benzoic acid. 5 grams of benzoic acid was
sublimated in an evaporating dish wherein pure benzoic acid was obtained. Recovered crystals were then collected
and triturated into fine powder and were placed inside capillary tubes labeled as purified. Pure benzoic acid was
triturated and was directly placed inside a separate capillary tube and labeled as pure. The last capillary tube was
filled by a 1:1 ratio of the pure and purified benzoic acid. The first two tubes were attached to a thermometer through
a rubber band and were immersed in an oil bath. There were four temperatures recorded, the time when both of the
acids first starts to sublime and the temperatures when the two capillary tubes have completely sublimated.

INTRODUCTION
Sublimation is the transition of a substance
directly from the solid to the gas phase without
passing through an intermediate liquid phase.
Sublimation is an endothermic phase
transition that occurs at temperatures and
pressures below a substance's triple point in
its phase diagram. Sublimation requires
additional energy and is an endothermic change.
Sublimation is a technique used by chemists to
purify compounds. A solid is typically placed in
a sublimation apparatus and heated
undervacuum. Under this reduced pressure, the
solid volatilizes and condenses as a purified
compound on a cooled surface (cold finger),
leaving a non-volatile residue
of impurities behind. Once heating ceases and
the vacuum is removed, the purified compound
may be collected from the cooling surface. [1] In
this experiment, the group should be able to
purify benzoic acid through sublimation,
determine and compare the melting point of the
product with a standard and calculate the
percentage recovery. Moreover, melting point
determination was employed together with
sublimation to ascertain the identity and purity of
an unknown compound. Melting point is defined
as the temperature at which its solid and liquid
phases coexist in equilibrium. The normal melting
point of a substance is its melting point at one
atmospheric pressure. Changes in pressure have
very small effects on melting points, but they
have large effects on boiling points. [2]

EXPERIMENTAL
A. Compounds tested (or Samples used)
Benzoic acid was used in this experiment. It is
a white crystalline organic compound belonging
to the family of carboxylic acid, widely used as


food preservative and in the manufacture of
various cosmetics, dyes, plastics and insect
repellents. [2]

B. Procedure
1. Preparation of Capillary tubes
We directly heated while rotating the capillary
tube using a Bunsen burner until it started to
melt and then we closed the other side.
2. Preparation of the hot oil bath set-up
In a clean beaker, we put a 250-mL of oil. Then
we placed the beaker on top of a tripod with wire
gauze. After, we placed a Bunsen burner
beneath, which served as the source of heat.
Then, the thermometer with attached capillary
tubes was submerged into the oil bath.
3. Purification of Benzoic acid
The 5.0grams of benzoic acid was placed in an
evaporating dish. Then it was covered with filter
paper and an inverted watch glass and was
placed securely using a masking tape. A damp
tissue was placed on top of the watch glass which
served as the cooling pad. The substance was
heated using a hot plate for 10 to 15 minutes
until most of the substances have been
vaporized. The substance was cooled. After
cooling, the watch glass was removed and the
sublimated were collected.
4. Determining the melting point
The sublimated substance was grinded until it
was in powder form. The powdered substance
was then put inside the capillary tubes. We filled
the capillary tubes until it is 3 5 mm high. The
capillary tubes were attached to the thermometer
and the ends of the capillary tubes were attached
close to the mercury of the thermometer. The
capillary tubes together with the thermometer
were submerged into the oil bath and were
continuously stirred. The temperature was taken
down at which the sublimate starts to melt and
when it is completely melted.


Figure 1. Purification of Benzoic acid through
Sublimation

The figure above shows the set-up for the
purification of benzoic acid. The set-up made use
of a hot plate, evaporating dish containing the
substance, filter paper, inverted watch class
together with a damp tissue paper above.

RESULTS AND DISCUSSION
After subjecting the substance to heating, the
vapor begun to solidify and became crystalline in
nature. The substance that was once amorphous,
was subjected to sublimation began to become a
colorless crystal which was later grinded into
powdered form. The 2.41 g that was collected
from the starting amount of Benzoic acid which
was 5.0 g. The percentage recovered from the
benzoic acid was 48.2%. The grinded crystals
were inserted into a capillary tube which was
attached to the thermometer, which was later
submerged into an oil bath. The oil bath was used
to melt the substance together with the standard
to be able to compare their melting points from
each other. The standard began to melt at 98C
o

and it was completely melted at 109C
o
. While the
sample started to melt at 118C
o
and it was
completely melted at 128C
o
. Therefore, one could
conclude that the standard has a higher melting
point compared to the sublimate which was
acquired though sublimation.



Table 1. Data and Results

Table 1 shows the different data and results
obtained from the experiment. Starting from the
first data, which is the weight of the original
benzoic acid, the second result which is the
weight of the sublimate which was gathered after
the purification, then the percentage recovered
as well as the temperature when the benzoic acid
melted.


Weight of the impure
Benzoic acid

5.0 g

Weight of the watch
glass + sublimate

90.11 g

Weight of the watch
glass (empty)

87.70g

Weight of the sublimate

2.41 g

Percentage recovery

48.2%

Melting point of Benzoic
acid

128C
o

Table 2. Temperature Recordings

Table two shows the data gathered in the
sublimation of impure benzoic acid and pure
benzoic acid. Both acids are placed in a capillary
tube and then joined together with a
thermometer by a rubber band then submerged
into the oil bath. The heat of the oil bath came
from the Bunsen burner and wire gauze. Then
the two acids are observed, the first column
indicates the temperature in which it started
sublimating while the second column indicates
the temperature when they completely
sublimated.


Sublimate

T
1
C
o

T
2C
o

Impure
Benzoic Acid

98C
o

109C
o

Pure Benzoic
Acid

118C
o

128C
o

CALCULATIONS

Weight of benzoic acid obtained
% Recovered = x 100
Weight of benzoic acid before
crystallization

2.41 g
% Recovered = x 100
5.0 g

% Recovered = 48.2 %


REFERENCES
[1]http://en.wikipedia.org/wiki/Sublimation_(pha
se_transition)
[2]http://www.scribd.com/doc/106152244/Subli
mation-and-Melting-Point-Determination
[3]http://www.britannica.com/EBchecked/topic/6
1357/benzoic-acid