SUBLIMATION AND MELTING POINT DETERMINATION

Jon Ellis G. Datu, Athina Darla B. Deala, Alan Nathan Derige, Mary Kimberly L. Espaldon, Ma.
Theresa Angeli M. Estabillo, and Jemielle Patricia A. Estrada
Group 3 2F Medical Technology Organic Chemistry Laboratory
ABSTRACT
The experiment is about Sublimation and Melting point determination. Sublimation is the transition of a
substance from the solid to the gas phase. Sublimation in this experiment was used to collect the
vaporized impure benzoic acid. The melting point of a solid is the temperature the solid changes to liquid
at atmospheric pressure. Melting point in this experiment was used to determine the purity of the
sublimate of impure benzoic acid. First, 5g of impure benzoic acid was placed in an evaporating dish and a
filter paper and on top of the filter paper, was an inverted pre-weighed watch glass, covering the
evaporating dish then it was heated on a hot plate, all the while a wet tissue was kept moist for 10 -15
minutes of heating. After cooling the whole set-up, the sublimate, which solidified and became crystalline
in nature, was collected. The sublimate on the pre-weighed watch glass was collected and the percentage
recovery was computed to be 8.6%. The sublimate on the melting point was grinded into fine powder and
placed on the open end which was not sealed by a Bunsen burner and the capillary tube was filled with
1mm of the sublimate. The capillary tube was then attached to a thermometer aligned to the mercury bulb
of the thermometer and was immersed in an oil bath and heated. The temperature at which the sublimate
started to melt was at 120 degrees Celsius and when it was completely melted it was at 122 degrees
Celsius. The difference of the initial and final melting point of pure benzoic acid should range from 0
degrees Celsius to 1 degrees Celsius and because the sublimate had a 2 degrees Celsius difference in its
melting point, it can be concluded to still have impurities.

INTRODUCTION
Sublimation is one of the phase transitions. In
this case, a solid is turning directly into a gas. As
a sublimating material changes from a solid to a
gas, it never passes through the liquid state [1].
If the vapor pressure is greater than the
atmospheric pressure at the melting point, the
solid will go through the process of sublimation.
Sublimation is a technique used to purify solid
mixtures. Melting point determination can be
used to find out the identity and purity of an
unknown compound [2].
The process of sublimation in this experiment is
used to purify the impure benzoic acid. The
purification process involved in sublimation is
applicable for impurities which are non-volatile or
with lower vapor pressure than the pure
compound or substance.
In this experiment, the objectives of the group
were (1) to purify the impure benzoic acid
through sublimation, (2) calculate the percentage
recovery of the benzoic acid after sublimation and
lastly, (3) to determine the melting points of the
sublimate and the pure benzoic acid through the
use of an oil bath. The significance of this
experiment is to understand the process of
sublimation and to properly execute the common
organic chemistry laboratory method.

EXPERIMENTAL
A. COMPOUNDS TESTED (OR SAMPLES
USED)
Benzoic Acid
It is a colorless crystalline solid and a simple
aromatic carboxylic acid. It occurs naturally in
many plants and it serves as an intermediate in
the biosynthesis of many secondary metabolites

B. PROCEDURE
1. SUBLIMATION
AND
MELTING
POINT DETERMINATION
In the experiment, 5g of impure benzoic acid
was placed in an evaporating dish. Followed by a
filter paper and on top of the paper, was an
inverted pre weighed watch glass, both acting
as a cover on the evaporating dish. Both (filter
paper and watch glass) were sealed on the dish,
leaving no opening with a masking tape and then
heated on a hot plate, all the while a wet tissue
was kept moist for the duration of the 10 -15
minutes of heating. After the set up was
cooled; the sublimate on the pre weighed
watch glass was carefully collected and the
percentage recovery was computed. The
sublimate on the melting point was grinded into

fine powder and placed on the open end which

was not sealed by a Bunsen burner. The capillary
tube was filled with 1mm of the sublimate. The
capillary tube was then attached to a
thermometer by a masking tape and aligned with
the mercury bulb of the thermometer. Lastly, the
thermometer and the capillary tube was
immersed in an oil bath and heated. The
temperature at which the sublimate started to
melt and when it was completely melted was
noted.

Fig
ure 1.
Acid

Benzoic

2. Computation
Percentage Recovery:

w weight of residue
=
100
w weight of sample

RESULTS AND DISCUSSION

Most of the 5.00 g impure benzoic acid was

vaporized when it was subjected to heating while it
was covered with perforated filter paper and a preweighed watch glass for 10-15 minutes, and while
the center of the watch glass was kept moist with
water. After cooling the whole set-up, the sublimate,
which solidified and became crystalline in nature,
was collected. The substance that was retrieved can
be seen as crystal-like, colorless, and even
resembled needles. The sublimate was then
pulverized into fine powder so that it would be
inserted in a capillary tube for melting point
determination. In Table 1, the weight of the
sublimate collected which was 0.43 g and the
percent recovery of the benzoic acid sample which
has a value of 8.6% could be seen.
Weight of the impure 5.00 g
benzoic acid
Weight of the watch glass 93.23 g
+ sublimate
Weight of the watch glass 92.80 g
(empty)
Weight of the sublimate
0.43 g
Percentage recovery
8.60%
Table 1. Weight of Sublimate and Container

Percentage
Recovery
of
Benzoic Acid Sample
% Benzoic Acid Sample =

0.43
100
5.00

0.43
x 100
5.00

= 8.6%
In Table 2, the data regarding the melting point
of the sublimate, as well as the pure benzoic acid,
could be seen. It was seen that the differences of the
initial melting point and final melting point of
sublimate and pure benzoic acid was 2o C and 1o C,
respectively.
Sublimate
Pure
Benzoic
Acid

TI
120o C
125o C

TF
122o C
126o C

Difference
2o C
1o C

Table 2. Temperature of Sublimate and Pure

Benzoic Acid

in class that the difference of the initial and final

melting point of pure benzoic acid should be 0o C to
1o C. Because the sublimate had a 2 o C difference in
its melting point, it showed that there were still
impurities present in the sublimate causing a higher
difference in the initial and final melting point.
REFERENCES
[1]
Morrissey, S. What is Sublimation in
Chemistry? - Definition, Process & Examples.
http://study.com/academy/lesson/what-issublimation-in-chemistry-definition-processexamples.html 10/11/15
Bathan, G.I., Bayquen, A.V., Crisostomo,
A.B.C., Cruz, C.T., de Guia, R.M., Farrow, F.L.,
Pena, G.T., Sarile, A.S. and Torres, P.C. (2014).
Laboratory Manual in Organic Chemistry. Revised
ed. Quezon City, Philippines: C&E Publishing, Inc
[2]

Figure 2. Crystallized Benzoic Acid

Sublimation was used to collect the vaporized

impure benzoic acid. Through this process, the
benzoic acid was also purified because the
impurities found in the impure benzoic acid did not
vaporize along with the pure benzoic acid due to
different evaporating points. Melting point was also
used in order to determine the purity of the
sublimate of impure benzoic acid. It was discussed