SUBLIMATION AND MELTING POINT DETERMINATION

Margarita Ysabel S. Mangahas, Cara Camille M. Matute, Emilyn D. Millares,

John Acener C. Padua and Kathryn Cheshire P. Pangilinan
Group 5 2A Medical Technology Organic Chemistry Laboratory
ABSTRACT
In this experiment, sublimation was used to purify solid mixtures. The compound used to undergo purification is
impure benzoic acid. The product obtained after the heating process is called the sublimate in the form of crystals.
The weight of the impure benzoic acid gave a lot of difference from the sublimate obtained from 5.0014 g to 0.3213 g,
respectively. Thus, the measured sublimate showed the low percentage recovery of the said compound. The sublimate
was then subjected to melting point determination together with the pure benzoic acid through the oil bath. The oil
bath was used since it is able to measure temperatures even those beyond 100 C and are highly recommendable for
compounds which have higher boiling points. As it was seen in the results for the melting point determination, the
sublimate started to melt at 116 C and stopped melting at 120 C while the pure benzoic acid started to melt at 120
C and ended at 121 C. The temperatures measured indicated that the pure benzoic acid has a higher vapour
pressure than the sublimate.

INTRODUCTION
Sublimation is the direct vaporization of a solid
by heating without passing through the liquid
state. [1] The process of sublimation in this
experiment is used to purify the impure benzoic
acid. The impurities in the benzoic acid have
amino compounds that are present in a larger
extent and must be removed because of phenyl
and benzyl compounds that seriously affect the
product.[3] This process occurs if the vapour
pressure of the substances greater than the
atmospheric pressure at the melting point.[2]
The process of purification involved in sublimation
is applicable for impurities which are non-volatile
or with lower vapor pressure than the pure
compound or substance.
The objectives of this experiment are: (1) to
purify the impure benzoic acid through
sublimation, (2) to calculate the percentage
recovery of the benzoic acid after sublimation,
and (3) to identify the melting points of the
sublimate and the pure benzoic acid through the
use of an oil bath.

extent because of the presence of hydrogenous

compounds. [3]

B. Procedure
1. Sublimation
Sublimation set-up was used to purify the
impure benzoic acid. Hot plate, evaporating dish,
5 g of impure benzoic acid, clean sheet of bond
paper to cover and masking tape for sealing,
watch glass, and moistened tissue paper were
needed as materials. 5 g of impure benzoic acid
was put into the evaporating dish and sealed with
a clean sheet of bond paper with holes on it using
a masking tape. Before putting the evaporating
dish on the hot plate, a pre-weighed watch glass
was set on the dish invertedly. While heating, the
tissue paper was put above the watch glass and
continuously moistened for 10-15 minutes until
most of the sample has vaporized. The set-up
was cooled and then the watch glass was
carefully inverted to collect the sublimate in a
transparent, crystalline, needle-like appearance.
The sublimate was weighed for percentage
recovery.

2. Melting Point Determination

EXPERIMENTAL
A. Sample Used
The samples used in the experiment were
impure benzoic acid, its sublimate and the pure
benzoic acid. The impure benzoic acid is said to
be non-volatile meaning it has a lower vapor
pressure than the pure compound. The impurities
found in formed benzene affect it to quite a large

The 0.3213 g of sublimate collected was

ground with the mortar and pestle. The
sublimates powdered form was well-packed into
3-5 mm capillary tube. The pure benzoic acid
followed the same procedure separately with the
sublimate. The capillary tubes were dropped into
the glass tubing to get rid of air spaces when if
present could affect the melting point of the
compound. The closed ends of the capillary tubes

were attached to a thermometer with a thread,

rubber band or copper wire. The tubes are
aligned with the
mercury bulb of the
thermometer. After attaching, the tubes were
immersed in an oil bath while being heated. The
oil bath is stirred constantly. The temperatures at
which the sublimate and pure benzoic acid
started melting as well as the temperature at
which they were completely melted were both
noted.

RESULTS AND DISCUSSION

Sublimation was the process used in the
experiment. The impure benzoic acid in the
evaporating dish has to be heated to be able to
form needle-like crystals which will eventually be
called the sublimate. The sublimate that passed
through the holes of the paper used as its
covering is to be collected to know its percentage
recovery. It was noticed that during the process
of sublimation the impure benzoic acid did not
pass through the liquid phase. The reason for is
that because the benzoic acid has non-volatile
impurities. The impure benzoic acid is also said to
have lower vapour pressure than the pure ones.

Evaporating dish
Watch Glass with Moistened Tissue Paper
Hot plate

Figure 1. Sublimation set-up

The sublimate collected was ground to be able
to determine its melting point through the
capillary tube method with the use of oil bath.
The melting point determination in this
experiment was done through the oil bath. The
oil bath is a laboratory heating device which uses
boiling oil as the temperature regulator.[5] It
operates the same principle as water bath but oil

has generally far higher boiling points than water

Capillary Tube with the Sublimate
and can be used to provide temperature greater
than 100 C. [6]

Stirring Rod
Capillary Tube with Pure Benzoic Acid
Thermometer

Oil Bath

Bunsen burner

Figure 2. Melting Point Determination set-up

The melting point determination is the
temperature at which the material changes from
a solid to its liquid state. [7] Determining the
melting point is a simple and fast method used in many
diverse areas of chemistry to obtain a first impression of
the purity of a substance. This is because even small
quantities of impurities change the melting point, or at
least clearly enlarge its melting range.
Table 1. Data
Weight of the impure benzoic acid
Weight of the watch glass +

5.0014 g
3.7262 g

sublimate
Weight of the watch glass (empty)
Weight of the sublimate
Percentage Recovery
Melting Point of the pure benzoic

3.4049 g
0.3213 g
6.42 %
120 C

acid
Melting point of the sublimate

121 C
116 C

120 C
Through the data obtained from the
experiment, it showed how sublimation affected
the weight of the impure benzoic acid until it
became a sublimate. The change in weight (from
5.0014 g to 0.3213 g) showed the turning point
of the where in the impure benzoic acid is to its
gaseous state. The pure benzoic acid has a high
vapour pressure which made it melt in a higher
temperature rather than the sublimate. It has a

smaller dipole moment meaning the higher

vapour pressure due to lower electrostatic
attractive forces in the form of crystals.[1]

REFERENCES
Bayguen, A.V., Cruz, C.T., de Guia,
R.M, Lampa, F.F., Pea, G.T., Sarile, A.S.
and Torres, P.C. (2009),Laboratory Manual in
Organic Chemistry,C&E Publishing, Inc
Bruice, P. Y. (2006). The Essentials of Organic
Chemistry. 1st Edition. Pearson Education, Inc.
pp 74-82

Impure

Benzoic

Acid.

http://www.ehow.com/about_6629946_impurebenzoic-acid_.html#ixzz1TsXTSUBZ. 2010.

Meting

Point

Determination.

http://www.scribd.com/doc/48324739/meltingpoint-determination. March 2009.

Oil

Bath.

http://www.homechemistry.org/view/Oil_Bath
Feb 3 2011

Oil

Bath

as

Laboratory

Technique.

http://www.biologyonline.org/dictionary/Oil_bath. 2008.

Sublimation.

http://www.chemicool.com/definition/sublimation
.html. June 14 2007.