SUBLIMATION AND MELTING POINT DETERMINATION

Easabelle Demman E. Cabacungan, Glen Katrine L. Canlas, Joseph Edward C. Capiral,

Hazel Joy Krissen F. Capulong and Allyson Denise N. Carlos
Group 2 2J-Pharmacy Organic Chemistry Laboratory
ABSTRACT
Benzoic acid underwent sublimation, a type of change in phase when a matter converts from a solid state
to gas state without intermediate liquid state [1]. In the experiment, 5 grams of impure Benzoic acid was
sublimed. The crystals was collected using a capillary tube and the temperature was determined with the
use of oil bath and thermometer. Benzoic acids impure state was converted to its pure state. The
temperature was 112C to 118C. It was lower than expected.
INTRODUCTION
Sublimation is the process where a matter from
solid state undergoes a direct phase conversion
to gas phase without passing through the liquid
phase. It is an endothermic reaction [2]. This is
one of the kinds of phase transition of matter.
For the sublimation of Benzoic acid, the group
used an oil bath, evaporating dish, hot plate,
thermometer and capillary tubes.
The group aimed to (1) purify the benzoic acid,
(2) determine the melting point of the product
with the standard one, and (3) calculate the
percentage recovery of the Benzoic acid.
EXPERIMENTAL
A. Compound tested
The sample used was 5 grams of impure
Benzoic acid.
B. Procedure
1. Before Sublimation
Using a triple-beam balance, 5 grams of
impure benzoic acid was weighed and was placed
into an evaporating dish. It was covered with
perforated filter paper. Perforated paper is where
the vapors of the impure benzoic acid rise up or
passed through [3]. It is also covered watch glass
and was sealed all the openings by masking
paper.
A wet tissue paper was placed above the watch
glass to increase the condensation of the sample.
The evaporating dish was heated using a hot
plate. It was heated until the crystals was
formed.
2. Sublimation
The evaporating dish was placed into the hot
plate and the vapors of the impure benzoic acid
formed between the walls of the watch glass and
the perforated filter.
3. After Sublimation

The percentage recovery was computed by this

formula:

recovery =

Weight of the sublimate

100
Weight of theimpure benzoic acid

.1
100 =2
5
3. Before Melting Point Determination
The group collected the crystals and transferred
into the capillary tube. Capillary tube was sealed
at one end. The group prepared a Melting point
set-up. It is composed of the oil bath,
thermometer, iron stand, tripod, and Bunsen
burner.
4. Melting Point Determination
The capillary tube was filled with 2mm of
sublimate. Using a thread, the tube was attached
to the thermometer. The tube and the mercury
bulb of the thermometer were aligned together
and was submerged in an oil bath.

Fig.1 Sublimation Set-up. (A) Perforated filter is

where the vapors rise up. (B) Watch glass was
where the vapors were deposited. (C) Wet Tissue
paper to keep the set-up cool.

Fig.2 sealing of the capillary tube. (A) Bunsen

burner was used as the sealer. (B) Capillary Tube
was sealed at one end.

RESULTS AND DISCUSSION

Fig. 6 Data Gathered
Weight of the impure
benzoic acid

5 grams

Weight of watch glass

+ Sublimate

89.20g

Weight of the watch

glass

89.10 grams

Weight of sublimate

0.10 grams

Percentage recovery

2%

Melting point of
benzoic acid

(Starting)112C to
(End)118C

After performing the experiment, 0.10 grams was

collected from the 5 grams of the impure benzoic
acid. The percentage recovery was 2%, which
was computed by multiplying the quotient of
weight of sublimate and the weight of the impure
benzoic acid 100%. This data and result are not
free from errors. As you can see the melting
point of benzoic acid crystals are relatively low
(112C to 118C) was compared to the actual
temperature which is 122C [4].

Fig. 4 Melting Point Determination Set-up. (A)

Thermometer was attached with capillary tube
(B) Iron Stand (C) Beaker it contains the oil bath
(D) Oil Bath (E) Bunsen burner(F) Capillary
Tube(G) Tripod

SOURCES
From the internet
[1] Jones, A. Sublimation. Retrieved 01
September
2016
from
http://physics.about.com/od/glossary/g/sublimati
on.htm
[2] Jones, A. Sublimation. Retrieved 01
September
2016
from
http://physics.about.com/od/glossary/g/sublimati
on.htm
[3] Dash, D. (2011). Analytical Chemistry. PHI
Learning Pvt. Ltd.
[4] Science and Technology in action. Recrystallization
of Benzoic Acid and Determination of its Melting Point.
Retrieved
(N.D.),
From
http://sta.ie/lesson/recrystallisation-of-benzoic-acid-anddetermination-of-its-melting-point