Experiment #3: SUBLIMATION AND MELTING POINT DETERMINATION

Ronia Bianca G. De Leon, Jethro Kyle C. De Vera, Evan Paula F. De Villa,

Ayla Jania B. Dizon, Mark Kevin G. Flores and Bianca E. Gabagat
Group 3

2B Medical Technology

Organic Chemistry Laboratory

ABSTRACT
The purpose of this experiment is to teach the students how to determine the sublimation and melting point of a
certain compound. The students were asked to place 5 g of benzoic acid in an evaporating dish. After covering the
dish, it was heated using a hot plate. Then the students collected all the sublimate and weighed it. Sublimation occurs
when the vapor pressure of a liquid is greater than the atmospheric pressure. Since the vapor can solidify, sublimation
was used by the group as the purification process. The sublimate collected was colorless needle-like crystals. On the
other hand, melting point was determined through the set-up using an oil bath and thermometer. The melting point of
the sample was 122 degrees Celsius, close to the standard which is 122.41 degrees Celsius.

INTRODUCTION
The vapor pressure of a solid varies with its
temperature. There are some solids that can pass
directly into the vapor phase without going
through the liquid phase. Since the vapor can
solidify, the vaporization-solidification cycle can
be used as a purification process. The purification
can be done only if the impurities are non-volatile
or have significantly lower vapor pressure than
the pure compound.
Non-polar substances are symmetrical
compounds that have high melting points and
high vapor pressures. The ease by which a nonpolar substance can break away from the solid
state is determined by the strength of
intermolecular forces. Symmetrical compounds
have a relatively even distribution of electron
density and a small dipole moment. A smaller
dipole moment means a higher vapor pressure
due to lower electrostatic attractive forces in the
crystal.
If the vapor pressure is greater than the
atmospheric pressure at the melting point, the
solid will sublime. Sublimation is a technique
used to purify solid mixtures. Melting point

determination can be employed to ascertain the

identity and purity of an unknown compound.
The main objectives of this experiment are for
the group to be able to purify benzoic acid by
sublimation, determine and compare the melting
point of the product with a standard and be able
to calculate the percentage recovery at the end
of the experiment.

EXPERIMENTAL
A. Compound Tested
Sample: Benzoic Acid
Other names: Carboxybenzene; E210; Dracylic
acid; Phenylmethanoic acid; Benzenecarboxylic
acid
Chemical formula: C7H6O2
Chemical Structure:

thermometer. Afterwards, it was immersed in an

oil bath with constant stirring. The temperature
was monitored from the time the sublimate
started melting to the point it has completely
melted.

RESULTS & DISCUSSION

1. Sublimation
Functional group: carboxyl or carboxy group
Molar mass: 122.12g.mol-1
Melting point: 122.41C

Table 1: Data and Results for Sublimation

Appearance: colorless crystalline solid

Odor: faint, pleasant odor
Uses: widely used as a food preservative, topical
antiseptics, inhalant decongestants, anti-fungal
treatment and in the manufacture of various
cosmetics, dyes, plastics, and insect repellants.

B. Procedure

Variables Measured
Weight of Benzoic Acid (Impure)

Weight
5g

Weight of watch glass

59.70 g

Weight of watch glass w/ Sublimate

60.72 g

Weight of Sublimate

1.02 g

1. Sublimation Set-up
A sublimation set-up was used in this
experiment. Five grams of impure benzoic acid
was placed in an evaporating dish and covered
with a perforated filter paper. A watch glass was
weighed and placed on top of the evaporating
dish and secured tightly with masking tape so as
to avoid evaporation. A dampened tissue paper
was then put on top of the watch glass to help it
cool. The set-up was heated on a hot plate for
10-15 minutes until most of the sample had
vaporized. As soon as the set-up has cooled
down, the sublimate was collected from the
watch glass and from the filter paper. The
sublimate was weighed after collection.
For the melting point determination, the
sublimate was ground into fine powder and put
into the open end of a capillary tube with one end
sealed using a Bunsen burner about 3-5mm down
the tube. The capillary tube was attached to a
thermometer with a thread. The closed end was
aligned with the mercury bulb of the

Formulae and Computations:

Weight of Sublimate= 1.02 g

= 60.72g 59.70g
= 1.02g

To compute for the weight of the sublimate,

the weight of the watch glass, 59.70g, was
subtracted to the weight of watch glass with the
sublimate, 60.72g that yields 1.02g. Thus, the
weight of the sublimate is 1.02g.

point is greater than that of water. Thus, it

provides a higher temperature and boiling point
for the setup.

Table 2. Percentage Recovery

From the data, the melting range of the impure

benzoic acid was quite far to each other (10C).
Result

Percentage recovery is the percentage of pure

substance extracted from the impure substance.
The percentage recovery of the sublimate was
computed by dividing 1.02g, the weight of
sublimate over 5g, weight of the impure benzoic
acid. The quotient was then multiplied to 100 to
get the percentage. The percentage recovery of
the sublimate was 20.4% which meant that
20.4% of the benzoic acid was recovered from
the 5 g impure benzoic acid. Having a high
percentage recovery meant that the substance
was close to being pure, if not completely pure.

2. Melting Point Determination

Table 3: Data and Results for Melting Point

Determination

Substances
Benzoic Acid

1st
Temperature

2nd
Temperature

118 C

122 C

Percentage Recovery

20.4 %

The sublimate produced is still impure for the

difference in its initial and final melting point is
greater than 2C. Thus, this proved that melting
point determination would help in determining if
the purification was successful.
Pure samples usually have sharp melting points
(a melting range of less than about 1C); impure
samples of the same compounds melt at lower
temperatures and over a wider range.
Various sources of error couldve affected the
purification of the impure benzoic acid. First, was
that not all of the crystals of sublimate had been
recovered. Second, was the substances in the
capillary tubes were too coarse, they did not pack
well, causing air pockets to slow heat transfer.
Another one could be not all of the impure
benzoic acid had gone into the process of
sublimation.

REFERENCES
Bathan, G., Bayquen, A., Crisostomo, A.B., et.
Al. (2014) Laboratory Manual in Organic
Chemistry. Quezon City: C&E Publishing Inc.

(n.d.).Retrieved from
At 118C, the sublimate started to melt and it
completely melted at 122C. Oil bath was
preferred in this experiment because its melting

https://en.wikipedia.org/wiki/Benzoic_acid