Experiment 3: Sublimation and Melting Point Determination

2BMT, Group 3, Dy, N.D.G., Gurion, R., Hernandez, A.M., Isidro, D.J., Lopez, J. and Macababbad, E.M.
Department of Pharmacy, Faculty of Pharmacy, University of Santo Tomas,
Espaa Boulevard, 1015 Manila, Philippines

ABSTRACT
In this experiment, a sample of Benzoic acid was purified by method of sublimation. This process
involves turning the sample from its solid phase to its gaseous phase, without having to pass through the
liquid phase. After that, the sample was subjected to the vaporization-solidification cycle, which turned it
into small, needle-like crystals called the sublimate. Melting point was then determined by use of oil bath.
Results show that the sublimate starts to melt at 118 C and stops at 120 C, whilst the pure sample starts
to melt at 120 C and stops at 122 C, showing that the pure Benzoic acid has a slightly higher vapor
pressure as compared to the sublimate.

INTRODUCTION
Purification by sublimation is a chemical process
used to separate nonvolatile impurities from
volatile compounds. The process of sublimation
involves heating an organic compound so that it
goes from a solid phase to a gaseous or vapor state
without going through the liquid phase. This
sublimation process can be useful for the
purification of organic compounds, such as
camphor, salicylic acid and benzoic acid. However,
the process is utilized when the compound has
nonvolatile impurities. [1]
The melting point of a substance is the
temperature at which the substance changes from a
solid to a liquid state. Melting point is one way to
determine the purity of a substance, due to the fact
that even small quantities of impurities can affect a
substances melting point. [2]
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.

METHODOLOGY

To start the process of sublimation, 5g of impure

benzoic acid was weighed in a pre-weighed
evaporating dish and then covered with a
perforated filter paper. An inverted watch glass,
which was pre-weighed, masking tape was used to
keep it attached to the evaporating dish and to keep
any moisture from escaping. A moistened tissue
paper was put on top of the watch glass. It was
allowed to heat in a hot plate for 15 minutes. After
cooling it to room temperature, the sublimate found
in the inverted watch glass and perforated filter
paper were collected and weighed in the weighing
scale. From the data collected, the percentage
recovery was calculated. For determination of
melting point, the sublimate was ground into a fine
powder using a mortar and a pestle, after which it
was packed into a capillary tube. To ensure that the
powder is tightly packed together, the closed end of
the capillary tube was dropped several times in a
glass tubing until it was well-packed with 3-5mm
of the sublimate. A sample of pure benzoic acid
was also weighed and packed for reference. After
assembly of an oil bath setup, the capillary tubes
were then stuck to a thermometer with its closed
end attached to the mercury bulb of the
thermometer using a masking tape. Immersing the
capillary tubes into the bath, the samples heated up.
The temperature at which both compounds started
to melt and the temperature at which both
have completely melted was then recorded.

RESULTS AND DISCUSSION

Sublimation
Sublimation is employed as a means of
purification of certain substances, which are heated
in closed containers. In most cases, the temperature
does not exceed a low red heat. Dissociation often
occurs in the process. [3] Table 1 describes the data
needed to compute for the percentage recovery of
the collected sublimate.
.
Weight of impure

Benzoic acid
5.0 g
Weight of Watch glass
+ sublimate
57.3 g
Weight of Watch glass
(empty)
56.8 g
Weight of Sublimate
0.5 g
Table 1. Data collected from sublimation.
From the data collected, the percentage recovery
can be found using the formula:
%

Recovery

Weight of sublimate
100
Weight of impure Benzoic acid
0.5 g
% Recovery = 5.0 g

100

% Recovery = 10%
Impure benzoic acid, as the name implies, is the
crude form of benzoic acid. The impurities of this
crude form are phthalic acid and benzylbenzoate.
Computation of percentage recovery is essential
because it shows us how impure the substance was,
and how accurate we were in following the
procedures of purification.
Based on the results obtained from Table 1, and
from calculation of percentage recovery, it shows
than 90% of the initial sample was made up of
impurities.
Melting Point Determination
Melting point refers to the temperature at which a
substance turns from its solid phase to its liquid
phase. It is a simple and fast way to determine how
pure a substance is.
For this process, an oil bath was used instead of a
water bath, as waters boiling point is lower than
that of benzoic acid.

After immersion of the capillary tubes into the oil

bath set up, the temperature at which it melts was
recorded. Table 2 shows the temperature at which it
starts to melt, and where it stops.

1st reading

Temperature
2nd
Reading

Average

Pure
Benzoic
120C
122C
121C
acid
Sublimate
118C
120C
119C
Table 2. Data collected from melting point
determination.
Based on the data gathered, there is a 2 difference
between the standard melting point and the melting
point of the sublimate. This may be due to leftover
impurities from mishandling and contamination.

REFERENCES
Organic Laboratory Techniques. (n.d.). Retrieved
from
http://www.chem.ucalgary.ca/courses/351/l
aboratory/meltingpoint.pdf
Sublimation. (n.d.). Retrieved from
http://www.lenntech.com/chemistry/sublim
ation.htm
What is purification by sublimation? (n.d.).
Retrieved from reference.com:
https://www.reference.com/businessfinance/purification-sublimation9f27387ec9b5218