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PURIFICATION OF IMPURE BENZOIC ACID THROUGH SUBLIMATION AND

MELTING POINT DETERMINATION


ABSTRACT
Sublimation is a process by which the substance goes directly from solid to liquid
phase. It is a technique used in the recovery of compounds where the substance is subjected to
heat while covered with a watch glass and allowed to cool to enable the collection of the
sublimate. For the experiment, impure benzoic acid was subjected to sublimation producing a
sublimate. It was then collected and grinded into fine powder allowing it to be pushed into a
capillary tube. The sublimate was compared to pure benzoic acid by noting their melting points.
Using the gathered data, the percentage recovery was calculated which is 22%.
[1]

INTRODUCTION
[1]

Sublimation is the process by


which the substance goes directly from the
solid to gaseous state without passing
through the liquid state. [2] In this process,
certain energy must be transferred to the
substance via heat. The substances identity
and temperature is essential since the energy
needed to sublime the substance are
particular with these factors. There is a need
to (a)excite the solid substance so that it
reaches
its
maximum heat
(energy)
capacity in the solid state; (b) sever all the
intermolecular interactions holding the solid
substance together; (c) and excite the
unbonded atoms of the substance so that it
reaches its minimum heat capacity in the
gaseous state.

effective temperature can be characteristic of


the compound and can be measured using a
common hot plate.
Another factor touched is melting
point. Melting point is the temperature at
which the solid and liquid forms of a pure
substance can exist in equilibrium. This will
later help in accomplishing the objectives of
the experiment which are (1) to purify the
benzoic acid through sublimation; (2) to
determine and compare the melting point of
the product with a standard; (3)and to
compute for the percentage of pure benzoic
acid acquired from the sublimate.
[4]

[3]

Sublimation can be important in


the recovery of compounds that are
suspended or dissolved in a fluid or a solid.
By allowing the suspending matrix to
sublimate away, the compounds can be
recovered, at least in crude form. This
method of recovery is advantageous since it
preserves the chemical structure or even the
activity of the target drug or enzyme. Many
compounds will sublimate when heated. The

METHODOLOGY
Materials
The experiment made use of two setups namely the sublimation set-up and the
melting point set-up.
Methods

Sublimation set-up
Five (5) grams of impure benzoic
acid was placed in an evaporating dish and
covered with perforated filter paper. An
inverted pre-weighed watch glass was
placed on top and sealed with masking tape,
carefully making sure that no spaces were
left unsealed. A moistened tissue paper was
placed on top of the watch glass. The set-up
was placed on a hot plate and allowed to
heat for ten to fifteen (10-15) minutes until
most of the sample has vaporized and was
then cooled. The pre-weighed watch glass
was inverted and the sample was collected
and weighed. This allowed the percentage
yield to be calculated.

completely melted (represented by final


temperature).
Table 1. Melting Point
Sample
Pure benzoic
Acid
Sublimate

Initial
Temperature
124C

Final
Temperature
128C

104C

110C

Figure 1. Benzoic Acid

Melting Point set-up


Prior to testing, one end of the
capillary tube was sealed using a bunsen
burner. The sublimate was then grinded into
fine powder and placed in the open end of
the tube. The sample was moved to the
closed end of the capillary tube end by
tapping until it is well-packed, occupying 35 millimeters (mm) of the tube end. The
same was done with pure benzoic acid in
another capillary tube. Both of them were
attached to a thermometer and placed in an
oil bath where their melting points were
observed by taking note of the temperature
at the time they started to melt.
RESULTS AND DISCUSSION
The table below shows the temperature
when the sublimate and pure benzoic acid
started to melt (represented by initial
temperature) and the temperature when they

Figure 2. Sublimate
[5]

The melting point of pure benzoic


acid is 122.5C. Based on the melting point
of 122.5C, there is an error in the gathered
data regarding the purity of the sublimate.
The resulting melting point of the initial
(104C) and the final (110C) temperature
were far from the original melting point.
Therefore the group was not able to purify
the impure benzoic acid completely. This
could be attributed to either some
inconsistency during the process or human
error committed by the group.
From the data gathered, the
percentage recovery is 22% as shown by the
computation below:

% recovery =

Weight of

pure

from
Encyclopedia.com:http://www.enc
yclopedia.com/doc/1G23448300541.html

x 100

Weight of impure

% recovery= 1.1 g

x 100

[4]

Melting Point. Encyclopedia


Britannica.2015. Retrieved
October 10, 2015 from
http://www.britannica.com/search
?query=MELTING%20POINT

5g
% recovery= 22%
This indicates that the percentage of
pure benzoic acid in 5 grams of impure
benzoic acid is 22%.
In conclusion, the sublimate
collected was not pure since its melting
point (110C ) was too far from the pure
benzoic acid (122.5C).
REFERENCES
[1]

Zumdahl, S. (2012). Chemistry: An


Atoms
First Approach.
United States: Cole, Cengage
Learing.

[2]

Nakajima, K. (n.d.). Heat of Sublimation.


Retrieved from
http://chemwiki.ucdavis.edu/Physic
al_Chemistry/Thermodynamics/Sta
te_Functions/Enthalpy/Heat_of_Su
blimation

[3]

"Sublimation." World of Forensic Science.


2005. Retrieved October 10, 2015

[5]

Gilbert, J. and Martin, S.


(2015). Experimental Organic
Chemistry: A Miniscale &
Microscale Approach. Retrieved
from
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