SUBLIMATION AND MELTING POINT DETERMINATION OF BENZOIC ACID

2D PH, Group 5, Mayo, P.L.C., Morales, A.C.C., Moroa, J.A.M., Ng, H.I.F., Ong, S.T.T., Panol,
M.V.C.F.
Department of Pharmacy, Faculty of Pharmacy, University of Santo Tomas
Espaa Boulevard, 1015 Manila, Philippines

ABSTRACT
Sublimation is a transition in the physical state from a solid phase to a gas phase, and it does not pass
through the liquid phase. This process is used as a purification method, and the purified substance
underwent melting point determination. The goals of the experiment are to purify the impure benzoic
acid, to know and compare the melting points of the pure and purified benzoic acid, and to calculate for
the percent recovery of the purified benzoic acid. The impure benzoic acid was exposed to heat to
sublimate, and the weight was computed for the percent recovery. The purified benzoic acid (sublimate)
and the pure benzoic acid, that is used as a standard, were placed on either sides of the thermometer and
determined its melting points in an oil bath. 10.1% of the benzoic acid was recovered from the impure
benzoic acid, and 1280C was the recorded temperature in which the sublimate has completely melted.

INTRODUCTION pure substance would be around one or two

Sublimation is a change in the physical state of a
substance from the solid phase to the gas phase,
not passing through the liquid phase. 1 It absorbs
heat as it changes and happens at temperatures
and pressures below the triple point, or the point
where the solid, liquid, and gas phases coincide
at an equilibrium.2 Sublimation works when a
solid compound is subjected to lower pressures,
which will result in the triple point, and will
directly change from the solid phase to the gas
phase.3 The molecules will only reposition, and
does not undergo chemical reaction. 4 Because of
the direct change, it is used as a purification
process. This process can happen if one of the
substances has a lower vapor pressure, or is non-
volatile, than the other substance.5
To test if a substance is pure or impure, melting
point determination is done. Symmetrical
compounds, like non-polar substances, are
compounds possessing high melting points and
vapor pressures. High vapor pressures are
caused by lower electrostatic attractive forces,
and would mean that there is a little dipole
moment.5 It is also the cause of the high melting
point of pure substances. The melting range of a
degrees, while an impure substance has the
capability to decrease or increase a melting
range.6 Thus, the purified sample should acquire
a higher and slight melting range than the
original sample.
The objectives of the experiments are: (1) to
purify benzoic acid by sublimation; (2) to
determine and to compare the melting point of
the product with a standard; and (3) to calculate
the percentage recovery. The substance to be
used in this experiment is the impure benzoic
acid, and it will be used for sublimation and
melting point determination.
METHODOLOGY
The materials needed for the experiment were
the following: a Bunsen burner, a beaker, a
watch glass, a perforated filter paper, an
evaporating dish, a mortar and pestle, a
thermometer, an iron stand and clamp, an iron
ring, a wire gauze, capillary tubes and masking
tape. Five (5) grams of impure benzoic acid
were weighed and placed in an evaporating dish.
The evaporating dish is then covered with the
perforated filter paper and covered again by the
preweighed watch glass. It was then placed on a
hot plate to heat. Wet tissue was set on the watch
glass so it would be cool. Ten (10) to fifteen (15)
minutes was allotted for the substance to heat
and to vaporize. After the allotted time, the setup
was removed from the hot plate and carefully
removed the watch glass and filter paper. The
sublimate was then collected, including the
crystals on the filter paper, and placed on the
watch glass to be weighed. The weight obtained
was then used to calculate the percent recovery.
FIGURE 3.1 Sublimation Set-Up
FIGURE 3.2 Melting Point Setup
To start the experiment for melting point
determination, the sublimate was triturated into a
fine powder. One group member closed one end
of a capillary tube, which is used as a container
for the sublimate. After triturating, the capillary
tube is pressed into the powdered sublimate and
is tapped on the table several times in order to be
packed around three (3) to five (5) millimeters.
The procedure was repeated this time with the
pure benzoic acid. The packed capillary tubes
are then secured to the thermometer near the
mercury bulb using masking tape. The
thermometer with the capillary tubes are
submersed into the oil bath to be heated.
Constant stirring is done in order to even out the
heat. The temperature is recorded when the
sublimate starts to melt and when it is
completely melted.
RESULTS AND DISCUSSION
Impure benzoic acid was in the form of white
powder before it was subjected to heat. When
placed on the hot plate, the heat aids the benzoic
acid to sublime faster. After the allotted time and
the setup was already cooled, the setup was
disassembled in the fume hood in order for the
crystals not to be blown away by air. The impure
benzoic acid became white, needle-like crystals
that adhere to the sides of the evaporating dish
and on the filter paper. The sublimate crystals
were weighed and was used to compute the
percent recovery.
recovery = ( weightweight of sublimate
of impurebenzoic acid )
x 100
recovery = ( 50.55 g g ) x 100
= 10.1%
The percent recovery is used for samples where
there is no chemical reaction involved. 7 In this
experiment, sublimation is a change in physical
state, so there is no chemical reaction in the
transition. The computed result shows that
10.1% of benzoic acid was recovered from the
impure one.
For melting point determination, the purified
benzoic acid and the standard were positioned
on either sides of the thermometer. Both
substances started to melt in 120 0C. The pure
benzoic acid was completely melted around
1240C, while the purified benzoic acid followed
at around 1280C. The theoretical melting point of
pure benzoic acid is around 122 0C.8 High
melting point records are a possible cause of
error because of the following: (1) the beaker
was not placed directly on the flame, and (2) the
wrong reading of the temperature.9
Sublimation is made possible if one of the
substances is nonvolatile, and that the vapor
pressure must be higher than the atmospheric
pressure. It is one of the methods of purification,
and the percent recovery is used to calculate for
the pure substance that sublimated from the
impure substance. On the other hand, melting
point is used as a guide if a substance is pure or
impure, and it can be determined by using an oil
bath so the temperature can increase over 100 0C.
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