SUBLIMATION AND MELTING POINT DETERMINATION OF BENZOIC ACID

University of Santo Tomas Faculty of Pharmacy; 2FPH Group 6

Pagaduan, Mikhaela; Pesito, Therese; Reyes, Thomas; Sarile, Criselda; Siapno; Yamilah;
Simsuangco, Paul
ABSTRACT
The aim of the past study was to evaluate the melting point of the product as well as to
establish the relationship of the product collected with a standard. Five grams (5.00 g) of
impure benzoic acid was heated and vaporized as the sublimate was collected thereafter. The
sublimate was weighed and the data was processed for a result of 24.00 % recovery of benzoic
acid.
To determine whether the sublimate was free from impurities, the experiment then moved on
to the melting point determination of the sublimate through the capillary method. The
collected sublimate as well as a sample of pure benzoic acid were packed in 2 capillary tubes
and was then bounded with a thermometer and immersed in an oil bath until further changes
in the physical state occurred. The recorded point of change of the impure benzoic acid started
at 130.00 C and ended at 131.00 C. On the other hand, the pure benzoic acid started at a later
131.00 C and quickly ended at 131.50 C. Upon deliberation, both of the tested samples were
between the ranges of 1C-2C which makes the sublimate closer to being qualified as a pure
substance. However the theoretical melting point of benzoic acid was 122.41 C. Upon
comparison, the data gathered were too far from the theoretical data, thus the product was
determined to be impure.
INTRODUCTION
Sublimation, in physics, conversion of a
substance from the solid to the vapour
state without its becoming liquid. An
example is the vaporization of frozen
carbon dioxide (dry ice) at ordinary
atmospheric pressure and temperature. The
phenomenon is the result of vapour
pressure and temperature relationships.
[1]

Melting point, temperature at which the
solid and liquid forms of a pure substance
can exist in equilibrium. As heat is applied
to a solid, its temperature will increase until
the melting point is reached. More heat
then will convert the solid into a liquid with
no temperature change. When all the solid
has melted, additional heat will raise the
temperature of the liquid. The melting
temperature of crystalline solids is a
characteristic figure and is used to identify
pure compounds and elements. Most
mixtures and amorphous solids melt over a
range of temperatures.
[2]

In this experiment, for the researchers to be
able to hypothetically collect pure benzoic
acid from the impure origin, the gathered
sample was vaporized and recollected the
sublimate. To test whether the sublimate
was pure, the researchers took advantage
of the melting point and was then tested
alongside with pure benzoic acid of equal
quantity. If the data gathered would be
between the ranges of 1 C to 2 C, the
researchers would then reach the
conclusion that the sublimate is pure or free
of any contamination. Otherwise, it would
then be concluded that it remained to be
impure due to its properties being
inconsistent with the standard substance.
At end of the experiment, the researchers
were able to grasp the following objectives:
(a) Collect benzoic acid from impure origin
through sublimation. (b) Evaluate the
percentage recovery of the collected
sublimate. (c) Deliberate whether the
sublimate still retained impure properties
or not by evaluating its melting point with a
pure sample of benzoic acid.
EXPERIMENTAL
The experiment began with the setup in
order to vaporize benzoic acid from the
impure origin. The materials and
instruments used for this phase of the
experiment were: hot plate, evaporating
dish, perforated filter paper, watch glass
(inverted; where the sublimate will be
gathered), masking tape (to temporarily
seal the watch glass and evaporating dish
together), and moistened tissue. Figure 1
shows the setup for this phase of the
experiment.

Five grams (5.00 g) of impure benzoic acid
was deposited in the evaporating dish,
following a layer of perforated filter paper,
and then a watch glass on top of the
evaporating dish and then sealed with
masking tape so as no vapor from benzoic
acid would escape. A layer of moist tissue
paper was applied on top of the watch glass
to cool down the vapors of benzoic acid and
quickly change its state as the sublimate on
the watch glass. The setup stood for a
length of 10-15 minutes at above 250.00 C
until most of the sample of impure benzoic
acid was vaporized on the hot plate. After
which, the setup was cooled and the
sublimate was collected and weighed from
the watch glass. Through the sublimates
computed weight, the researchers also
computed the sublimates percentage of
recovery and was then recorded.
On the next phase of the experiment, it had
a different setup for the capillary method of
determining the melting point. The capillary
method, see Figure 2 for setup, called for
the following materials: 2 capillary tubes (to
store the samples), thermometer (to
measure the melting point, an oil bath
setup where the samples were heated upon.

The sublimate of the impure benzoic acid
and pure benzoic acid were each grinded
and packed in a slightly modified capillary
tube with a sealed end. The capillary tubes,
along with the thermometer were
immersed into the oil bath and it was
observed as its temperature gradually rose
above 100.00 C, which makes the oil bath a
lot more convenient in this experiment than
water bath due to its higher heat capacity.
RESULT AND DISCUSSION
In the first phase, after subjecting the
sample of benzoic acid of impure origin to
vaporization, the heat changed the state of
benzoic acid into a gaseous state. As it
gradually accumulated through the
perforated filter paper and started to
solidify on the watch glass due to the moist
tissue paper which serves as the cooling
material which lowers the temperature of
the substances in sequential contact with it.
The researchers were able to collect 1.20 g
of sublimate from the original sample of
5.00 g thus as calculated:

The resulting percentage of recovery of
benzoic acid was 24.00 %. See Table 1 for
the results of the first phase of the
experiment (sublimation).
After which, the crystals were grinded and
packed in the capillary tube bounded on the
thermometer. It was subjected to heat and
the recorded results for the melting point of
the samples. The assumed pure sample
exhibited an average melting point of
approximately 1 C higher than the melting
point of the sublimate. However the
melting point was observed to be too far
from the theoretical melting point of
benzoic acid which is 122.41 C, thus the
experiment was deliberated that it
remained to be impure. See table 2 for the
results and observations for the melting
point.
Weight of impure
benzoic acid
5.00 g
Weight of empty
watch glass
52.00 g
Weight of watch
glass + sublimate
53.20 g
Weight of
sublimate
1.20 g
Percentage
Recovery
24.00 %
TABLE 1. Data and results collected
processed from sublimation
Initial
melting
Final
melting
temperature temperature
Sublimate
of benzoic
acid
130.00 C 131.00 C
Pure
benzoic
acid
(standard)
131.00 C 131.50 C
TABLE 2. RECORDED RESULTS FOR THE
INITIAL AND FINAL MELTING TEMPERATURE
CONCLUSION
From the final results, it could be said that
there had been an error that affected the
reliability of the final product
[4]
. It was
unusual for the pure sample of benzoic acid
to exhibit a melting point too high, way
higher than the original theoretical value. In
conclusion the possible errors that were
involved were: random error, due to
environmental factors that slightly
influenced the temperature upon the time
recorded; or measurement error due to the
device (thermometer) slope of reliability in
the empirical results.
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