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SUBLIMATION AND MELTING POINT DETERMINATION OF BENZOIC ACID

ABSTRACT
This experiment was conducted to determine the purity of benzoic acid through sublimation and melting
point determination using its crude form, impure benzoic acid. The sample of impure benzoic acid was first
sublimated, wherein crystals were formed and observed in the watch glass covering the evaporating dish
with the perforated filter paper after heating. The crystals (sublimate) were then collected. The sublimate
and the pure benzoic acid are then individually packed in capillary tubes, which are used to determine the
melting point of the substance through the use of an oil bath. The melting point of the impure benzoic acid
obtained from the experiment was then compared to the standard value of the melting point of the pure
benzoic acid, which is in the range of 122-124C.

INTRODUCTION
Sublimation, in chemistry, is the transition of a
substance directly from the solid phase to the gas
phase without passing through an intermediate
liquid phase. The vapor, which is in the gaseous
phase, can solidify, making sublimation a
purification process. Sublimation can then be
classified as a purification technique for solid
mixtures. Sublimation however, is limited to
impurities that are non-volatile or have a lower
vapor pressure than the pure compound.
Sublimation however, is not limited to its
purification properties. It is also used to describe
the reverse process, meaning gas changing back
to solid state upon cooling. Melting point
determination
is
often
associated
with
sublimation especially when trying to test the
purity of the substance or compound.
Melting point is the temperature at which a
solid changes to liquid at atmospheric pressure.
Meaning the solid and liquid phases of a
substance coexist in equilibrium. The melting
point of benzoic acid is higher than the boiling
point if water, that is why an oil bath was used in
the experiment.
There was only one compound used in the
experiment, and that is Benzoic Acid. Also known
as Dracylic acid or Benzeneformic acid.
Considered as the simplest aromatic carboxylic
acid containing carboxyl group bonded directly to
a benzene ring. Benzoic acid is a white crystalline
organic compound that has a boiling point of
247C and a melting point of 122C.

Structure of Benzoic Acid


It is an organic compound that occurs naturally
in numerous plants and resins. Benzoic acids has
many uses, it is used a microbial agent in

toothpastes,
mouthwashes,
deodorants and the like.

cosmetics,

As stated earlier, the crude form of Benzoic


acid, which is impure benzoic acid, was used in
the experiment. Benzoic acid is formed from the
oxidation of toluene, the oxidation process can
only be carried out in liquid phase and with the
presence of a catalyst. The newly formed
benzene then contains impurities due to the
presence of benzyl and phenyl, which affect the
product.
The objective of this experiment or study is to
purify benzoic acid by sublimation, determine and
compare the melting point of the product with a
standard and to calculate the percentage
recovery.

EXPERIMENTAL
A. Compounds tested
5.0g Benzoic Acid (impure)
Benzoic Acid (Pure)
B. Procedure
1. Preparation of Capillary Tubes
Two capillary tubes are prepared and one of the
ends of each tube is heated using a Bunsen
burner to seal it. While heating one end of each
of the capillary tubes, the tube was rotated to
make the seal even. It was heated continuously
until the capillary tube was totally sealed.
2. Preparation of Impure Benzoic Acid
Sublimate (Sublimation)
5g of impure benzoic acid was placed in an
evaporating dish and the dish was covered with a
perforated filter paper and an inverted preweighed watch glass was placed on top of the
filter paper and then heated in a hot plate for 1015 minutes.

Table 1. Data and Results


1. Weight of the impure benzoic acid

2. Weight of the watch glass + sublimate

3. Placing of Pure and Impure Benzoic acid


in Capillary tubes
The sublimate that was collected was grinded
into a fine powder and then placed in one of
the capillary tubes. The closed end of the
capillary tube was dropped down through a
glass tubing several times until the tube was
well packed with 3-5mm of the sublimate.
The same process was done in filling the
other capillary with the pure benzoic acid.
4. Melting Point Determination
An oil bath was prepared and the capillary
tubes were attached to the end of a
thermometer with a piece of thread. The
thermometer was then immersed in the oil
bath and heated. The temperatures at which
the sublimate and the pure benzoic acid start
to melt and completely melted were then
recorded.

3. Weight of watch glass (empty)

5.0g

94.57g

94.0485g

4. Weight of the sublimate

0.5215g

5. Percentage recovery

10.43%

Table 1 includes all the data needed for the


computation of percentage recovery of benzoic
acid after the sublimation process.
Computations for Percentage Recovery:
% Recovery = Weight of Sublimate x 100
Weight of Impure Benzoic Acid
% Recovery = 0.5215 g x 100
5g
% Recovery = 10.43%
Table 2 represents the melting points of the pure and
impure benzoic acid. Temperature 1 being the
temperature that they start to melt and temperature 2
being the temperature at which they are completely
melted.
Table 2. Melting Points

Figure 3: Melting point determination using


oil bath

RESULTS AND DISCUSSION

Pure

Sublimate

Temperature 1

110C

112C

Temperature 2

114C

118C

After subjecting the pure benzoic acid and


the impure benzoic acid (sublimate) in the
following procedures, here is the list of data
that
was
gathered
throughout
the
experimenting process:

REFERENCES

[1]http://en.wikipedia.org/wiki/Sublimation_(pha
se_transition)

[2]http://www.infoplease.com/encyclopedia/scie
nce/sublimation-chemistry.html
[3] http://www.ehow.com

[4] http://orgchem.colorado.edu/
[5]
http://physics.about.com/od/gloassary/g/sublima
tion.htm
[6] http://www.chemicalland21.com
Books:

Bayquen A. (2009). Laboratory Manual in


Organic Chemistry. Quezon City. C&E Publishing,
Inc.
Whitten, Davis, Peck, Stanley (2010). Chemistry.
9th Edition. USA: Brooks/Cole