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Sublimation and Melting Point Determination

Adolfo, Angela Nicole G., Alcaraz, Frances Jillian F.
Aliman, Stephanie T., Astor, Jashmin D.
Bauzon, Franchesca D., Cabral, Danica Rose G.
Department of Pharmacy, Faculty of Pharmacy
University of Santo Tomas

ABSTRACT
The sample of benzoic acid was purified through sublimation. This process occurs if
the vapor pressure of a substance is greater than the atmospheric pressure. The product
obtained after the heating process is called a sublimate, and it is in the form of needlelike crystals. For the melting point determination, the sublimated was grinded into a fine
powder and a small tube was pressed into it. Pure benzoic acid was also pressed into
the tube for comparative reasons. The two capillary tubes together with the thermometer
was immersed in an oil bath and was heated. The oil bath was used since it is able to
withstand temperatures exceeding 100 and is therefore able to measure more
accurately.
than the pure compound.
INTRODUCTION

In this experiment, sublimation is

Sublimation is a process of direct

used to purify the crude form benzoic acid

vaporization of solids without passing

which is impure. It has amino compounds

through the liquid state. Also, it will occur

which must be removed because it

in solids only if the vapor pressure is

contains phenyl and benzyl compounds

greater than the atmospheric pressure at

that can affect the product. Moreover,

the melting point. The vaporization-

there is the process of melting point

solidification cycle can be used as a

determination to ascertain the identity and

purification process which is applicable

purity of an unkown compound that

only if the impurities are non-volatile or

should be done together with sublimation.

have significantly lower vapor pressure

The following are the objectives to be

achieved by the group:

tubing. Pure benzoic acid was also

weighed and well-packed in capillary

1) to use the process of sublimation to

tubes to serve as a standard of reference.

purify the impure benzoic acid

The capillary tubes were then attached to

2) to determine and compare the melting

a thermometer using a thread, the closed

points of the sublimate and the pure

end attached to the mercury bulb of the

benzoic acid

thermometer. An oil bath setup was then

3) to calculate the percentage recovery of

assembled, where the capillary tubes will

the benzoic acid

be immersed, and then it was put into

heat.

METHODOLOGY

The

students

recorded

the

temperature at which both compounds

started to melt and the temperature at

First a sublimation setup was used to

which both has completely melted.

purify the benzoic acid, place 5g of

impure benzoic acid in an evaporating

RESULTS AND DISCUSSION

dish covered with a perforated filter paper

and a pre-weighed inverted watch glass,

Table 1. Data and Results

fastened it using a masking tape to serve

Weight of impure

as a cover. Heat it on a hot plate for 15

benzoic acid
Weight of watch

5g

glass + sublimate
Weight of watch

94 g

glass (empty)
Weight of sublimate

93.5 g

minutes, while dabbing a moistened

tissue paper on top of the watch glass.
Allow it to cool after to room temperature,
then collect the sublimate found in the
watch glass and perforated filter paper,

0.5 g

weigh it in the same weighing scale used

Percentage

to weighing the pre-weighed watch glass

recovery
Melting point of

10%

benzoic acid

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used

in

percentage

the

setup.

recovery

Calculate
from

the

the
data

collected.
For the determination of melting
point, the sublimate was packed into a
capillary tube, and to ensure that it is
tightly packed together the capillary tube
was dropped for several times in a glass

Table 2. Melting Points

Temperature

Temperatur

e2

Sublimate

21

22

Standard

19

22

the standard in order to compare their

melting points. The standard began to
melt at 21 and it completely melted at

CALCULATIONS

22. The sample began to melt at 19

and it completely melted at 22.

mass of sublimate
% recovery =
x 100
mass of sample

CONCLUSION
Sublimation method is very

= x 100

0.5 g
5g

= 10%
Discussion

effective for purifying substances in small

quantities because there's a very little
loss of the material in the process. Based
on the gathered date and results of the
experiment yielded a lower result

The benzoic acid (the sublimate) was

for the percentage recovery. This maybe

heated on a hot plate, and solidified into

because of the small amount of crystals

crystalline forms after approximately 15

or sublimate collected within the process

minutes. This was due to the vapor of the

of sublimation. Longer time for the

benzoic acid acting upon the heat and

process to occur is needed so enough

proceeding into the sublimation phase.

and more sublimate will be gathered.

The 0.5 g of the benzoic acid that was

collected from the previous 5.0 g of

In melting point determination,

benzoic acid sample will be used to

experiment shows that the sublimate is

compute for the percentage recovery of

still not that pure but is close to being a

the substance, which resulted in 10%.

pure benzoic acid, because the range of

The colorless needle-like crystals were

2C indicates a pure substance but the

later grinded on to be able to insert it into

collected sublimate has a range of 4C.

the capillary tubes. The grinded crystals

Factors that might affect the experiment

are then inserted into the capillary tube

included loss vapor due to poor

attached to a thermometer, which was

sublimation set-up or inaccurate

later subjected to a hot oil bath which was

measurements of the substances.

used to melt the substance together with

REFERENCES

The University of North Carolina at Chapel Hill (2014). Melting and sublimation.
Retrievedfrom
https://cssac.unc.edu/programs/learningcenter/Resources/Study/Guides/Chemistry%20102/Melting%20and%20Sublimation

The Wired Chemist (2016). Determination of melting point. Retrieved from

http://www.wiredchemist.com/chemistry/instructional/laboratory-tutorials/determinationof-melting-point
DOCUMENTATION

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