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Sublimation and Melting Point Determination

Mheriz Drona, MaiahDinglasan, Lourdes Domingo, Diane Dyjongco, Princess ArasherEspolong, Alex Estanislao

Abstract
This study focused on the determination and comparison of the melting point of the product
with a standard. Specifically, it aimed to purify benzoic acid by sublimation and calculate its
percentage recovery.
The group was assigned to prepare five grams of benzoic acid for sublimation. After the
sublimation set-up was assembled, the sample was heated for 10-15 minutes until most of the
sample has vaporized and allowed to cool down. The sublimate was collected in the preweighed watch glass and weighed. The percentage recovery of the sublimate was calculated.
For melting determination, the sublimate and standard was grinded into a fine powder and putin
separate capillary tube. The capillary tube was attached to the thermometer with a piece of
thread. It is also immersed in an oil bath and heated. The temperature at which the sublimate
starts to melt and completely melted was recorded.

Introduction
Sublimation is the transition from solid
phase to the gas phase without passing
through an intermediate liquid phase. The
term is also used to describe the reverse
process of the gas changing directly to the
solid again upon cooling. Sublimation also
occurs when air saturated with water vapor
is suddenly cooled below the freezing point
of water. Frost and snowflakes are thus
formed by water changing directly from the
gaseous to the solid state. In sublimation,
sublimate is collected. Sublimate is the
purified form of the sample. The limitations
of sublimation as a purification method is
not as selective as crystallization, it typically
requires a vacuum and usually requires that
the compound you are trying to separate is
volatile, while everything else in the mixture
is not volatile.
Melting point is the temperature at which
solid becomes a liquid at a fixed pressure,

usually standard pressure. In this study, oil


bath was used for the melting point
determination. Oil bath is preferable
because initial boiling point of oil used is
more than 100C, hence can be used for
temperatures above 100C. Also, the vapor
generated by oil is less as compared to
water at normal working temperature. The
oil has less chance of exposure to the latent
heat of water. Lastly, it is relatively uniform
use in temperature.
The study aimed to purify the benzoic acid
by sublimation, determine and compare the
melting point of the product with a standard,
and calculate its percentage recovery.

Experimental and Procedures


A. Compounds Tested
An impure and pure benzoic acid was used
in sublimation and melting point
determination.

B. Procedure
In the process of sublimation, a 5g of
impure benzoic acid was placed in an
evaporating dish. The dish was covered
with a perforated filter paper. On top of the
filter paper, an inverted pre-weighed watch
glass was placed. All the opening was
sealed with masking tape. It was heated
using a hot plate. A tissue paper kept moist
with water was placed on the top of the
watch glass. The heating was continued for
10-15 minutes until most of the sample has
vaporized. After heating, the set-up was
allowed to cool. Watch glass was carefully
inverted. Sublimate (including the crystals
adhering to the perforated filter paper) was
collected. The mass of the sublimate and
standard was recorded to compute the
percentage recovery.

drop down through glass tubing several


times until it was well-packed with 3-5mm of
the sublimate. Then, the capillary tube was
attached to a thermometer with a piece of
thread. The closed end was aligned with the
mercury bulb of the thermometer. Lastly,
capillary tubes was immersed in an oil bath
and heated. The temperature at which the
sublimate starts and when it is completely
melted was recorded.

Results and Discussion


After all of the procedures, 1g of sublimate
was collected from 5g of impure benzoic
acid. A percentage recovery as computed
after getting the weight of the sublimate and
impure benzoic acid then multiply it by 100.
Weight of impure benzoic acid
Weight of the watch glass + sublimate
Weight of the watch glass (empty)
Weight of the sublimate
For melting point determination, the
sublimate was grinded into a fine powder.
One end of the capillary tube was sealed
using a Bunsen burner. The open end of the
capillary tube was pressed into the powder.
The closed end of the capillary tube was

The above table shows the values gathered


from the experiment. These values were
then used to compute for the percentage
recovery.

90g +
9

point of the benzoic acid has a range of


120C-128C.

Conclusion

Percentage recovery = wt of sublimate


wt of benzoic acid

= 1g/5g x 100
= 20%
The melting point of the benzoic acid was
also obtained. The group discovered that it
is necessary to grind the sample so that it
will form a fine powder for melting point
determination as its standard operating
procedure, no matter how the solid is
obtained. This allows the efficient and
uniform packaging in the capillary tube. It
was also discovered that the sublimate
should be pack uniformly because any large
dead air spaces will cause non-uniform heat
transfer within the tube. This causes some
parts of the sample to melt before the
others, resulting poor reproducibility.
A well-packed tube will melt almost all at
one to gain a sharp, reproducible melting
point.
T
T
Sublimate
120C
128C
Pure Benzoic
121C
125C
Acid
At 120C, the sublimate started to melt and
it completely melted at 128C. On the other
hand, the pure benzoic acid started to melt
at 121C and completely melted at 125C.
Based on the data obtained, the melting

Sublimation is an effective way for purifying


substances in small quantities. The
percentage recovery of the sublimate may
determine if the substance produced was
pure or not. As seen in the results, the
experiment yielded a lower result for the
percentage recovery. This maybe due to
fewer crystals or sublimate collected within
the process of sublimation. Moreover, the
melting point can also be a criterion of
purity.

References
[1] http://study.com/academy/lesson/what-issublimation-in-chemistry-definition-processexamples.html
[2]http://www.infoplease.com/encyclopedia/sci
ence/sublimation-chemistry.html
[3]http://ochemwonderstudents.wikispaces.co
m/SublimationLab
[4]http://www.scribd.com/doc/106152244/Subli
mation-and-Melting-Point-Determination
[5] Bathan, G. et al. (2014). Laboratory
Manual in Organic Chemistry. Quezon City:
C&E Publishing,Inc.

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