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Sublimation and Melting Point Determination

C.P. Espinola, E. Galamiton, K.D. Geronimo, A.C. Greas, J.N. Guce, O. Icamen
Group 3, 2FPH, Faculty of Pharmacy, University of Santo Tomas, Espaa, Manila

ABSTRACT
In this experiment, the process of sublimation was used to decontaminate the solid mixtures. Sublimation is the practice of vaporizing a solid material
and condensing the vapors to again form the solid directly, without passing through an intermediate liquid state. Impure benzoic acid was the compound
used to undergo purification. The sublimate was the product attained subsequently the heating process in the form of crystals. Impure benzoic acid and
the sublimate weighed 5.00 grams and 3.80 grams, respectively. Consequently, it lead to a low percentage recovery of the compound. Through the oil
bath, the sublimate was formerly exposed to melting point determination together with the pure benzoic acid. The oil bath was used since its initial
boiling point is more than 100C, hence can be used for temperatures above 100C and vapor generated by oil are less as compared to water at normal
working temperatures. As things go for the melting point determination, the sublimate started to liquefy at 117C and stopped melting at the temperature
of 123C while the pure benzoic acid started to melt at 121C and completed at 123C. Generalized, the temperature gathered specified that the
sublimate has a lower vapor pressure compared to the pure benzoic acid.

I.

Introduction
II.
III. As with liquids and gases, intermolecular forces
determine the physical properties of solids. The
melting point of a solid is simply the temperature at
which the crystal lattice is disrupted, and the solid
changes to a liquid. The energy that must be added
to the solid in order to melt it is called the enthalpy of
fusion. The enthalpy of fusion of a solid is directly
proportional to melting point--the more energy
required to melt a solid, the higher the melting point.
IV. Sublimation is the transition of a solid directly to
a gas, or vice versa. This behavior is most
commonly associated with carbon dioxide and dry
ice.1
V.
VI. Sublimation is a process where some solids can
pass directly to vapor without passing through liquid
phase. It is technique used to purify compounds. In
the experiment, it was used to purify impure benzoic
acid. Melting point determination can be employed to
ascertain the identity and purity of the unknown
compound. In the experiment, the powdered
sublimate and pure benzoic acid was placed in an oil
bath to determine their melting point.2
VII.
VIII.Crystallization is a process of formation of solid
crystals precipitating from a solution that is melted or
more rarely deposited directly from a gas. It is also
an aspect of precipitation obtained through a
variation of the solubility conditions of the solute in
the solvent.
IX.
X. Benzoic acid is an aromatic monocarboxylic
acid. It is a solid with sublimation point of greater
than or equal to 100C.
XI.
XII. The objectives of the experiment are: (1) purify
benzoic acid by sublimation, (2) determine and
compare the melting point of the product with a
standard, and (3) calculate the percentage recovery.
XIII.
XIV.

XV.
XVI.
Methodology
XVII.
1. Preparation of the capillary tubes
XVIII.
XIX.
On the blue side of the capillary tube,
heat one end by means of Bunsen burner. Even
though heating one end of the capillary tube, take
tums to make it even. Remain heating it until the
other end of capillary tube is thoroughly locked.
XX.

Figure 2.1 Heating of capillary tube


XXII.
2. Preparation of the hot-oil bath set-up
XXIII.
XXIV.
In a clean 250 mL beaker, place unused
cooking oil (Canola Oil) about half-full. Position the
beaker on top of a tripod with a wire gauzed and a
Bunsen burner underneath it. Fasten the
thermometer in a clamp and submerge it with the
capillary tubes in the oil bath.
XXI.

XXV.

XXVI.

Figure 2.2 Experimental set-up


XXVII.

3. Purification of the Benzoic acid


XXVIII.

XXIX.
The 5.00 grams of impure benzoic acid
was placed in an evaporating dish. It was covered
with a perforated filter paper. Above the filter paper,
an inverted tared watch glass was positioned. The
substance was heated using a hot plate and cooled
at the center top of a watch glass with a wet tissue
paper kept moist with water using a dropping
pipette. Let it stand for 10 to 15 minutes until most
of the sample has vaporized. End the heating
process and proceed in cooling the set-up.

XXXVIII.

Figure 2.4 Collected sublimate

4. Determining of Melting Point


XXXIX.
XL.
The sublimate was triturated using the
mortar and pestle into a fine powder.
XLI.
Figure 2.5 Trituration of sublimate

XXX.

XLII.

XXXI.

Figure 2.3 Heating of impure benzoic


acid and formation of crystals
XXXII.

XXXIII.
The tared watch glass was cautiously
upturned and the sublimate was collected and
weighed in a triple beam balance. Determine the
percentage recovery.
XXXIV.
XXXV.
XXXVI.
XXXVII.

XLIII.
The capillary tube was pushed in the
open end into the powder and was released in the
close end down through a glass tubing a number of
times until it is compacted with a 1 centimeter of the
sublimate.
XLIV.
Figure 2.6 Filling of powder in the tubes

XLV.
The capillary tube was attached to a
thermometer with a piece of rubber band or a
thread line up to the close end of the capillary tube
with the mercury bulb of the thermometer. At that
juncture, it was dipped in an oil bath and heated.
The temperatures were recorded at which the
sublimate took place to melt and entirely melted.
XLVI.
Figure 2.7 Heating of the sublimate

LXI. Table 3.1 Variables used for determining the


percentage recovery

LXII.

Weight
of
Impure
Benzoi
c Acid
LXIV. Weight
of the
Watch
Glass +
Sublim
ate
LXVI. Weight
of the
Watch
Glass
(empty)
LXVIII. Weight
of the
Sublim
ate
LXX. Percent
age
Recove
ry

XLVII.

XLVIII. Results and Discussion


XLIX.
1. Formation of crystals
L.
LI. The impure benzoic acid formed needle-like
crystals after being heated in the evaporating dish
which became the sublimate. It has a non-volatile
impurity and has a lower vapor pressure than a
pure benzoic acid that is why it did not pass through
a liquid phase during the sublimation.
LII.
2. Factors that may affect the purity of the benzoic
acid
LIII.
The purity of recrystallized material
obtained depends on several factors: the original
extent of contamination, the relative solubilitys of
the desired compound versus the contaminant, the
rate of crystallization, and the final temperature of
the crystallization.

LXIII.

5.00g

LXV.

92.00g

LXVII. 88.20g

LXIX.

3.80g

LXXI.

76%

LXXII.
LXXIII.

Percentage Recovery:

LXXIV.

Recovery

weight of sublimate
x 100
weight of benzoic acid

( g watch glass+benzoic )( g watch glass)


x 100
weight of benzoic
LXXV.

(3.8 g)
x 100
(5.00 g)

LXXVI.

LXXVIII.

= 76% recovery

LIV.
LV.
LVI.
LVII.
LVIII.

LXXVII.

LXXIX.
A percentage recovery of 76% is
obtained after computing the ratio weight of
sublimate and weight of impure benzoic acid
multiplied by 100.

LIX.
LX. The data gathered from the experiment are:

LXXX.
Oil bath was used because it does not
evaporate and it can be heated to a much higher

temperatures especially for experiments that require


temperatures greater than 100oC.
LXXXI.
The melting point of the sublimate is
higher than the melting point of pure benzoic acid. A
pure substance has a fixed melting point and has a
range of 1oC to 2oC. On the other hand, the
sublimate has a melting point of wider range.
LXXXII.
are:

The data gathered from the experiment

LXXXIII.

Table 3.2 Temperatures of benzoic acid

LXXXIV.

LXXXVII.

XC.

LXXXV.P
u
r
e
LXXXVIII.
121C
XCI.
1
2
3

LXXXVI.
Impure

LXXXIX.
117C
XCII. 1
2
3

XCIII.
XCIV.
XCV.
XCVI. Conclusion
XCVII.
XCVIII.
The students concluded that sublimation
can be used to purify and remove unwanted
substance/s in a solution. It is shown in the results
that there is a difference between the melting point
of pure and impure benzoic acid. The reason why
there is a difference in the melting point of pure and

impure benzoic acid is because the melting point of


the
impurities
namely
phthalic
acid
and
benzylbenzoate exists in the compound and they
have a higher melting point than the benzoic
acid.3 The percentage recovery indicates the
percentage of pure substance extracted from the
impure substance.4 The results show that the
percentage recovery is 76%. This implies that the
higher the percentage recovery, the purer the
substance is.
XCIX.
C.
References
CI.
CII. [2] Bathan, G.I., Bayquen, A.V., Crisostomo,
A.B.C., Cruz, C.T., De Guia, R.M., Farrow, F.L.,
Pea, G.T., Sarile, A.S. & Torres, P.C. (2014).
Laboratory Manual in Organic Chemistry. Manila:
C&E Publishing, Inc. p.37-39
CIII.
[1] [No author mentioned] Melting and
Sublimation
CIV.
https://cssac.unc.edu/programs/learning
-center/Resources/Study/Guides/Chemistry
%20102/Melting%20and%20Sublimation
CV. [3] [No author mentioned] Why does melting
point of impure benzoic acid is higher than that of
the pure benzoic acid?
CVI.
https://www.researchgate.net/post/Why_
does_melting_point_of_impure_benzoic_acid_is_hig
her_than_that_of_the_pure_benzoic_acid
CVII.
[4]
[No
author
mentioned]
Recrystallization of Benzoic Acid and Determination
of its Melting Point
CVIII.
http://editions.sciencetechnologyaction.c
om/lessons/2/26/GSK-lesson.pdf
CIX.
[5] Sayfa, A. (2011). Crystallization and
Sublimation
http://muglaengineering.blogspot.com/2011/12/cryst
allisation-and-sublimation.html