1

CHEM 200L Experiment 1- 2JMT Group 1

SUBLIMATION AND BOILING POINT DETERMINATION
Abatay, B., Aniceto, S., Asenci, J.*, Babista, C., Ballesteros, E., Cadelia, K.
Department of Medical Technology, Faculty of Pharmacy
University of Santo Tomas
------------------------------------------------------------------------------------------------------------------------------ABSTRACT
Sublimation
condensing

the

is

the

vapors

process
to

of

again

vaporizing
form

the

solid
solid

substance
directly,

and
without

passing through an intermediate liquid state. The objective of the experiment is to be able to
demonstrate the sublimation process and the identification of the melting points of the sublimate
compared to the melting point of a standard. The sublimation process was done through heating of
impure benzoic acid inside an evaporating dish covered with a perforated filter paper and watch
glass, on the other hand, the melting point was determined through the use of an oil bath. The
experiment yielded a 9.86 % recovery of benzoic acid from impure benzoic acid and melting points
of

both

122oC.

------------------------------------------------------------------------------------------------------------------------------INTRODUCTION

depression is the reason why adding salt to

Sublimation is the conversion

frozen streets helps to melt the ice.

between the solid and the gaseous phases

The objectives of this experiment

of matter, with no intermediate liquid stage.

are: (1) to purify the impure benzoic acid

For those of us interested in the water

through

cycle, sublimation is most often used to

the melting points of the sublimate and the

describe the process of snow and ice

pure benzoic acid through the use of an oil

changing into water vapor in the air without

bath and (3) to calculate the percentage

first melting into water. The process of

recovery of the benzoic acid

sublimation,

(2)

to

identify

sublimation in this experiment is used to

purify the impure benzoic acid. Impure
benzoic acid contains the impurities phthalic
acid and benzyl benzoate.
of impurities in

The presence

a substance results

in

METHODOLOGY
During the process of sublimation,
the group placed a 5 g of impure benzoic

acid in an evaporating dish. On top of the

lower melting point due to a process called

filter paper was an inverted pre-weighed

melting point depression. Melting point

watch glass. The set-up was then secured

2
with masking tape and heated using a hot

When the sample was measured, it can

plate. A moist tissue paper was placed on

be observed that the impure benzoic acid

the center top of the watch glass. The set-

was a white powdered substance. To

up was heated for 10-15 minutes until most

separate the benzoic acid from the mixture,

of the sample has vaporized. After heating

a sublimation set-up was used as a

it, the set up was cooled and the pre-

purification method. As seen in Table 1, the

weighed watch glass was inverted. The

empty watch glass weight 49.4416 grams.

sublimate, including those adhering to the

After the sublimation process has been

perforated filter paper, was collected in the

done,

pre-weighed watch glass and weighed the

appearance of a spiky crystal structure

sublimate. The percentage recovery was

surrounding the inside of the watch glass.

then calculated using the data gathered.

The sublimate with the watch glass was

For melting point determination, the

the

collected

sample

had

the

weighed and had a mass of 49.9059 grams.

sublimate was grinded into a fine powder. A

The crystal-like sublimate was then

capillary tube was sealed using the Bunsen

collected, pulverized, and weighed which

burner. The open end of the capillary tube

yielded 0.4643 grams. It can also be

was used to place the powder inside it. The

observed

closed end of the capillary tube was

pulverization, is now an off-white powder.

dropped several times in the glass tubing

The percent recovery was calculated by

until it is well packed with 3-5mm of the

dividing the sublimate by the mass of the

sublimate. The capillary tube was then

impure benzoic acid then multiplying it to a

attached to the thermometer with a thread,

hundred, yielding 9.286% as seen in Table

that

the

sublimate,

aligning the closed end of the capillary tube

with the mercury bulb of the thermometer.
The capillary tube was immersed in an oil
bath and was heated and stirred constantly.
The temperature was observed at which the
sublimate starts to melt and when it is
completely melted
RESULTS AND DISCUSSION
1. Sublimation set-up and collection of
sublimates

2.
Table 1. Data
Name of Sample

Mass of substance
(g)

after

Impure benzoic acid

5.0000 g

sublimate

0.4643 g

Empty watch glass

49.4416 g

Watch

glass

with 49. 9059 g

sublimate

Computing for the Percentage Recovery

0.4643 g of Sublimate
x 100=
5.0000 g of Impure Benzoic acid
= 9.286%
2. Melting point determination
Now that the sublimate has been
pulverized into a fine power, a melting point
set-up

was

used

to

determine

what

temperature the sublimate would start to

melt and eventually evaporate. The melting
point of a substance is the temperature in
which it changes from a solid state to a
liquid state. Determining the melting point of
benzoic acid is important in this experiment
because what were used were both of
impure and pure samples. The sublimate
was compacted to a capillary tube until it
was filled 3mm high. The capillary tube was
then subjected to a hot oil bath. A hot oil
bath was used for this because unlike water
baths, oil baths can reach temperatures
higher than 100C. The sample was heated
until

signs

experiment

of
was

melting

showed.

completed

once

The
the

sublimate has completely evaporated from

the tube.
Table 3. Temperature of Sublimate

Sublimate

Temperature

Start

was at contact with the second distillate, the

distillate produced a bright orange flame.

0C

However, after a couple of minutes, the

Melting Point

122 C

flame went out. As the flame of the match

Completely Evaporated

143oC

was at contact with the last distillate, the

flame was extinguished.

When the sublimate started changing

phase, it was noted that the temperature

REFERENCES

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Determination of Its Melting Point. (n.d.).

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September

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Temperature

Start

0oC

Melting Point

122oC

Completely Evaporated

143oC

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