Experiment 1 (Simple and Fractional Distillation)

1
Simple and Fractional Distillation

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
Distillation is one of the oldest and still most common methods for both the
purification and the identification of organic liquids. It is a physical process used to
separate chemicals from a mixture by the difference in how easily they vaporize. The
experiment used the Simple Distillation Method to separate the components of 30 mL
alcohol (vodka) and water. The distillate was collected with the aid of a calibrated test
tube (0.5 mL) until it reaches the temperature of 99 C. Also, the first, second and last
distillate were used for testing the presence of alcohol. Throughout the process, there is
a directly proportional relationship between the volume and temperature of the distillate.
In the flammability test, the first and second distillate shows the presence of alcohol
while the last one is not flammable at all. With the records obtained, a graph between
the volume and temperature of distillate was plotted and the percentage of alcohol and
percentage loss were also computed. Thus, simple distillation is not a so much complex
process of extraction and purifying liquids. Heating and vaporization are just the 2 major
process used to separate the components of alcohol (vodka) and water.
mixture by selective condensation and

INTRODUCTION
evaporation. It is a process of purifying

compounds by means of separating
Distillation is used to separate

the
component substances from a liquid
more volatile substance from non-volatile

or less volatile substance. There are two
types of distillation, namely simple and
fractional.
Fractional
distillation
is
which the condensed vapor is collected.
essentially the same as simple distillation
These instruments were tightly
except that a fractionating column is
secured to prevent breakage of the
placed between the boiling flask and the
apparatuses. First, in the distilling flask
condenser. The fractionating column is
containing pieces of boiling stones, a
usually filled with glass or plastic beads.
30mL of vodka was added. The flask was

heated with an alcohol lamp constantly.
In the experiment, the simple
Ideally, the substance with the lowest
distillation was used to separate the
boiling
point
vaporizes
first
the
components substances of the vodka.
temperature remaining constant until that
The following are the objectives to be
substance has completely distilled. The
achieved by the group:
vapor is led into the condenser where, on

being cooled, it reverts to the liquid
1.)
To
be
able
to
separate
the
(condenses) and runs off into a calibrated
components of the alcoholic beverage
test tube that serves as a receiving
(vodka) by distillation.
vessel. The one obtained is called as the
2.) To set up a distillation curve.
distillate and those substances having a
3.) To calculate the percent ethanol
higher boiling point remain in the flask
present in the vodka.
and constitute the residue.
4.) To compare the simple and fractional

distillation process efficiency in terms of
separating mixtures of liquid.
After which, the temperature of

the first drop in every test tube was
recorded until it reached the temperature
METHODOLOGY
of 99 C. The first, second and last

distillate were used to test its flammability
A simple distillation apparatus
in a watch glass. The distilling flask was
consists essentially of three parts: a flask
cooled and the volume of the residue was
equipped with a thermometer and with an
recorded.
outlet tube from which the vapor is
temperature then was plotted in a graph
emitted; a condenser that consists of two
and the percentage of alcohol present in
tubes of placed one within the other and
the distillates were computed. On the
so arranged that the smaller (in which the
contrary, the percentage loss was also
vapor is condensed) is held in a stream of
computed.
coolant in the larger; and a vessel in
The
volume
and
the
Distillate
First
Second
Last
RESULTS AND DISCUSSION
Flame Test
+
+
-
Table 1. Volume and Temperature

Table 2 shows that a positive
of Distillate
TEST
VOLUME
TUBE
(mL)
0.5
1.0
1.5
2.0
2.5
3.0
3.5
4.0
4.5
5.0
5.5
6.0
6.5
7.0
7.5
8.0
8.5
9.0
9.5
10.0
10.5
11.0
11.5
12.0
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
TEMPERATURE
result in the flame test indicates the
(C)
presence of alcohol and a negative result
83
84
84
84
84
85
87
88
88
89
90
91
92
92
93
94
95
95
96
96
97
98
98
99
indicates that there is no alcohol. In the

first and second distillate, a blue with
orange tip flames was produced while the
last distillate did not produce any flame. It
shows that as the distillation continues,
the amount of alcohol decreases.
Table 1 shows that as the volume

of distillate increases, the temperature
also
increase
until
it
reaches
Figure 1. Simple Distillation Setup
the
temperature of 99 C. It shows that the
Figure 1 shows the setup where
volume and temperature are directly
the distillation was held. Since there is no
proportional.
fractionating column present, it is only just

a Simple Distillation setup.
Table 2. Flammability of Distillate
is usually the atmospheric pressure. The

vapor pressure is a very sensitive function
of temperature. It does not increase
linearly but in fact increases exponentially
with temperature, showing that there they
are directly proportional with each other.
When the vapor pressure of the liquid
equals the applied pressure, the liquid
Figure 2. Graph of Temperature and
boils. Thus, the boiling point of a liquid is
Volume of Distillate
the temperature at which the vapor

pressure equals the applied pressure.
Figure 2 shows that as the
The normal boiling point of a liquid is the
mixture is heated, the temperature rises
temperature at which the vapor pressure
until it reaches the temperature of the
of a liquid equals atmospheric pressure
lowest boiling substance in the mixture.
(1 atm). The boiling point of a liquid is a
The resultant hot vapor passes into a
measure of its volatility and its purity.
condenser and is converted to the liquid,
CALCULATIONS
which is then collected in a receiver flask.

The other components of the mixture
%v/v alcohol = Vf - Vi x 100
remain in their original phase until the
Vs
most volatile substance has all boiled off.

Only then does the temperature of the
= 12.0 - 0 x 100
gas phase rises again until it reaches the
30
boiling point of a second component in

the mixture, and so on.
= 40 % alcohol
This is the underlying principle

behind
distillation.
At
any
given
%loss = Vs - (Vd + Vr) x 100

Vs
temperature a liquid is in equilibrium with

its vapor. This equilibrium is described by
= 30 - (12.0 + 12.0) x 100
the vapor pressure of the liquid. The
30
vapor pressure is the pressure that the

molecules at the surface of the liquid
exert against the external pressure, which
= 20 % loss
CONCLUSION
increases,
the
presence
of
alcohol
decreases and also making the mixture

In the experiment, it was fairly
not flammable.
observed the fact that the process of

distillation of simple and fractional are not
REFERENCES
much
Helmenstine, A. (2016). Understand the

principles of distillation. About
education, 1-5. Retrieved from
http://chemistry.about.com/cs/5/f/bldi
tillation.htm
different
except
for
the
augmentation of the apparatus of the

fractional distillation. It is known as the
fractionating column that is usually filled
with glass or plastic beads. These beads
improve the separation between the
liquids being distilled. The reason that
fractional
distillation
gives
better
separation between the liquids is because

the glass beads in the fractionating
Natural Ingredient Resource Center.

(2015, May). Boiling points and
distillation. Retrieved from
http://naturalingredient.org/wp/wp-con
tent/uploads/Distillation.pdf
Winkle, M. v. (1967). Mass Transfer
Processes.
In
M. v.
Cinkle,
Distillation. New York: McGraw-Hill.
column provide "theoretical plates" on

which the refluxing liquid can condense,
re-evaporate,
and
condense
again,
essentially distilling the compound over

and
over.
distillation
Other
is
than
simple
that,
simple
process
of
extraction and purifying liquids by heating

and vaporization of the components of
alcohol (vodka) and water. Thus, based
on the experiment, as the temperature
DOCUMENTATION
Yoder, C. (2016). Distillation. Wired

chemist. Retrieved from
http://www.wiredchemist.com/chemist
ry/instructional/laboratory-tutorials/dis
tillation

Experiment 1 (Simple and Fractional Distillation)

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What are the objectives of the experiment?

What are the objectives of the experiment?

How does the simple distillation apparatus work?

How does the simple distillation apparatus work?

1

Simple and Fractional Distillation

mixture by selective condensation and

evaporation. It is a process of purifying

Distillation is used to separate

more volatile substance from non-volatile

which the condensed vapor is collected.

essentially the same as simple distillation

These instruments were tightly

except that a fractionating column is

secured to prevent breakage of the

placed between the boiling flask and the

apparatuses. First, in the distilling flask

condenser. The fractionating column is

containing pieces of boiling stones, a

usually filled with glass or plastic beads.

30mL of vodka was added. The flask was

In the experiment, the simple

Ideally, the substance with the lowest

distillation was used to separate the

components substances of the vodka.

temperature remaining constant until that

The following are the objectives to be

substance has completely distilled. The

achieved by the group:

vapor is led into the condenser where, on

(condenses) and runs off into a calibrated

components of the alcoholic beverage

test tube that serves as a receiving

vessel. The one obtained is called as the

2.) To set up a distillation curve.

distillate and those substances having a

3.) To calculate the percent ethanol

higher boiling point remain in the flask

present in the vodka.

and constitute the residue.

4.) To compare the simple and fractional

After which, the temperature of

of 99 C. The first, second and last

A simple distillation apparatus

in a watch glass. The distilling flask was

consists essentially of three parts: a flask

cooled and the volume of the residue was

equipped with a thermometer and with an

outlet tube from which the vapor is

temperature then was plotted in a graph

emitted; a condenser that consists of two

and the percentage of alcohol present in

tubes of placed one within the other and

the distillates were computed. On the

so arranged that the smaller (in which the

contrary, the percentage loss was also

vapor is condensed) is held in a stream of

coolant in the larger; and a vessel in

RESULTS AND DISCUSSION

Table 1. Volume and Temperature