University of Santo Tomas

Faculty of Pharmacy
Organic Chemistry Laboratory

The Percentage of Ethanol using Simple Distillation Method

*Urmaza,A.M; Valenton,J.G.; Villaceran,A.R.; Yap,K.M.; Zabala,K.; Zipagan,W.R.

Abstract
Vodka is composed primarily of water and ethanol with traces of impurities and flavorings and it has
40 percent alcohol by volume (80 proof). The experiment aimed to separate its components, alcohol
and water, and to determine its percent concentration of ethanol by using the simple distillation
method. A certain volume (30 mL) of vodka was placed on the distillation set-up and was heated
constantly. A certain volume (0.5 mL) of distillate was collected in every test tube until the
temperature reached close to 100 oC. The volume of distillate collected by the end of the distillation
was 10.0mL at 99 oC, giving a percent alcohol of 33.33%.

Introduction The experiment aims to (1)

separate the components of an
Distillation is the process of
alcoholic beverage (vodka) by
purifying and concentrating a liquid
distillation process, more
through separating its components
specifically by simple distillation,
by heating it to the point of
(2) calculate the percentage
vaporization and collecting the
alcohol and percentage loss in the
cooled condensate in another
alcoholic beverage (vodka) and (3)
container. This purifying technique
differentiate simple and fractional
is used to separate substances that
distillation techniques.
have different boiling points. There
are four types of distillation: Experimental
simple, fractional, vacuum and
In the experiment, all the
steam distillation. Distillation can
needed materials were prepared
be use in purifying water or other
and carefully set-up the simple
substances and removing or
distillation apparatus. The joints
separating the components of
were tightly sealed with a masking
mixture such as the vodka. Vodka
tape in order to prevent vapor loss.
is colorless liquor, usually distilled
The quick-fit distilling flask
from fermented grains such as
contains 3 pieces of boiling stones
sorghum, corn, rye or wheat. It is
and a certain volume (30mL) of the
believe to be originated in the
sample beverage (vodka). After
growing region of western Russia.
which, the flask was heated with
It usually has an alcohol content of
an bunsen burner constantly being
40% [1-4].
rotated around the flask. In every shaped stones added to liquids to
test tube, a certain volume make them boil more smoothly.
(0.05mL) of distillate was being
collected and recorded until it
reached 99oC. The set-up was
cooled and the volume of the
residue was recorded. The first and
the last distillate were tested for
flammability test. The temperature
readings versus the volume of the
distillate collected were plotted.
The percent alcohol and percent
loss were also calculated.

Results & Discussion

In the experiment, quick-fit

Figure 1. Quick-fit apparatus
apparatus was used. The Simple Distillation

components of quick-fit apparatus

are (1)pear-shaped flask, where They provide nucleation sites so
the residue is placed, (2) still the liquid boils easily without
head(distilling head), it holds the becoming superheated.
thermometer to allow the
temperature of vapors to be The heating of the flask
monitored during the distillation, should be slowly rotated. When the
(3) liebig condenser, a tube solution boils, a ring of condensate
surrounded by a water jacket to rising up the still head can be
cool and condense vapors, (4) observed. If heating is too rapid
thermometer, measures the and the condensate is pushed too
temperature, (5) receiver adapter, rapidly, equilibrium between liquid
connects the condenser and and vapor will not occur and
receiver, (6) round bottom flask, separation of the components will
where the distillate is placed.[1 & not be satisfactory. If the flask is
2]. Refer to Fig.1. heated too strongly before the
distilling head has been warmed by
In a pear-shaped flask hot vapors and condensate, the
contains the sample and 3 pieces still head may flood, or shows an
of boiling stones. The boiling excessive amount of liquid in one
stones are small, irregularly or more portions. [4].
 The following table shows the corresponds to the component with
result from the simple distillation: the least boiling point which is
separated first, and the second

Test Volume Temperature Flame corresponds with the highest

o
Tube (mL) C Test
boiling point that is drawn off at
1 0.50 78 Positive
2 1.00 79 the last. The component with the
3 1.50 79 highest boiling point can be
4 2.00 80
5 2.50 80 distilled and redistilled until it
6 3.00 81 becomes pure [2].
7 3.50 82
8 4.00 88 According to Dalton’s Law of
9 4.50 94
10 5.00 95 Partial Pressure, a mixture will only
11 5.50 95 boil if the sum of the two partial
12 6.00 95
13 6.50 96 pressures is equal to the
14 7.00 96 atmospheric pressure. And
15 7.50 97
16 8.00 97 according to Raoult’s Law, the
17 8.50 98 partial vapor pressure of a mixture
18 9.00 98
19 9.50 99 in an ideal solution is equal to the
20 10.00 99 Negative vapor pressure of that pure
mixture times its mole fraction in
Table 1. Volume, Temperature and
Flammability Test of the distillate the liquid. A mixture must not have
a mole fraction of water that is 0.7
because it will not boil at 100oC
and is less than atmospheric
Table 1 show that as the
pressure. The concept of Dalton’s
volume of distillate increase, the
and Raoult’s law is that the vapor
temperature also increases until it
composition above a mixture is
comes to a point wherein the
dependent both on the vapor
temperature closes to 100oC. In
pressures of the pure compound
this experiment, two distinct
fractions are obtained. The first
 and on their mole fraction in the increases, the temperature also
mixture [2 & 4]. increases. When the temperature
reached close to 100oC, the
In the flammability test, the
temperature stopped from rising
first test tube produced a blue
and is constant as showcased by
flame which means that ethanol is
the straight lines in the chart. The
present in the first distillate, while
highlighted part is the azeotrope,
in the 20th test tube, it did not
which is a mixture that distills at a
produce flame because alcohol was
constant boiling point and with a
removed. It shows that as the
constant composition. The boiling
distillation of the sample continues,
point of the azeotrope is lower than
there is a decreasing amount of
that of either pure component.
alcohol being gathered in the
Because boiling point is lower, the
separate test tubes. The first test
azeotrope will distill before a
tube contains more alcohol
component present in excess.
compared to the last test tubes
Thus, the excess component will
used which contain the last few
not distill as pure compound until
drops of distillate.
the azeotrope has completely distill
120
T [2-4].
E 100
M 80 After performing the
P
E 60 flammability test, the percent
R 40 alcohol and percent loss can then
A
T 20 be computed using these formulas.
U 0
R 5 5 5 5 5 5 5 5 5 5 volume of distillate
E 0 . 1. 2. 3 . 4 . 5. 6 . 7 . 8. 9. % alcohol= × 100
volume of sample
o
C
Volume(o(mL)
Figure 2. Temperature C) versus Volume % Loss=vol of sample -
(mL) of distillate
¿¿
Figure 2 shows that as the
volume of distillate collected
 And so, using the more than 25ºC from each other at
formulas above, one atmospheric pressure.
Fractional distillation separates
10 ml
% al cohol= ×100
30 ml liquid much better than simple
distillation because of the glass
% Alcohol=33.33 %
beads in the fractionating column.
30 mL−(13.5 mL+10 mL) Simple distillation gives poorer
% Loss= x 100
30 mL
separation than fractional
% Loss=21.66 % distillation for it provides
theoretical plates on which the
Therefore, the percent
refluxing liquid can condense, re-
alcohol of the sample is 33.33%.
evaporate and condense again,
The percent loss of 21.66%, on the
essentially distilling the compound
other hand, is quite near compared
over and over again. [2, 4 &6].
to the original alcohol content of
vodka. This explains that there is References
some part of the sample that is
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evaporation due to the constant Organic Laboratory. 4th ed. New
York: John Wiley & Sons, Inc. pp.
heating of the flask. The percent
617-651.
loss also shows that there is an
[2] Pavia, D.I., et.al. (1999).
excessive heating of the flask that
Introduction to Organic Laboratory
caused the rapid evaporation of the Technique: A Microscale Approach.
sample or it can be caused by the pp 22-54.
mishandling of the test tube that [3] Russell, C.A. (2000).
caused to the careless collection of Chemistry, Society and
distillate [6]. Environment: A New History of the
British Chemical Industry. Royal
Simple distillation is used in
Society of Chemistry. pp.69.
separating components of liquid
mixtures, which have boiling point
[4] Fessenden, R.J., Fessenden,
J.S. & Fiest, P. (2001) Organic
Laboratory Techniques. 3rd ed.
California, USA: Brooks/Cole. pp.
77-96.

[4]Vodka.http://www.associatepub
[6]Distillation.http://www.pharmpe
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