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Determination of Percent Ethanol in Vodka with the use of Simple Distillation

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Experiment #1
Determination of Percent Ethanol in Vodka with the use of Simple
Distillation
*De Alva, Mycaela; Decena, Mark Paulo D.; Enriquez, Floen Michael S.; Galvez,
Kristine Bernadette S.; Haghani Rad, Nilufar O.; and Lacap, Dixie Mae N.
2D-Pharmacy

Abstract
Distillation is the process of purifying and concentrating a liquid through
separating its components by heating it to the point of vaporization and
collecting the cooled condensate in another container. This experiment aims to
separate the components of an alcoholic beverage by simple distillation, to calculate the
percent ethanol in vodka and its percentage loss and to construct a distillation curve.
In this experiment, the set-up used is the simple distillation. Simple distillation
refers to the "simple" separation of compounds by evaporating the liquid and collecting it after
it passes through a condenser to be changed into a liquid state.
A certain volume (15mL) of vodka was placed on the distillation set-up and was heated
constantly. A calibrated test tube was used to collect 0.5 mL of distillate until the temperature
reached close to 100!. The volume of distillate collected by the end of the experiment was
9.5 mL at 100!, giving a percent alcohol of 36.6% and a loss of 10%.


I. Introduction

Distillation is the process
of purifying and concentrating a
liquid through separating its
components by heating it to the
point of vaporization and collecting
the cooled condensate in another
container. Volatility is the ease with
which a liquid vaporizes. This
purifying technique is used to
separate substances that have
different boiling points. There are
four types of distillation: simple,
fractional, vacuum and steam
distillation. This separation process
can be use to separate the
components of mixtures such as
vodka. Vodka is colorless liquor,
usually distilled from fermented
grains such as sorghum, corn, rye or
wheat. In this experiment, the set-up
used is the simple distillation. Simple
distillation refers to the "simple" separation
of compounds by evaporating the liquid
and collecting it after it passes through a
condenser to be changed into a liquid
state.
This experiment aims to (1) separate
the components of an alcoholic beverage
by simple distillation, (2) to calculate the
percent ethanol in vodka and its
percentage loss and (3) to construct a
distillation curve.

II. Methodology

All the needed materials were
prepared before the investigation
was made to avoid delay and to
minimize time. The alcoholic
beverage was obtained and the
brand was recorded. The simple
distillation set-up should be tightly
Determination of Percent Ethanol in Vodka with the use of Simple Distillation
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secured in order to prevent vapor
loss. The quick-fit distilling flask
contains three (3) pieces of boiling
stones and 15mL of the vodka. The
water in the condenser was gently
turned on. Subsequently, the flask
was heated with an alcohol lamp
constantly being rotated around the
flask to control the distribution of
heat, until the first drop of the
distillate reached the receiving flasks,
which are the test tubes, calibrated
into 0.5 milliliters each. In every test
tube, 0.5 milliliters of distillate was
being collected and recorded until it
reached !""#.
The flammability of the first and
last distillate was checked. In order
to do so, three to five drops of each
distillate were put into a watch glass
and ignite it with a match. If the
distillate ignites, it is flammable. If
the distillate did not ignite, it is non-
flammable. The presence of flame
pertains that there is ethanol in the
distillate. The boiling temperature
and the volume of distillate was
graphed. The percent ethanol in the
vodka was determined based on the
graph and the flammability test. The
percentage of ethanol present and
percent loss was then calculated.
The following formulas were used to
determine the stated herein:

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III. Results

Figure 1Simple distillation setup

Before the distillation process
starts or at 0 volume, the
temperature is at 30!.

Table 1 Volume and Temperature of
the distillate

Volume of distillate Temperature (!!
0.5 mL 81
1.0 mL 81
1.5 mL 81
2.0 mL 81
2.5 mL 82
3.0 mL 82
3.5 mL 83
4.0 mL 83
4.5 mL 83
5.0 mL 84
5.5 mL 85
6.0 mL 85
6.5 mL 87
7.0 mL 88
7.5 mL 90
8.0 mL 92
8.5 mL 95
9.0 mL 97
9.5 mL 100


Determination of Percent Ethanol in Vodka with the use of Simple Distillation
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Table 1 shows the results of
the boiling temperature for simple
distillation. It explains that as volume
of distillate increase, the
temperature also increases. In this
experiment, the first distillate that
has the least boiling point and
separated first and the last distillate
that has the highest boiling point
were tested for flammability.
According to Dalton’s Law
of Partial Pressure, a mixture will
only boil if the sum of the two partial
pressures is equal to the atmospheric
pressure. And according to Raoult’s
Law, the partial vapor pressure of a
mixture in an ideal solution is equal
to the vapor pressure of that pure
mixture times its mole fraction in the
liquid. A mixture must not have a
mole fraction of water that is
0.7because it will not boil at 100!
and is less than atmospheric
pressure. The concept of Dalton’s
and Raoult’s law is that the vapor
composition above a mixture is
dependent both on the vapor
pressures of the pure compound and
on their mole fraction in the mixture.
In the flammability test, the
first distillate produced a blue flame,
which explains that it has a presence
of ethanol while in the last distillate,
it did not produce flame for it was
already water produced because
alcohol was removed.
With this experiment, it shows
that as temperature increases, the
amount of alcohol in the mixture
decreases.


Figure 2 Temperature as a function
of volume

The figure 1 shows the
relationship between the
temperature and the volume of
distillate collected. The 0.5mL to 6.5
mL is the azeotrope, which is a
mixture that distills at a constant
boiling point and with a constant
composition. The boiling point of the
azeotrope is lower than that of the
pure component. Because of this,
the azeotrope will distill before a
component present in excess. Thus,
the excess component will not distill
as pure compound until the
azeotrope has completely distill.
The experiment used
aforementioned formula to calculate
the percentage of ethanol present
and percent loss.

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Determination of Percent Ethanol in Vodka with the use of Simple Distillation
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With the results gathered, the
percentage of alcohol obtained from
the simple distillation process was
36.6% while the percentage loss was
10%.

IV. Discussions
To interpret the data gathered,
the results was recorded and
tabulated. From the results obtained,
the percentage of alcohol obtained
from the simple distillation process
was 36.6% while the percentage loss
was 10%. The percentage loss of
10% explains that there is some part
of the sample that is loss caused by
evaporation due to constant heating
of the flask. It also shows that there
is an excessive heating of the flask
that caused the rapid evaporation of
the sample.

V. References

[1] Mayo, D.W., Pike, R.M. &
Trumper, P. K.
(2000).MicroscaleOrganic
Laboratory. 4
th
ed. NewYork: John Wiley & Sons,
Inc. pp.617-651.

[2] Russell, C.A. (2000).
Chemistry, Society and Environment:
A New History of theBritish Chemical
Industry
. RoyalSociety of Chemistry. pp.69

[3]
http://www.scribd.com/doc/1771740
5/Simple-and-Fractional-Distillation-
2EMT-Group-1-2009