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Fractional Distillation of Ginebra San Miguel Gin

Hajime Q. Nakaegawa, Maria Elijah A. Natanawan, Jarvin E. Nipales, Jodine P. Novilla, Jonel G. Nuevo
Group 6 2A, Department of Biochemistry, Faculty of Pharmacy, University of Santo Tomas

Abstract
Distillation is the process of converting a liquid into a vapor, condensing the vapor, and collecting the distillate in
another container. This technique is used to separate components in a liquid mixture by boiling away the more volatile
liquid. The primary objective of this experiment was to separate the components of Ginebra San Miguel Gin using
fractional distillation. The mixture component was heated by an alcohol lamp until a temperature of 100 degrees Celsius
was obtained. The distillate was collected in 0.5mL calibrated test tubes and was used for the determination of the
percentage of ethanol in the mixture and the percent of gin lost. As a result, the researchers obtained a 33.33% ethanol
from the mixture component. The percentage loss of gin cant be obtained because the volume of residue was mistakenly
discarded by the researchers.

Introduction
Distillation is one of the most common
techniques in purifying and separating organic
liquids. This technique is used to separate
components in a liquid mixture which have
different boiling points, or to separate a
component that is not volatile. It was
discovered by the Greek alchemists and was
used years of chemical research in the
laboratory. Since then, the process has evolved
significantly by innovating the equipment and
apparatuses that have now been made in order
to make the process of distillation easier and
faster.
Distillation involves four types or
methods, namely, simple distillation, fractional
distillation, vacuum distillation, and steam
distillation. The technique itself involves two
major processes, namely, evaporation and
condensation. The liquid mixture is first
vaporized by heating, then condensed back to
a liquid which is called the distillate. This will be
collected by a separate flask or container. The
liquid substance that is left in the original
distillation after the whole process is called the
residue.
Boiling point plays an important role in
distillation. The boiling point of a liquid can be
defined as the temperature at which its vapor
pressure is equal to the external pressure
acting on the liquid, in this case, atmospheric
pressure.
A mixture having two different
substances with different boiling points can be
separated into their individual components

using distillation. In the researchers case, the


substances to be separated were the alcohol
and ethanol mixture in Ginebra San Miguel gin.
The objective of the experiment was to
perform the distillation process. Vodka and Gin
were decided to be the mixture to be distilled. It
also aimed to separate the components of the
alcoholic beverage, calculate the percentage of
ethanol and the percentage of ethanol lost in
the mixture, and lastly to differentiate the
process of simple distillation from fractional
distillation in terms of their efficiency. All even
groups in the class were tasked to do fractional
distillation, while the odd groups in simple
distillation. Groups 1 to 4 used white wine or
vodka as their mixture, while Groups 5 to 8
used gin.
Simple distillation works for most
common
separation
and
purification
procedures of organic liquids. It is used when
the boiling point difference of the two
components to be separated is large. It can be
efficiently used if the substances have at least
50 degrees difference in their boiling points.
Generally, this process was designed to
evaporate a liquid from a solution of nonvolatile substance. In situations when the
difference is lesser, it is highly advised to use
fractional distillation. This distillation is
performed by the use of a fractionating column
which the researchers used in the experiment.
This report will deal with the results
obtained from the fractional distillation process

as it was the distillation assigned to the


researchers group.
Materials and Methods
Materials
The experiment required a micro-scale
distillation set-up in order to be performed
properly. This primary apparatuses for this type
of set-up consisted of a pear-shaped distilling
flask containing boiling chips, a fractionating
column, a still head that placed the mercurial
thermometer in place, a water condenser,
rubber tubing, and an adaptor.
Other materials used in the experiment
were iron stands, clamps, graduated cylinder,
test tubes, alcohol lamp which served as the
source of heat, and a continuous supply of
water. Figure 1.0 shows a sample of the
fractional distillation set-up using a heater as
the source of heat.

pear-shaped distilling flask. An alcohol lamp


was placed directly beneath and continuously
rotated until the gin started to boil. The
temperature of the gin during the first distillate
was recorded. The distillate was kept in the
mean time for the flammability test to be
performed after.
Test tubes were set after the first
distillate Rapid drops of the distillate
succeeded after the first drops. Temperatures
were recorded for every test tube whenever the
distillate reaches the 0.5mL mark. This was
done in order to keep track of the total distillate
collected, and to note the change in
temperature in accordance to the volume of the
mixture.
The researchers were able to use a total
of 8 test tubes and reached the maximum
temperature needed which was 100 degrees
Celsius. The distillate from the last test tube
was also kept for the flammability test. The
remaining residue in the pear was also needed
to be kept. Unfortunately, the remaining residue
was accidentally discarded by the researchers.
Results and Discussion

GRAPH 1.0
Fractional Distillation of Ginebra San Miguel Gin
Summary of Temperature (C) vs Volume (mL)
120
100
80

FIGURE 1.0
Fractional Distillation set-up

Temperature (deg. Celsius)

60
40
20

Method

0
0123456789

Prior to performing the distillation


experiment, thirty test tubes were numbered
and calibrated to the 0.5mL mark before
heating. Fifteen milliliters (15 mL) of Ginebra
San Miguel was then used placed into the

Volume of Distillate (mL)

The researchers were able to reach the


maximum temperature needed for the
experiment, which was 100 degrees Celsius.
Graph 1.0 below shows a summary of the
temperature versus the volume of the distillate
collected during the duration of the experiment.
Table 1.0 below shows the values that
were used to make Graph 1.0 for better
understanding of results presented. It can be
observed that there is a relationship between
the Volume and the Temperature. As seen in
Graph 1.0 and Table 1.0, there was a constant
increase of temperature as the volume of
distillate increased. This means that the
relationship between the temperature and the
distillate in the experiment is directly
proportional.

TABLE 1.0
Fractional Distillation of Ginebra San Miguel Gin
Summary of Temperature (C) vs Volume (mL)

Volume (mL)

Temperature
(deg. Celsius)

0.5
1
1.5
2
2.5
3
3.5
4
4.5
5
5.5
6
6.5
7
7.5
8
8.5

80.5
81
81
81
81
81
81
81
81.5
82
82.5
85
86
98
99.5
100
100

However, as seen in the graph and


table, there was a constant temperature of 81
degrees Celsius from volumes 1.0 to 4.0mL.
This part is the azeotrope of the mixture being

condensed and vaporized continuously in the


fractionating column to become ethanol itself.
Azeotropes are mixtures that are distilled at a
constant boiling temperature, with constant
composition. The boiling point of an azeotrope
is lower than both components to be
separated. Because the boiling point is lower,
the azeotrope will be distilled first before the
components in excess. Because of this, the
excess component will not be distilled as a
pure substance until the azeotrope has been
completely distilled.
This means that throughout the constant
temperature reading, ethanol was the one
being produced as the distillate.
It is important to consider that the
number of times that the process of
vaporization and condensation occurs depends
on the efficiency of the fractionating column.
The more efficient the fractionating column, the
more times this happens and the purer the final
product will be. With azeotropes, the vapor
liquid curves are not ideal and have a point
where the vapor curve meets the liquid curve.
This point is called the azeotrope point.
There are two important principles
involved in the distillation process. First one is
Daltons Law of Partial Pressure. This states
that a mixture will only boil if the sum of the two
partial pressures is equal to the atmospheric
pressure. Second is Raoults Law, which states
that 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 which is 0.7 because it will not
boil at 100 degrees Celsius, which is waters
boiling point. The concept behind these two
laws is that vapor composition is dependent on
both pressures of the compound and on their
mole fraction in the mixture.
After completely heating up to 100
degrees Celsius, flammability test was
performed on the first and last distillate
collected. The first distillate was tested to be
flammable because no distillate remained after
testing. This proves that ethanol was still
present in the first drops of the experiment. The

last distillate produced no flame. This proves


that ethanol was absent in the last distillate.
The last distillate was water.
Using the following formulas below, both
the percent of ethanol in the mixture and the
percent of ethanol lost in the mixture were to
be computed. Unfortunately, the residue that
was supposedly used by the researchers was
discarded accidently. This is why no
percentage loss of ethanol can be obtained in
this experiment. Given the following formulas:
ethanol=

volume of ethanol
100
volume of sample

where
Volume of Ethanol=Vf Vi

loss=

where
Vd=Volume of total distillate

Vr=Volume of Residue

100
theoretical

error =

Using the formula, the researchers were


only able to obtain the percentage of ethanol
present:
ethanol=

15.00 mL(5.5 mL+Vr)


100
15.00 mL

% loss = unknown
And now for the % error in the
experiment,
4033.33 100
40
error =
% error = 16.68%

V sample(Vd +Vr)
100
V sample

theoreticalactual

loss=

5.500.50 mL
100
15.00 mL

% ethanol = 33.33%
And the percentage loss cannot be
computed because of the discarded residue,
but this should be in the form of:

Therefore, the percentage of ethanol in


the experiment was 33.33% which is quite near
from the true value of 40% of ethanol present
in the Ginebra San Miguel Gin. This might be
caused by the constant heating of the flask
which leads to the loss of the ethanol. This
made a low percentage error in the
experiment, which is 16.68%. The percentage
loss of ethanol was not unknown because it
was accidentally discarded by the researchers.
Nevertheless, the percentage loss has an
objective in the experiment. This shows that
there was an excessive heating of the flask
that caused the rapid evaporation of the
sample or that this loss might have been cause
by the mishandling of the test tubes
In conclusion, fractional distillation is a
better preference to be used in the separation
of water and ethanol. The boiling point of
ethanol is 78.1 degrees Celsius, while water is
100 degrees Celsius. The difference of their
boiling points is 21.9 degrees Celsius, which,
as stated above, makes Simple Distillation not
a good choice since a difference of at least 50
degrees Celsius in order to obtain efficient and
proper
results.
Furthermore,
fractional
distillation is more accurate compared to
simple distillation because the use of a
fractionating column provides an efficient
exchange of heat and material between the
condensate flowing down the column and

vapors going up. By the use of a fractionating


column, there is a repeated cycle of
condensing and vaporizing in the substance.
This produces a more pure distillate compared
to simple distillation.
References
Books and Journal Articles
Bathan, G., Bayquen, A., Crisostomo, A.B.,
Cruz, C., et.al. (2014). Laboratory
Manual in Organic Chemistry (Revised
Edition). (pp.13-14).
Health, K. (2003). Laboratory Chemistry
Organic
Techniques.
Birmingham,
United Kingdom: Curriculum Press.
Pavia, D., Lampman, G., Kriz G., & Engel, R.
(2005).
Introduction
to
Organic
Laboratory Techniques: A Small Scale
Approach (2nd Ed.). (pp.733-746)
Whitten, K., Davis R., Peck, M., & Stanley, G.
(2010). Chemistry (9th Ed.). (p. 463)
Internet
http://www.wiredchemist.com/chemistry/instruct
ional/laboratory-tutorials/distillation
http://www.wfu.edu/chem/courses/organic/distill
/distillation.htm