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Organic Chemistry Laboratory CH200 (2015-2016) Experiment 1

Determination of percent ethanol present in Ginebra San Miguel Premium Gin


through Simple and Fractional Distillation
Angelo G. Tolentino*, Eloisa Francesca T. Umali, Janine Pearl G. Villaflor, Kim Nicole M. Yap
Department of Biological Sciences, College of Science
University of Santo Tomas, Espana Street, Manila 1008
Date Submitted: September 1, 2015
Abstract
The experiment performed is about the separation of the components of an alcoholic beverage with the use of simple
and fractional distillation. The primary goal of the separation of the two components (water and ethanol) is the determination
of percent ethanol present in the beverage.
There are two setups used: simple distillation and fractional distillation. The separation is due to the difference in
volatility of the components. Simple distillation is much simpler than fractional distillation and is commonly used to separate
pure liquids with their boiling points largely different from one another. Fractional distillation is a better way to separate
compounds but it takes longer to finish the process. Fractional distillation setup has a column with beads that provides
theoretical plates that enable fluid to condense, evaporate and re-condense again. The more volatile component will go to the
upper end of the column while the less volatile will go below the column.
Keywords: Distillation, Theoretical plates, Volatility

Introduction
Of all the techniques employed in the laboratory none has such an ancient lineage as that of
distillation. The first uses of distillation are shrouded in antiquity, but certainly by the Middle Ages a
body of literature existed describing various aspects of the technique. The Encyclopedia of Denis
Diderot (1713-1784), which appeared in seventeen volumes from 1751-1772, contains an extensive
entry on distillation with many references to various treatises on the subject. R. J. Forbes has produced
perhaps the most definitive study of the subject from antiquity through the nineteenth century in his
book A Short History of the Art of Distillation. [1]
Distillation is defined as a process in which a liquid or vapor mixture of two or more substances
is separated into its component fractions of desired purity, by the application and removal of heat. [2]
The experiment focus is to separate the components of an alcoholic beverage, assuming there is
water and ethanol only and excluding presence of flavors or any other component. This also aims to get
% ethanol present and to compare efficiency of simple and fractional distillation.
*TOLENTINO, Angelo G.

There are two types of distillation: simple and fractional. Simple distillation set-up includes a
distilling flask, distilling head, thermometer adapter, condenser, receiver adapter, receiving flask, iron
stands (for support on condenser and distilling flask) and a submersible pump. Simple distillation is
much easier than fractional because it only needs a little amount of time for the process to be done.
Fractional distillation, on the other hand, includes all components of simple distillation but with the
additional of fractional column with theoretical plates inside. Theoretical plates disperse liquids by
placing higher volatility liquid in the upper part of the plate and the lower volatile in the lower column.
With this column, this setup is much better in separating liquids and can readily purify mixtures than of
simple distillation.
There is no better option to be used because both types have different purpose. Simple
distillation is best used in mixtures with liquids boiling points are far from each other while fractional
distillation is best used when boiling points of liquids are quite close to each other.
The alcohol used is a Ginebra San Miguel product, Premium Gin extracted from juniper berries.
35% is the accepted % ethanol present in the gin. In the experiment, the % ethanol will be tested
whether what distillation setup is more efficient in getting a result close to the accepted value. The
efficiency of the setups will be confirmed by the % loss.
Methodology
The set up for simple distillation was assembled. Joints were greased to prevent vapor loss.
25mL of the sample beverage was placed in the distilling flask. Two pieces of boiling chips were then
added to the flask. The flask was heated with a Bunsen flame constantly being rotated around the flask.
Calibrated test tubes were used to collect 0.5mL distillate. The temperature was recorded after every
0.5mL distillate collected. Distillation was stopped when the temperature reached 96.4 degrees Celsius.
The set up was cooled. The remaining liquid from the distilling flask was poured into a 10mL graduated
cylinder. The volume was recorded. Finally, the temperature readings versus volume of distillate were
plotted. The % ethanol was also calculated.

Fig
ure A. Simple distillation

Figure B. Fractional distillation

Results and Discussion


Table 1. Volume Temperature Tally per 0.5 ml (Simple Distillation)
Volume (ml)
First drop
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
12.5
13.0
13.5
14.0
14.5

Temperature
(C)
60.5
73.5
76.2
77.9
78.4
78.4
79.2
79.9
80.5
79.9
80.0
80.7
80.3
82.3
83.6
85.0
87.5
90.6
92.7
93.6
94.5
95.0
95.7
96.0
96.4
96.6
96.6
96.6
96.6
96.4

Volume vs Temperature
90.5
80.5
Temperature(C)
70.5
60.5
First 0.5
drop
11.522.533.544.555.566.577.588.599.5
110.5
0 11
11.5
12
12.5
13
13.5
14
14.5
Volume(ml)
Volume vs Temperature

Figure 1. Volume-Temperature Relationship (Simple Distillation)


1st inflection point 0.5ml
2nd inflection point 8.5ml
Volume left 5.6 ml
Ethanol=

Loss=

8.5
100=34
25

25(2.5+12+5.6)
100=20.
25

Error=

3534
100=2.9
35

The temperature at every 0.5ml distillate collected was recorded. At 60.5 degrees Celsius, the
first drop was obtained. At 73.5 degrees Celsius, the first 0.5ml was collected. Throughout the
distillation process, the temperature increases as more volume of the distillate was collected. However,
there are instances when the temperature decreased of no more than 1 degree Celsius. The decreased
temperatures were observed at volumes 4.5ml, 6.0ml and 14.5ml with .6 degrees Celsius, .4 degrees
Celsius and .2 degrees Celsius less than the previous temperatures, respectively. These occurrences are
caused by experimental errors. The distillation was stopped at the volume of 14.5ml at 96.4 degrees
Celsius. The volume left in the distilling flask has a volume of 5.6ml. Using the obtained data, the
%ethanol is 34% and % Loss of 19.6% was calculated.

Table 2. Volume Temperature Tally per 0.5 ml (Fractional Distillation)


Volume (ml)
First drop
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
12.5
13.0
13.5

Temperature
(C)
72
72
76
76
78
78
78
78
78
78
78
79
78
82
88
90
92
92
92
92
91
92
93
95
96
97
97
97

Volume vs Temperature
97
92
87
Temperature(C)

82
77
72
First drop
0.511.522.533.544.555.566.577.588.599.5
10
10.5
11
11.5
12
12.5
13
13.5
Volume(ml)
Volume vs Temperature

Figure 2. Volume Temperature Relationship (Fractional Distillation)


1st inflection point 1.5ml
2nd inflection point 6.5ml
Volume left 2ml
Ethanol=

Loss=

8
100=32
25

25(6+7.5+2)
100=38
25

Error=

3532
100=8.6
35

The temperature of the first drop was recorded ml. 0.5ml of the distillate was collected and the
temperature for each 0.5ml mark. The first inflection point was at 1.5ml and the second inflection point
was at 6.5ml. The percent ethanol was solved by dividing the 2nd inflection point to the total volume that
was distilled and then multiplied to 100 that yields 26%.
Conclusion
Distillation is a process of separating components of a mixture. Separation of ethanol and water
through simple distillation and fractional distillation was completed and was able to determine the %

ethanol present. 34% ethanol was distilled from the sample, which is 1% different from the true value
for simple distillation and a 32% ethanol was distilled from fractional distillation. The % loss for simple
distillation setup is 20% while for fractional distillation, it is 38%. It shows that fractional distillation is
more efficient because despite the large % loss, still it was able to get 3% difference from the true value
while for simple distillation, very strict and meticulous process should be followed to obtain a %ethanol
close to the accepted value.
References
[1] Saltzman, M.D. (1999). The art of distillation and the dawn of hydrocarbon society. Bulletin for the
History of Chemistry, 24, 53
[2] http://lorien.ncl.ac.uk/ming/distil/distil0.htm Retrieved on August 29, 2015