SIMPLE AND FRACTIONAL DISTILLATION

Bienn Paulo A. Laforteza, Michael James O. Lazatin, Gell Marvi C. Lee

Mary Therese S.D. Leoncio and Denise T. Magdamit
Group 6 2G Medical Technology Organic Chemistry Laboratory

ABSTRACT
Distillation is the extraction of volatile component of a mixture through a two way process, evaporation and
condensation. The experiment aimed to differentiate simple from fractional distillation, to separate its components,
alcohol and water, and to determine its percent concentration of ethanol by using the fractional distillation method.
Vodka was the alcoholic beverage that was purified. A certain volume (30 mL) of vodka was placed on the pear-
shaped flask with boiling chips on a fractional distillation set-up and was heated constantly with an alcohol lamp. A
0.50 mL of distillate was collected in every test tube until the temperature reached close to 100 oC. The first and last
distillates were kept and its flammability was tested. The first distillate was flammable meaning it has the component,
ethanol, while the last distillate inflammable thus, having the water component after being purified. The volume of
distillate collected by the end of the distillation was 15.5 mL at 99 oC, giving a percent ethanol of 15%

INTRODUCTION tubes. The instruments were tightly secured and

Distillation is a process of converting a liquid to a
vapour, condensing the vapour and then collecting the
distillate in another container.1 Distillation is a widely
used method for separating mixtures based on
differences in the conditions required to change the
phase of components of the mixture.2 Distillation is an
important commercial process that is used in the
purification of a large variety of materials.3 Distillation
can be used in purifying water or other substances and
removing or separating the components of mixture
such as an alcoholic beverage like vodka. Vodka is a
clear liquor manufactured from ethyl alcohol. It lacks
color, and normally has very little taste or aroma. It is
said to have been originally created from potatoes in
Russia for medicinal purposes. Nowadays, Vodka is
distilled from barley, wheat or rye. Most flavored
vodka contains 30-35% alcohol, whereas clear vodka
is normally 40%, with a few brands offering a 50%
product on top. 4 There are four distillation methods
namely simple distillation, fractional distillation,
vacuum distillation and steam distillation.1 The
objectives of the experiment are (1) Differentiate
simple and fractional distillation, (2) Separate the
components of an alcoholic beverage (vodka) and (3)
Calculate the percentage of ethanol in the beverage.
EXPERIMENTAL
A.Compound tested or samples used
The sample used was clear unflavored vodka. (Cossack
Vodka)
B. Procedure
The set-up used was a fractional distillation set-up
(See Figure 1). The apparatus used were the following:
iron stand, iron rings, iron clamps, alcohol lamp, pear
shaped flask (with 30 mL vodka), still head,
thermometer, fractionating column (with boiling
stones) , condenser, rubber tubing, adapter and test
sturdy. The quick-fit distilling flask contains few pieces
of boiling stones and 30mL of the sample beverage
which is the vodka. After which, the flask was heated
with an alcohol lamp constantly being rotated under
the flask. In every test tube, a certain volume (0.5mL)
of distillate was collected and recorded until it reached
98-100o C. The first distillate and the last distillate
were kept to test its flammability. The set-up was
cooled and the volume of the residue was recorded.
The first and the last distillate were tested for
flammability test in a watch glass. The temperature
readings versus the volume of the distillate collected
were plotted in a graph. The percentage of ethanol and
the percentage loss were also computed.
RESULTS AND DISCUSSIONS
Table 1 (see next pages) shows that as the volume of
distillate increases, the temperature also increases
until it comes to a point wherein the temperature
closes to 99oC. When the temperature become
constant and shows a constant slope in the graph, it
confirms the presence of ethanol in the sample
wherein it is most concentrated.
Table 2 (see next pages) shows the graphed type of
the table of values of the temperature and volume of
the distillate. The constant values which signifies a
steady slope is the volume of the ethanol (5.0mL to
0.50mL). All in all, the volume of the distillate is 15.5
mL and the volume of the residue is 11.4 mL.
In the flammability test, the first distillate produced a
blue flame with an orange tip which makes it
flammable. The last distillate didn’t produce any flame
at all which makes it not flammable. Thus, the
component of the first distillate is ethyl alcohol and the
component of the last distillate is water. It shows that
as the distillation of the sample continues, there is a
decreasing amount of alcohol being gathered in the
separate test tubes. The first test tube contains more
alcohol compared to the last test tubes used which
contain the last few drops of distillate.
After performing the flammability test, the percent
alcohol, percent loss and percentage error were
computed:
% EtOH=5.0mL -0.50 mL x100
30mL
Simple distillation is used in separating components of
liquid mixtures, which have significantly different
boiling point while fractional distillation is used in
separating mixtures with boiling points close to each
other. Fractional distillation separates liquid much
better than simple distillation because of the boiling
chips in the fractionating column. Simple distillation
gives poorer separation than fractional distillation for it
provides theoretical plates on which the refluxing liquid
can condense, re-evaporate and condense again,
essentially distilling the compound over and over
again. Simple distillation has one distillation cycle while
the fractional distillation has two.

=15 % EtOH REFERENCES:

From book:
[1] Bayquen, A.V., Cruz, C.T., De Guia, R.M., Lampa,
F.F., Pena, G.T., Sarile, A.S. & Torres, P.C. (2009).
Laboratory Manual in Organic Chemistry. Manila: C&E
Publishing, Inc. p.13-14

% loss= 30mL – (11.4mL + 15.5 mL) x100 From Internet:

[2] Helmenstine, A.M. What is Distillation?
30mL http://chemistry.about.com/cs/5/f/bldistillation.htm
7/22/12
= 10.33% loss [3] [No author mentioned] Distillation.
http://www.umsl.edu/~orglab/documents/distillation/d
ist.htm 7/22/12
[4] Drinks Mixer. Vodka.
http://www.drinksmixer.com/desc28.html 7/22/12
[5] [No author mentioned] Distillation.
http://www.pharmpedia. com/Distillation. 7/22/12
% error= | 15 – 40 | x100 [6] [No author mentioned] Simple and Fractional
Distillation.
40 http://www.scribd.com/doc/17717405/Simple-and-
Fractional-Distillation-2EMT-Group-1-2009 7/22/12
=62.5%

Therefore, the percent ethanol content is 15%. The

percent loss is 10.33%. This explains that there was
some part of the sample that was lost which was
caused by evaporation due to the constant heating of
the flask. The percent loss also shows that there was
an excessive heating of the flask that caused the rapid
evaporation of the sample or it can be caused by them
was handling of the test tube that caused to the
careless collection of distillate.5

Listed below are the following possible sources of

error: (1) Parallax reading of temperature, (2) 0.5ml
calibration is not accurate and precise during the
experiment (3) Few drops of distillate were missed
while replacing new test tube for the distillate were not
accounted (4) Accurate measurement of residue was
skipped, resulting to 0% error (5) Distillate might have
vaporize during the experiment before it was tested to
flammability test (6) Not all test tubes were tested for
flammability test. 6
 Table 2. Graph of the Temperature versus
Volume

Figure 1. Fractional Distillation Set-up

Table 1. Temperature and Volume of the

Distillate

Test tube no. Volume (mL) Temp.oC

1 0.00 34
2 0.50 76 Table 3. Graph of the Temperature versus
3 1.00 76 Volume
4 1.50 76 150
5 2.00 76
6 2.50 76 100
7 3.00 76
8 3.50 76
9 4.00 76 50
10 4.50 76
11 5.00 76
12 5.50 80 0
0

8
1
2
3

5
6
7

9
10
11
12
13
14
15
13 6.00 81
14 6.50 83
15 7.00 84
16 7.50 85
17 8.00 86
18 8.50 87
19 9.00 90
20 9.50 92
21 10.00 93
22 10.50 95
23 11.00 96
24 11.50 96
25 12.00 96
26 12.50 97
27 13.00 97
28 13.50 97
29 14.00 97
30 14.50 98
31 15.00 98
32 15.5 99