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SIMPLE AND FRACTIONAL DISTILLATION

Kristianne Samantha G. Gonzales, Camille Louisse R. Lee, Danielle Sabrina E. Lim, Kenneth H. Lim,
Ieoh Kenzo T. Macatiag, Miguel Antonio L. Mendoza
Group 6
2D Medical Technology
Organic Chemistry Laboratory

Abstract
Distillation is the process of separating different components in a liquid substance by means of
evaporation and condensation. After which, collecting the distillate in another container. The objectives of
the experiment were to differentiate simple distillation from fractional distillation, separate the
components of an alcoholic beverage, specifically, vodka and to calculate the percentage of ethanol in a
beverage. A certain volume of vodka (20 ml) was placed in the quick-fitting distilling flask that contained
boiling stones on a fractional distillation set-up and was heated with an alcohol lamp constantly being
rotated under the flask. In every test tube, a certain volume (0.5 mL) of distillate was collected and
recorded until it reached 100C. The first distillate and the last distillate were kept to test its flammability.
The first distillate was flammable meaning it contained ethanol while the last distillate was not flammable,
meaning it only contains water. The volume of distillate collected by the end of the distillation was 6.5 ml
at 100 C, giving a percent ethanol of 12.5%

Introduction
Distillation is a commonly used method for
more efficient in terms of decontamination
or
separation of substances. A fractional distillation
apparatus includes a fractionating column placed
between the pot and the distilling head, as
shown in Figure 1. The objective of this
experiment is to (a) Differentiate simple and
fractional
distillation,
(b)
Separate
the
components purifying liquids and separating
mixtures
of
liquids
into
their
individual
components.
Familiar examples include the
distillation of crude fermentation broths into
alcoholic spirits such as gin and vodka, and the
fractionation of crude oil into useful products
such as gasoline and heating oil. In the organic
lab, distillation is used for purifying solvents and
liquid reaction products. There are four methods
of distillation: simple distillation, fractional
distillation, vacuum distillation, and steam
distillation. In this experiment we used the simple
and fractional method. If one compound is much
more volatile than the other, the compounds can
be separated in one evaporation step. Such a
step is called simple distillation which is a set-up
where a solution or mixture of substances with
different volatility is separated through exposure
to heat. Evaporation takes place, changing liquid
to gas. Vapors form and pass through a
condenser wherein it changes its form from gas
to liquid. The collected vapor is the distillate of
the experiment. Residue is the remains in the
set-up that didnt pass through the process of
evaporation and condensation. It uses an
apparatus that consists of only a pot, a
distillation head, a condenser, an adapter, and a
receiver.

Figure 1. Simple Distillation set-up


When the boiling points of two compounds
differ by less than 40 C, they cannot be
separated efficiently by simple distillation.
Fractional
distillations
undergo
series
of
evaporation
and
condensation
process to purify more complex mixtures. It is of
an alcoholic beverage; and (c) Calculate the
percentage of ethanol in a beverage.

RESULTS AND DISCUSSION


For the fractional distillation, the temperature
was at 30C. The first drop for the first test tube
happened after the temperature on the set-up
reached 82C. When the drops reached 0.5mL,
the temperature remained at 82C. Table 1 (see
page 4) shows all the data gathered from the
experiments.
In the flammability test, the contents for the
first test tube and the last test tube for the
fractional distillation set-up were tested for their
flammability.

Figure 2. Fractional Distillation

Experimental
A. Compounds tested (or Samples used)
The sample used was clear unflavored
vodka. (Cossack Blue Vodka)

B. Procedure
The set-up used was a fractional distillation setup (See Figure 1). The apparatus used were the
following: iron stand, iron rings, iron clamps,
alcohol lamp, quick-fit distilling flask, still head
thermometer, fractioning column (with boiling
stones), condenser, rubber tubing, adapter and
test tubes. The instruments were tightly secured,
assembled and sturdy. The quick-fit distilling flask
contained few pieces of boiling stones and 20 mL
of the sample beverage which is vodka. After
which, the flask was heated with an alcohol lamp
constantly being rotated under the flask. In every
test tube, a certain volume (0.5 mL) of distillate
was collected and recorded until it reached
100C. The first distillate and the last distillate
were kept to test its flammability. The first and
the last distillate were tested for flammability test
in a watch glass. The set-up was cooled and the
volume of the residue was recorded. The
temperature readings versus the volume of the
distillate collected were plotted in a graph. The
percentage

of ethanol

percentage loss (%

(%

v
v )

and

the

v
v ) were also computed.

The first distillate produced a blue flame with


an orange tip, which makes them flammable. As
for the last distillates there were no flames
observed, which makes them non-flammable.
Thus, the component of the first distillates is
ethyl alcohol and the component of the last
distillates is water. This test shows that as the
distillation of the sample continues, there is a
decrease in the ethyl alcohol component for the
distillates gathered.
The data gathered above were graphed in
order to see the relationship of temperature to
the volume of distillate collected from the
sample. (Figure 3 in page 4)
(See figure 3 in page 4) The values from the
first drop until the value that signifies a steady
slope accounts for the volume of the ethanol
collected (6.0mL for simple and 2.5mL for
fractional set-up). All in all, the volume of the
distillate is for the simple distillation is 14mL and
the volume of the residue is 16mL. Meanwhile,
the volume of the distillate is 6.5mL and the
volume of the residue is 8mL for the fractional
distillation. This information was needed to be
able to compute for the percentage of ethanol in
the vodka and the percentage loss in the
experiment for both simple and fractional
distillations.
Calculations for fractional distillation:
%Ethanol =

Volume of Ethanol
100
Volume of Sample

2.5 mL
100
20 mL

30.0 mL(14.0 mL+16.0 mL)


100
20.0 mL

= 12.5%

= 0% loss

%Loss

True valueExperimental value


100
Volume sample(volume distillate+volume residue)
100
True value
Volume sample
error =

20.0 mL (6.6 mL+8 mL)


100
20.0 mL

32.512.5
100
32.5

20
100
32.5

= 27.5% loss

True valueExperimental value

100
True value

error =

32.520
100
32.5

12.5
100
32.5

Therefore, the percentage of ethanol was found


to be 20% with a percentage loss of 0% and
12.5% with a percentage loss of 27.5% for
simple distillation and fractional distillation
respectively. The percentage loss during the
fractional distillation set-up suggests that there
were some parts of the sample lost due to
evaporation because of the constant heating of
the flask. Another reason for the excessive
percent loss was the failure to collect some drops
of distillate due to the time interval of replacing
the test tube.

= 61.5%
Calculations for simple distillation:
%Ethanol =

Volume of Ethanol
100
Volume of Sample
6.0 mL
100
3 o mL

= 20%
%Loss

= 38.5%

The percentage error that resulted from the


experiment was higher than the expected result.
It is therefore concluded that errors must have
occurred during this experiment. The possible
sources of error in the experiment were: parallax
reading of the thermometer, 0.5 calibration of the
receiving test tube was not accurate and precise,
room temperature might have affected the
readings in the thermometer, distillate may have
vaporized before flammability test, few drops of
the distillate were not accounted, and accuracy of
measurement of the volume of residue.

References

Volume sample( volume distillate+ volume residue )


100
Volume sample
From books

[1]Bathan, G., Bayquen, A., & Crisostomo, A. et


al. (2014). Simple and
Test
Fractional Distillation. In
Tube
Volume
Laboratory
Manual
in
No.
Organic
Chemistry.
1
0.5
Queszon
City,
2
1.0
Philippinnes.
C&E
3
1.5
Publishing, Inc. p 13-14.
4
2.0
Test
Temperature 5 Flammability
2.5
Test
Volume
Tube
6
3.0
Fractional
7
3.5
No.
8
82
+4.0
1
0.5
9
4.5
2
1.0
83
10
5.0
3
1.5
84
11
5.5
84
4
2.0
12
6.0
5
2.5
85
13
6.5
6
3.0
86
14
7.0
89
7
3.5
15
7.5
91
8
4.0
16
8.0
9
4.5
94
10
5.0
97
17
8.5
97
11
5.5
18
9.0
12
6.0
98
19
9.5
100
-10.0
13
6.5
20
21
22
23
24
25
26
27
28
29
30
31
32

10.5
11.0
11.5
12.0
12.5
13.0
13.5
14.0
14.5
15.0
15.5
16.0

From the internet (on-line)


[2]de Leon, P., Dejelo, M., Dolojan, J.D. and
Gatdula, E.J. Determination of Percent Ethanol in
White Castle Whisky with the use of Simple and
Fractional Distillation.
http://www.scribd.com/doc/36789109/Distillation
-of-Alcoholic-Beverage-Formal-Report 9/20/15
[3]Gonong, D.A., Gutierez, H.A., Hagiwara, K.,
Javier, C.B. and Labajo, A.M. Distillation of
Alcohol in Vodka.

http://www.scribd.com/doc/36247410/Distillation
-of-Alcohol-inFlammability
Temperature
Vodka 9/20/15
Test
Simple
78
79
84
84
84
84
84
86
87
87
87
87
87
88
88
88
88
89
90
90
92
94
94
94
94
96
96
98
98
98
99
100

[4]Laforteza,
B.P.,
Lazatin, M.J., Lee, G.M.,
Leoncio,
Mt.T.
and
Magdamit, D. Simple
and
Fractional
Distillation.

http://www.scribd.com/doc/105189778/Simpleand-Fractional-Distillation-formal-Report#scribd 9
/20/15

Table 1. Results for Fractional Distillation

Table 2. Results of Simple Distillation

Figure 3. Graph of Temperature vs. Volume (Fractional Distillation)


100
90
80
70
Temperature

60
50
40
30
Volume (mL)

Figure 4. Graph of Temperature vs. Volume (Simple Distillation)

100.00

90.00

80.00

70.00
Temperature

60.00

50.00

40.00

30.00

Volume