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CHEM 200L Expt 1 2A-Biochemistry Group 2

SIMPLE AND FRACTIONAL DISTILLATION
Aquino, M.,* Badua, A., Belardo, A., Cabasag, A., Cantal, I., Carlos, M.
Department of Biochemistry, Faculty of Pharmacy
University of Santo Tomas
ABSTRACT
Fractional distillation system is presented for ethanol concentration detection in
vodka. This experiment aimed to differentiate simple from fractional distillation, to separate
components of an alcoholic beverage, and to calculate the percentage of ethanol in a
beverage. The proposed system consists of fractional distillation setup. In the proposed
system, boiling chips were subjected in the vodka sample and alcohol lamp was used to
vaporize the ethanol and carry it to the fractionating column. Temperature was recorded
throughout the experiment as the vodka sample started to boil. Each distillate was collected
using the 0.5 mL calibrated test tubes until the temperature reaches 100C. To test the
flammability of each distillate, flame test was performed. Finally, the percent ethanol was
computed by dividing the amount of distillate to initial volume of vodka sample multiplied by
100. The results of the experiment yielded 50% ethanol, with 100% proof. The validity of the
proposed system was verified using a control sample with 80% alcohol concentration, which
shows that the experimental results are above the true value. The real-world applicability of
the proposed fractional distillation system was demonstrated by measuring the ethanol
concentration of a commercial alcoholic beverage sample.
INTRODUCTION

carefully distilled. The two main types of

Ethanol, also called ethyl alcohol, is

distillation are "simple distillation" and

the principal type of alcohol present in

"fractional distillation", and both are widely

alcoholic beverages. It is formed by the

used in organic chemistry laboratories.

fermentation of sugar, quite possibly the

Simple distillation is used when the

oldest example of organic synthesis.

liquid is relatively pure (containing no more

Ethanol can also be made in the lab by a

than 10% liquid contaminants), has a non-

totally different process, but the ethanol

volatile

produced in the lab is identical to the

contaminant, or is mixed with another liquid

ethanol produced by the fermentation.

with a boiling point that differs by at least 25

component,

such

as

solid

Alcohol is a volatile liquid prepared

C. Fractional distillation is used when

by fermentation Alcohol acts as a central

separating mixtures of liquids whose boiling

nervous system (CNS) depressant, a

points are more similar (separated by less

diuretic, and a disinfectant.

than 25 C).

Distillation

is

one of

the most

The purpose of this experiment is to

common laboratory technique employed

differentiate

by chemists for the purification of organic

fractional

liquids. Compounds in a mixture with

components of the vodka sample, and to

different

determine the percentage of ethanol in the

boiling

points

separate

into

individual components when the mixture is

sample.

simple
distillation,

distillation
to

separate

from
the

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METHODOLOGY
A. Assembly of Fractional Distillation
Setup
The

analysts

assembled

the

fractional distillation setup according to the

following steps:
1. Clamp the distilling flask securely
to the iron stand. This is the
weight-bearing

part

of

Figure
1.

Actual

the

apparatus.
2. Fit fractionating column into joint in
flask.
3. Clamp fractionating column loosely

fractional distillation setup

B. Calibration of Test Tubes

in place. The fractionating column

should be perfectly vertical.
4. Attach distilling head firmly into top
joint on fractionating column.
5. Attach condenser to distilling head.

Test

tubes

were

calibrated

by

measuring 0.5 mL of water using the

serological pipette and marking each test
tubes.

Hold in place by clamping loosely

to iron stand.
6. Attach distilling head to condenser.
7. Connect rubber tubing from tap to
water-inlet connector to condenser.
8. Connect second rubber tubing to
top condenser and place the free
end into sink.
9. Pull thermometer

The analysts measured accurately

20 mL of the vodka sample in a microdistilling flask by using a serological pipette.
Next, 3 pieces of boiling chips were put in
the distilling flask and alcohol lamp was

adapter

and

attach to distilling head. Loosen

adapter and position the bulb of
thermometer just below the sidearm of distilling head. Tighten
adapter to hold thermometer in
place.

C. Fractional Distillation of Ethanol

used as the source of heat. The analysts

take note of the temperature throughout the
experiment,

for

the

reason

that

the

distillation experiment is done when the

temperature reaches 100C. The distillate
was received by the calibrated test tubes,
and the the first drop of distillate was
discarded. After each test tube reaches the
0.5 mL mark, 3 drops of distillate was lit
using a matchstick for the flame test. When
the

temperature

reaches

100C,

the

distillation was completed. The residue was

cooled and measured using a graduated
cylinder.

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liquid is converted into a vapor. In the liquid

20 mL Vodka sample
(distilling flask)

phase, the substance is held together by

+ 3 pcs boiling chips

to distill until 100C

intermolecular forces [1]. Condensation is a

phase-change process in which vapor

Distillates
(Collected in 0.5 mL
calibrated test tubes)
Perform flame test

Residue
Measure volume

Figure 2. Schematic diagram of distillation

converts into liquid when the temperature of

the vapor is reduced below the saturation
temperature corresponding to the pressure
in the vapor [2].

process of ethanol

One of the differences of simple and

fractional

D. Calculations
After
method,

distillation

is

the

use

of

fractionating column, an apparatus used

the

fractional

results

were

distillation

obtained

by

calculating the percent ethanol, percent

widely for countercurrent contacting of

vapor and liquid to effect separations by
distillation or absorption [3].

loss, and proof. The following formulas

were used by the analysts:

The principle of fractional distillation

is that different liquids boil at different
temperature. The miscible liquids boil at

1. % Ethanol

EtOH =

different temperature and evaporate at

mL distillate
100
initial Vsx

different temperature.
In fractional distillation, the liquid
and vapor pass through the column in

2. % Loss

opposite directions, the liquid downward

V (V D +V R)
Loss= S
100
Vs

and the vapor upward, a pattern known as

countercurrent flow. Liquid is held onto the
plates by barriers over which the liquid exits
the

plates,

passing

into

vertical

VD = total volume of distillate

downcomer that conveys the liquid to the

VR = volume of residue

plate below. Vapor rises up the column

VS = volume Sx

through the plates successively [4]. The

fractionating

3. Proof

column

ensures

that

the

ethanol vapor reaching the condenser is in

Proof =2 EtOH

a possible pure state. Condensation of

vapours of the less volatile liquid, which is
RESULTS AND DISCUSSION

water, will start before than those of more

volatile liquid, which is ethanol. So by time,

Distillation uses the principle of

vaporization

and

condensation.

Vaporization is the process by which a

the vapours rising in the fractionating

column will be more of ethanol and the

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liquid flowing down will consists of water.

contains ethanol. However, it was observed

The

and

that the first distillate has stronger flame

condensation is repeated. As a result of

and faster rate of combustion, which is

successive distillations, the vapours of

because

ethanol will reach at the top, from there

compared to the last distillate. The residue

they are taken into the condenser and

on the other hand, which measured 10.11

finally the substance is transferred to the

mL, is non-flammable, which means that it

receiver, which is 0.5 mL calibrated test

contains water.

process

of

distillations

of

the

presence

of

ethanol

tubes. The distillation process is ended

when the temperature reaches 100C. In
this experiment, the analysts collected 20
test tubes, which is equivalent to 10.00 mL
of distillate.
Table 1. Temperature of distillate obtained
per each 0.5 mL calibrated test tubes.
Test Tube
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Temperature (in C)
80.00
80.00
80.00
80.00
80.00
80.00
80.10
80.10
80.13
80.13
80.13
80.13
80.13
80.15
80.17
80.18
80.00
82.20
93.00
100.00

Flame test was performed to check

Figure 3. Flame test of test tube 13.

For the calculations, the analysts
used the formula in the previous section
and the following results were obtained: (1)
50% Ethanol, (2) -50.55% loss, and (3)
100% Proof.
The

results

obtained

were

compared to the original purity of the vodka

sample, which is only 80%. It means that
there were a few errors caused by the
analysts which can be corrected by proper
use of techniques and methods.

CONCLUSION

the flammability of each distillate collected.

3 drops of each test tube was lit by a

This experiment has presented a

matchstick in a watch glass. All 20 test

fractional distillation system for ethanol

tubes were flammable, which means that it

concentration purposes.

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The same type of information can
be collected for fractional distillation as
was for simple distillation. However,
fractional distillation is usually carried out
to

separate

two

miscible

liquids.

Fractional distillation uses fractionating

column which ensures that the distillate
will be in its possible pure state.

Education. http://dx.doi.org/10.1036/10978542.757542
[3] Souders, Mott. (2014). Distillation
column. In AccessScience. McGraw-Hill
Education. http://dx.doi.org/10.1036/10978542.270800
[4] King, C. Judson. (2014). Distillation. In
AccessScience. McGraw-Hill Education.
http://dx.doi.org/10.1036/10978542.201100

The components of the vodka

sample were successfully separated by
means of the distillation process.
The

purity

of

ethanol

was

calculated by dividing the volume in

distillate by the initial amount of vodka
sample multiplied by 100. The proof of
the experimental value is greater than
the controlled sample, which means that
there were errors in the experiment
performed.
The major principles involved in the
distillation

includes

condensation.

This

vaporization
technique

and
is

applicable for separation of two liquids

with different boiling points.
Proper techniques and methods
must always be observed by the analysts
to avoid errors.
REFERENCES
[1] Atkins, Peter W. (2014). Evaporation.
In
AccessScience.
McGraw-Hill
Education.http://dx.doi.org/10.1036/10978542.247100
[2] Dhir, Vijay K. (2014). Condensation.
In
AccessScience.
McGraw-Hill

Chan-Chiung Liu, Yao-Nan Wang, LungMing Fu, Chien Chieh, Micro-distillation

system for formaldehyde concentration
detection, Chemical Engineering Journal,
Volume 304, 15 November 2016, Pages
419-425,
ISSN
1385-8947,
http://dx.doi.org/10.1016/j.cej.2016.06.114
Fractional Distillation. (2016). Journal of
Visualized Experiments, doi:10.3791/5700
King, C. Judson. (2014). Distillation. In
AccessScience. McGraw-Hill Education.
http://dx.doi.org/10.1036/1097-8542.20110