SIMPLE AND FRACTIONAL DISTILLATION

Castillo, Fayrene Jean G.  Chan, Miguel Antonio K.  Cortez, Xianthine Kelly B.

Cruz, Ma. Concepcion S.  Dabu, Alvin Paul D.C.
Group 2 – 2DMT

ABSTRACT
Distillation is the process of converting a liquid to a vapor, condensing the vapor, and then, collecting the distillate in
another container. There are two types of distillation namely, simple and fractional. The group was assigned to
perform fractional distillation which aims to separate the components in a liquid mixture having different boiling
points. The liquid mixture used was vodka and the quick-fit apparatus was used to perform the distillation. The
mixture was then allowed to boil up to 100 degrees Celsius and the distillate was collected in test tubes limiting the
volume collected by each tube to 0.5 ml. Each distillate drop and its corresponding temperature were recorded and
the data retrieved were used to compute and determine the percentage of ethanol in the liquid mixture.

Introduction: bottomed flask (called distilling flask) where the

Distillation has been considered as one of the
oldest and most applied chemical technique
throughout history, it being performed for
purification of liquids. Such method developed
hand in hand with the early evolution of
chemistry.
Basically, this process involves the heating of a
liquid and separating the condensed vapors. By
heating the liquid until it boils, the resultant hot
vapors are captured and the condensed vapors
can be collected. Purification of a compound uses
distillation by separating it from a non-volatile or
a less-volatile material.
Boiling point plays an important role in
distillation. In a mixture, if two different
compounds that have different boiling points are
distilled properly, they can be separated into
individual components. Such is the case with the
ethanol-water mixture present in vodka.
It is an aim of this experiment to perform a
distillation process. Vodka was decided as the
mixture to be distilled. It is also an aim to be
able to separate the components of an alcoholic
beverage, calculate the percentage of ethanol
contained by the beverage and to distinguish or
differentiate simple from fractional distillation in
terms of their efficiency. To be able to do so, one
of the two most widely used type of distillation
process was performed by each group.
Simple distillation is useful in separating a
solid from a liquid or to separate two liquids with
very different boiling points; preferably, the
difference in the boiling points of these two
liquids must be at least 70oC. This type of
distillation was designed to evaporate a volatile
liquid from a solution of non-volatile substance
where the vapor is condensed in the water
condenser and then collected in the receiver. A
simple distillation set-up consists of a round-
liquid is placed; this distillation flask bears a
stillhead (or distillation head) which is connected
to a water condenser (Leibig condenser). The
stillhead has an attached thermometer adapter
with a thermometer; and an adapter is attached
to the condenser, connecting it to the receiving
flask.
As mentioned, the preferable difference in the
boiling points of two liquids in a mixture must be
at least 70oC, because those mixtures whose
boiling points are less than 70oC (that which have
almost similar boiling points) cannot be applied
with simple distillation. Simple distillation is not
efficient for separating liquids whose boiling
points lie close to each other. These situations
require fractional distillation.
Fractional distillation is useful in separating a
complex mixture of miscible liquids, such as
ethanol and water, into their components in
accordance with their boiling points. This
distillation process is performed with a
fractionating column. In this column, the vapours
from the heated liquid pass up. The temperature
in the column gradually decreases along its
length, therefore cooling the vapours. As cooled,
the components turn back into a liquid. The
components in the mixture are condensed in
different levels and by this, they are separated.
The components with higher boiling points
condense on the column and return to the
solution while the components with lower boiling
points pass through the column and are
collected. Rectification or enrichment refers to
the purification of the more volatile component
by contact between such counter-current streams
of vapour and liquid.
This report will tackle the results obtained from
fractional distillation as it was the type of
distillation assigned to the group to be
performed.
Methodology:
The group was tasked to perform fractional
distillation of vodka. Preparing the apparatus, an
example of a fractional distillation set-up is
shown in Figure 1.0:
Results/Discussion Table:
The group was not able to reach the 100OC
temperature limit required. The temperature
stopped increasing at 96oC only. Table 1.0 will
summarize the number of test tubes used, the
volume and the temperature.

Number of Volume of Temperature

Test Tube Distillate (OC)
used (mL)
1 0.5 76
2 1 76
3 1.5 78
4 2 78
5 2.5 78
6 3 80
7 3.5 80
8 4 80
9 4.5 80
10 5 80
11 5.5 82
12 6 82
13 6.5 84
Figure 1.0 Fractional distillation set-up 14 7 84
15 7.5 86
16 8 86
Prior to the experiment, fifteen (15) test tubes 17 8.5 88
were prepared. Each test tube was numbered
18 9 88
accordingly and was given a calibration of 0.5mL.
19 9.5 90
30mL of vodka was introduced into the quick-fit 20 10 90
distilling flask. An alcohol lamp was held beneath 21 10.5 90
the distilling flask, rotating it continuously until 22 11 92
the vodka started to boil. 23 11.5 92
24 12 94
The temperature during the first drop of the 25 12.5 94
distillate was recorded. The distillate, on the 26 13 96
other hand, was kept until the end of the 27 13.5 96
experiment to perform the flammability test. Table 1.0 Shows the summary of the data recorded
for the fractional distillation.
There was a rapid drop of distillate. Each
distillate was received by the test tube which had As shown by the table, the group was able to
a calibration of 0.5mL each. This is to keep track record 27 test tubes that were used during
of the total volume of distillate accumulated, and distillation. Each test tube has a 0.5 mL
to note the change in temperature increase in calibration; by multiplying the the number of test
relation to the volume of the mixture. tube used by the 0.5 calibration per test tube, we
can conclude that the total volume of distillate
The experiment performed did not reach 100oC. collected is 13.5mL. The temperature, as
The substance in the flask had already stopped mentioned, did not reach 100 OC but only up to
increasing in temperature even if constant heat 96 OC. We can see in the data that the interval of
was applied; it only reached 96oC from the 26th the increase in temperature is about 2OC. The
test tube. The 27th test tube had to wait a short temperature stayed at 80OC for the longest time
span of time until it was filled up to the 0.5mL compared to the other interval of temperature
mark because the substance was already increase. This is because the ethanol-water
inadequate. The last drop was kept also for the mixture is an example of an azeotropic mixture
flammability test. meaning, each component’s volatility is strongly
affected by the presence of the other component.
Here is the graph that will summarize the
temperature vs. volume of the distillate
collected throughout the experiment:
Graph 1.0 The plotted line graph of the recorded
volume and temperature of the distillate.
Compared to the results of simple distillation, the
interval of the increase in temperature in
fractional distillation is manifested more in the
former. In fractional distillation, the obtained
substance is more pure than the substance
obtained from simple distillation. This is because
the boiling point recorded is close to the original
boiling point of the components. The fractionating
column with boiling stones also helped gain a
more pure result. The repeated evaporation and
condensation during fractional distillation aid in
the complete purification of the more volatile
liquid.
The principle behind fractional distillation is
provided by the theory of Raoult’s Law. The law
states that the vapor pressure of a solution at
any given temperature is the sum of the vapor
pressures of each substance multiplied by its
mole fraction in the solution.
Mixtures that are miscible, and are therefore
subjected to fractional distillation are considered
ideal solutions. These solutions follow the
Raoult’s law. Actually, the said law only works for
ideal solutions. However, in the case of vodka, an
ethanol-water azeotropic mixture, it cannot be
fully separated by fractional distillation. It can
only be partially separated into its components.
Ideal solutions are not really ideal. However, they
are almost ideal because the two components
that form the mixture are very closely similar
with each other. An ideal solution is formed when
there are two different components with the
same size, shape and intermolecular forces.
Distillation works because the vapor above the
solution has a higher mole fraction of the more
volatile component than the liquid.
Boiling the vodka, the vapor on top of the boiling
liquid will be richer in the more volatile
component, in this case with ethanol. This vapor
will now travel to the fractionating column and
will eventually reach the height of the column
where it could condense due to the low
temperature at that part of the column. The
condensation will produce a liquid that is rich,
still, in ethanol. The liquid will then go down the
column where it will meet new vapors. This will
cause the already condensed vapor to reboil.
On the other hand, the liquid left behind each
reboiling is richer in the lesser-volatile
component. Over time, as ethanol passes into the
column into the condenser, the liquid in the flask
will be richer in water.
The cycle of boiling-condensing-reboiling must
happen repetitively so as to make the process
effective. The boiling stones inside the
fractionating column allow the column to have an
increased surface area. Increase in surface area
will permit maximum possible contact between
the condensed liquid that is going down the
column and the hot vapour travelling upward the
column. Without this, there would be no contact
between the liquid and the vapour.
During the flammability test, the first drop of the
distillate produced flame while the last drop did
not react to the flame. This means that the
process of distillation was successful and that the
components of vodka were separated to ethanol
and water.
References:
BOOK
1. Chemistry by McMurry, J.
2. Chemistry by Abrash
3. General Chemistry: Principles and
Structures by Brady
4. Purification of Laboratory Chemicals by
Perrin & Armarego
INTERNET
1. http://www.chemguide.co.uk/physical/phaseeq
ia/idealpd.html
2. http://home.clara.net/rod.beavon/distil.htm
3. http://orgchem.colorado.edu/hndbksupport/dis
t/dist.html