FRACTIONAL DISTILLATION

ABSTRACT
The separation of components of the alcoholic beverage, vodka, using fractional distillation was the main
objective of this experiment. Smirnoff was the brand of vodka used. Temperature readings taken at times
when distillates were collected show that distillates taken when temperatures ranged from about eighty
degrees Celsius to ninety-four degrees Celsius had an alcoholic odor and produced a strong flame during
the flammability test. Distillates collected at temperatures approaching one hundred degrees Celsius
possessed no odor and did not produce any flame. The first and final distillate possess significant
differences in odor and flammability test. The observation that the first up to the twenty-third distillates
contained the most concentration of alcohol while the remaining distillates taken at increasing
temperatures gradually contained more concentration of water were based from those results. The
percentage volume alcohol was close to the true alcohol percentage of forty percent as presented on the
label, based on the percentage by volume of ethanol and percentage by volume of loss calculated from
the results. The percentage by volume of loss was minimal meaning most of the sample was collected.
The percentage by volume of alcohol remained the same, and the percentage by volume of loss for
fractional distillation was slightly less than the value obtained from simple distillation when comparing the
obtained data to a simple distillation simple distillation set up. This showed that fractional distillation is
more effective at separating substances with differences in boiling point than simple distillation.

I. INTRODUCTION By the end of the experiment, the following

The task for the first experiment was to
completely separate a mixture wherein the
liquids have different boiling points through the
method of distillation. The process of distillation
involves the boiling of the mixture until the liquid
with the lower boiling point begins to turn into a
vapor which will then be collected in a
condenser. The collected vapor will be cooled
down by the said apparatus that will cause it to
turn back into a liquid out the other end of the
tube to be received by another flask. [1]
Simple distillation is a kind of distillation that is
best used to separate liquids with a huge
difference in boiling point. A simple distillation
setup consists of a boiling flask connected to an
adapter with a thermometer on top that is used
to determine the temperature at which the liquid
is boiling. The lateral side of the adapter is
connected to a condenser where cold water
constantly passes through, leading to a receiving
flask.
Fractional distillation, on the other hand, is a
kind of distillation that is best used in separating
liquids whose boiling points are closer together.
A fractional distillation setup is similar to a
simple distillation setup, only with the addition of
a fractionating column. Fractionating columns
are often filled with glass beads that help with
providing “theoretical plates” that will help the
liquid to condense, re-evaporate and condense
once again. This will ensure a better separation
between the substances present. [2]
objectives must be attained: (1) compare and
contrast simple and fractional distillation (2)
calculate the percentage of ethanol in a vodka
sample (3) identify which distillation is most
efficient for the sample used.
II. EXPERIMENTAL
A. Test Compound/s (or Sample/s)
used
Thirty milliliters of Smirnoff Vodka was used
for fractional distillation. Smirnoff Vodka is a
grain based and triple distilled clear liquid
mixture of forty percent ethanol (80-proof) and
water.
B. Procedure
1. Fractional Distillation
Fractional distillation set-up was carefully
assembled for the distillation of vodka. For
distillate receivers, several test tubes were
calibrated to half a milliliter and were numbered
accordingly. Next, boiling stones and thirty
milliliters of Smirnoff Vodka were introduced to
the distilling flask. By rotating an alcohol lamp,
the distilling flask was heated up until the vodka
started to boil. The first drop of the distillate was
read and recorded. Each half a milliliter of the
distillate was collected using the prepared test
tubes and the temperature at the time of
collection was recorded as well. Collecting of the
distillate was stopped when the temperature
reached a hundred degrees Celsius.
Figure 1.​​ Fractional Distillation Set-up [3]
2. Flammability Test
Three to five drops of distillate from the first
test tube were put on a watch glass and lit with a
matchstick to test its flammability. The same
step was repeated on the last test tube of
distillate. The flammability of the first and last
test tube of distillate was determined and
compared. The same step was repeated for the
remaining test tubes of distillates and the
flammability of each was recorded accordingly.
The volumes of the residue and distillate
collected were measured. Lastly, the percent
ethanol and percent loss was computed for and
recorded.
Before the experiment was conducted, the
conditions must be initially maintained at
standard room temperature. Tabulated in Table 1
are the data collected from the distillate with its
corresponding relative temperature, odor and
flammability. It was observed in the second to
twelveth distillate that the temperature remained
constant at 80 ℃ because a substantial amount
of ethanol were concentrated in this particular
portion. Considering that the boiling point of
ethanol is 78 ℃, it can be inferred that the
distillate collected near that particular range
would yield the expected component. As the
temperature steadily increases up to the 100 ℃
mark, the distillate being collected from the
twenty-fourth to the twenty-eighth distillate
began to exhibit an odorless smell and failed to
produce a flame in the flammability test. From
this result, it can be concluded that the distillate
subsequently contains an increasing amount of
water concentration which has a boiling point of
100 ℃.
The flammability test of the presence of
ethanol is represented by the following balanced
combustion equation:
​ ​ 2CO​2​ + 3H​2​O
C​2​H​5​OH +3O​2​ →
Distillates with ethanol would react with
oxygen to produce carbon dioxide, water and
heat.
Based on the results gathered, the first and
the last distillate has comparatively significant
differences. The first distillate possesses a strong
alcoholic odor and was able to produce a flame in
the flammability test. On the other hand, the last
distillate had an odorless smell and did not
produce a flame.

III. RESULTS AND DISCUSSION Table 1. ​Data for the Distillate Collected at a
Starting Temperature of 22℃ Room Temperature
Fractional distillation underwent two rounds of
(All distillates were collected at 0.5 mL)
evaporation and condensation due to the
presence of a theoretical plate in the
fractionating column for the particular set-up. Distillate Temperature Odor Flammability
The cycle occurs in the column containing the Collected collected (℃) Test
packing material which serves to provide a larger
F1 78 alcoholic flammable
vertical surface area in order to directly prevent
the upward movement of the gas to the F2 80 alcoholic flammable
condenser. As a result, the components were
F3 80 alcoholic flammable
more efficiently separated within the repeating
cycles of the vapor being condensed and F4 80 alcoholic flammable
evaporated before reaching the distillation head
[2]. F5 80 alcoholic flammable

F6 80 alcoholic flammable
 F7 80 alcoholic flammable

F8 80 alcoholic flammable

F9 80 alcoholic flammable

F10 80 alcoholic flammable

F11 80 alcoholic flammable

F12 80 alcoholic flammable

F13 81 alcoholic flammable

F14 82 alcoholic flammable

A total volume of 30 mL was used for the
F15 82 alcoholic flammable experiment. The volume of total fractions
collected from fractional distillation is 14 mL. In
F16 84 alcoholic flammable
addition, 11.3 mL of the fractions are flammable
F17 85 alcoholic flammable and the residue is measured at 13 mL.
After conducting the flammability test, the
F18 87 alcoholic flammable percentage ethanol and percentage loss were
F19 88 alcoholic flammable computed with the obtained data:

F20 88 alcoholic flammable Percentage of Alcohol (%v/v alcohol)

vol of f lammable f ractions, mL
F21 90 alcoholic flammable = 30mL x 100%
11.5mL
F22 90 alcoholic flammable = 30mL x 100%

F23 94 alcoholic flammable

= 38.33%
F24 96 faint not Percentage of Ethanol
alcoholic flammable total samples used x vol of samples
= 30mL x 100%
F25 98 odorless not 11 x 0.5mL
= 30mL x 100%
flammable
= 18.33%
F26 99 odorless not
flammable

F27 99 odorless not Percentage loss (%v/v loss)

flammable 30mL-(vol of residue+vol of fraction)= vol
of sample lost
F28 100 odorless not vol of sample lost, mL
flammable = 30mL x 100%
30mL − (14mL+13mL)
= 30mL x 100%
​Figure 1 represents a line graph of the 3mL
temperature and the volume of the distillate = 30mL x 100%
collected. It can be observed that most of the
concentration of ethanol were collected at its = 10%
boiling point of 78 ℃. The graph evidently
corresponds to the data collected in the first The percentage ethanol is computed as
table. 18.33%. The percentage alcohol, on the other
hand, was compared to the percentage alcohol of
Figure 2. ​Temperature (℃) vs. Volume (mL) of the sample used in the experiment. The
Distillate Collected percentage alcohol that was computed (38.33%)
possesses a certain level of accuracy with the
true value of 40%. The percentage loss, on the
other hand, measures the effectivity of the
distillation in separating the liquid components.
Based on the results, only 10% of the sample
was lost that can possibly be accounted from the
evaporation caused by constant heating of the
flask.
The data were subsequently compared with
the results of a simple distillation set-up. The
percentage alcohol were of the same values of
38.33% while the percentage loss on a fractional
distillation set-up (10%) is slightly less than that
of a simple distillation set-up (10.3%). In
general, fractional distillation is more suitable in
separating components with boiling point
differences because of the repeated evaporation
condensation cycle.
As the temperature gradually increases to the
final mark and the distillation of the sample
continues, the concentration of alcohol decreases
and the composition changes into water. The
components were successfully separated and the
percentage alcohol of the alcoholic beverage
sample was computed as 38.33%. The
percentage ethanol, on the other hand, is
18.33%. The fractional distillation set-up was
presented to be a more efficient technique in
separating components of different boiling points
because it undergo two rounds of evaporation
and condensation within its fractionating column.

REFERENCES
[1] Becker, A. (2016). How to Explain Simple vs
Fractional Distillation.
https://education.seattlepi.com/explain-simple-v
s-fractional-distillation-3690.html
[2] ​Pedersen, S. F., & Myers, A. M. (2011).
Understanding the principles of organic
chemistry: A laboratory course​. Belmont, CA:
Brooks/Cole.
[3] ​What is fractional distillation? - Definition &
process. (n.d.). Retrieved from
https://study.com/academy/lesson/what-is-fracti
onal-distillation-definition-process.html#lesson