CM133L Organic Chemistry Laboratory

1st Quarter SY 2022 - 2023

Fractional Distillation
Aspuria, Aicee Julliane I.1, Badillo, Allyssa Sophia, R.1, Caalim, Alexandria Nicole A.1

CM133L/A21, School of Chemical, Biological and Material Engineering and Science, Mapua University
1

ABSTRACT

This experiment was conducted to separate mixtures of volatile liquids with relatively close boiling points using fractional
distillation technique. A mixture containing equal amounts of Toluene and Carbon Tetrachloride were experimented – letting
the substance with lower boiling point evaporate first, isolating it from the higher boiling point compound. Due to the errors
done while setting up the fractional column, the experiment did not yield any result. Although the aforementioned process is a
great technique for volatile liquid separation, it was deemed to be highly complicated to perform. Simply put, proper packing of
glass fibers inside the column was not accomplished. The overly tight packing condensed the vapor too quickly, not letting it
go up the column. Hence, the experiment procedure was terminated even before the first distillation process was finished. It is
therefore recommended for future researchers to carefully and properly pack glass wool and glass beads in the fractional
column. Since there is no exact amount for this process, it is necessary to know the concepts before the actual experiment to
avoid encountering such errors.

Keywords: Volatile Liquids, Fractional Distillation, Glass Beads, Separation Technique

INTRODUCTION

Distillation is a separation process of two or more
compounds depending on their boiling points – the
temperature wherein the vapor pressure of the liquid
matches and becomes equal to the outside pressure
exerted on its surface. In this method, the lower-boiling-
point substance evaporates first, separating it from the
compound with higher boiling point. The sample solution is
put in a container, then a part of it vaporizes and condenses
in a different container, collecting all the distillate.
To achieve a purer substance, Fractional Distillation is used
to separate mixtures of liquids with similar boiling points
(closer than 50 degrees to one another). The vapor rises
when the mixture is heated and enters the fractionating
column. As it cools, vapor condenses on the packing
material of the column. This liquid is forced to evaporate
once again by the heat of increasing vapor, advancing it up
the column which finally produces a higher purity sample of
the mixture's more volatile component (condensate). This is
why fractional distillation leads to a better separation than
simple distillation.
This laboratory work offers practice utilizing fractional
distillation to break down a homogenous mixture or solution
into its pure constituents. This physical method of
separation is widely used in both the laboratory and in
business. On a massive production scale, it is applied to
refine petroleum into the "fractions" that are used for
gasoline, heating oil, and things alike. On the other hand, I t
is used in the laboratory every time a combination of liquids
is needed to be separated. Moreover, fractional distillation
may be used to determine the unknown components of a
solution by recording the boiling temperature of the
collected fractions and observing its other physical
characteristics.
In a nutshell, the objectives of this experiment include the
following:
- Practicing how to assemble the set up for fractional
distillation
- Purify compounds using fractional distillation
- Understand the concepts underlying this separation
technique and apply it in real life situations
MATERIALS AND METHODS
To achieve the objectives of this experiment, the laboratory
assistant demonstrated to the student researchers how the
procedures must be done. Due to its lengthy process, it was
not done per group but was just observed as a class. The
materials needed to carry out a fractional distillation

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includes the following: Quick fit, hot plate, thermometer, and
reagents being experimented.
As part of the demonstration, the laboratory assistant
assembled the set-up as shown in Figure 1. It is crucial to
dry all the glassware before doing so. The pear shaped
flask was filled with 10mL of Carbon Tetrachloride (CCl4),
10mL of Toluene (C6H5CH3), and a small amount of glass
beads. The fractionating column was then packed with
glass wool and beads alternately. This part was done very
cautiously while wearing googles and gloves since glass
fibers are hazardous to touch and breathe.
Figure 1. Fractional Distillation Set-up
After fitting all the parts of the set-up, the distillation process
was started by turning the hot plate on. Five bottles (test
tube fitted with cork or graduated cylinders) were prepared
and labelled according to the table below.
Table 1. Bottle Labels for First Distillation
Temperature Range Label
76 – 80 °C A in it.
81 – 88 °C B
89 - 98 °C C Then, collect distillate fraction from temperature ranges of
99 – 106 °C D 76–80°C, 81–88°C, 89–98°C, and 99–106°C in bottles F,
107 – 111 °C E
Experiment 04│ Group No. 2│ September 11, 2022
Due to the errors done while setting up the fractional
column, the experiment was terminated at this part.
However, to serve as reference for future researchers, the
proceeding steps must be conducted. Fractions of distillate
coming out at the temperature range given Table 1 must be
collected accordingly. Once the temperature reaches
107°C, the hot plate can be switched off. The remaining
liquid in the column must be allowed to drain in the pear
shaped flask, cooled to room temperature, and transferred
to Bottle E. The researcher can then measure the volume of
the distillate gathered and record in the data sheet.
The second distillation can be performed by pouring the
liquid in Bottle A in a round bottom flask. Obtain another set
of bottles and label them based on Table 2.
Table 2. Bottle Labels for Second Distillation
Temperature Range Label
76 – 80 °C F
81 – 88 °C G
89 - 98 °C H
99 – 106 °C I
107 – 111 °C J
The distillate collected at the temperature range of 76-80°C
must be placed in bottle F. Turn the hot plate off once the
solution reaches 80°C, drain the remaining liquid in the
column to a round bottom flask, cool it down to room
temperature, and pour Bottle B distillate from first distillation
in it.
After doing so, collect the distillate from temperature ranges
of 76–80°C and 81–88°C in bottles F and G, respectively.
Turn the hot plate off once the solution reaches 88°C, drain
the remaining liquid in the column to a round bottom flask,
cool it down to room temperature, and pour Bottle C
distillate from first distillation in it.
In the same manner, collect distillate fraction from
temperature ranges of 76–80°C, 81–88°C, and 89–98°C in
bottles F, G, and H, respectively. Turn the hot plate off once
the solution reaches 98°C, drain the remaining liquid in the
column to a round bottom flask, cool it down to room
temperature, and pour Bottle D distillate from first distillation
G, H, and I, respectively. Turn the hot plate off once the
solution reaches 106°C, drain the remaining liquid in the
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column to a round bottom flask, cool it down to room
temperature, and pour Bottle E distillate from first distillation
in it.
Lastly, collect distillate fractions at 76–80°C, 81–88°C, 89–
98°C, 99–106°C, and 107–111°C in bottles F, G, H, I, and
J, respectively. Like before, allow the remaining liquid in the
column to drain in the round bottom flask, cool it down, and
transfer it to Bottle I.
Record all volume obtained from each of the bottle in the
data sheet.
RESULTS AND DISCUSSIONS
In this experiment, fractional distillation technique is used to
separate a mixture of volatile compounds namely Toluene
and Carbon Tetrachloride. According to PubChem (n.d.),
Toluene appears as a clear colorless liquid with a distinctive
smell while Carbon tetrachloride has a heavy, sweet odor.
Their boiling points are 110.6 °C and 76.72 °C,
respectively, having a difference of only 33.88 °C.
When two compounds having relatively close boiling points
are heated using fractional distillation, the vapor that rises
above the liquid will be made up of both compounds at the
boiling point (Lower, 2022). For instance, two substances A
and B are mixed in equal ratios but A has a lower boiling
point than B. The vapor that rises above the liquid as the
combination begins to boil will be enriched with compound
A while still containing a substantial amount of compound
B. The mixture ratio would be 65:35 = A:B if compound A
were to enrich the vapor by 30%. It is to be noted that the
vapor transforms into a liquid with the same ratio as it cools
in the condenser.
The liquid that remained in the still pot after the first
distillation would contain higher amount of compound B.
The distillate of 65:35 = A:B must be transferred to a fresh
sample container and distilled once more to further purify A.
The distillate for the second cycle would be around 85:15 if
vapor was once more enhanced by 30% with compound A.
By the third cycle of this example, the distillate would be
pure A if the procedure continuously enriches the distillate
by 30%. The amount of compound A would thus need to be
increased through a succession of
Experiment 04│ Group No. 2│ September 11, 2022
vaporization/condensation cycles in order to surpass what
is achieved from a simple distillation set-up. The name
given to this series of cycles is Fractional Distillation.
The "fractionating" columns (part of the set-up) used in
fractional distillation are insulated to enable several
vaporization-condensation cycles to take place within a
single column. The more volatile (lower-boiling) component
vaporizes first, which passes through the packed material
or closely spaced "plates" that make up the fractionating
column. The vapor condenses on various surfaces inside
the column, which re-vaporizes due to the steam generated
from the bottom part of the set-up. The vapor gets
progressively enriched in the more volatile component
throughout each stage of the vapor/liquid equilibrium. The
mixture distills one component at a time in fractions with
enough theoretical plates - the region in the column where
the rising vapor and the re-condensing liquid reach
equilibrium. The Height Equivalent to the Theoretical Plate
(HETP), which measures separation power in such
systems, is the distance (length) between theoretical plates.
The purity of separated compounds will depend on how
long the column is, or how much plates it contains (Lab
Society, 2021). Consequently, each fraction will consist of
only a single pure substance with enough plates.
Here we can see that as a mixture goes through more
vaporization and condensation cycles, the better their
components’ separation will be. Although fractionating
column with more surface area improves separation, it also
increases processing time. Additionally, any liquid that cling
to the packing material's surface or pores won't continue to
evaporate, stopping the distillation process when the
packing material is drenched with the condensate. Liquid
hold-up is the term for this condensation on the column's
surfaces. This is the main reason why the experiment did
not gather any results. The concepts stated above were not
proven in actual using this laboratory work due to the
improper packing of glass wool.
CONCLUSIONS AND RECOMMENDATIONS
This week’s experiment led to the application of fractional
distillation technique by separating a mixture of two volatile
compounds with boiling points close to one another. The
researchers found that the aforementioned technique
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produces purer compounds as compared to simple REFERENCES

distillation which uses a shorter distillation column, allowing
less room for the different compounds to fully separate.
Although the researchers were taught enough knowledge to
make assumptions regarding the experiment’s results, the
objectives were not met due to certain errors encountered.
Lab Society. (2021, March 4). Fractional distillation [The
complete guide]. Lab Society - Buy Lab
Equipment
Online. https://labsociety.com/fractional-
distillation/

Overall, it can be concluded that although fractional Lower, S. (2022, February 20). 8.9: Distillation. Chemistry
distillation is a great technique for volatile liquid separation, LibreTexts. https://chem.libretexts.org/Bookshelve
it is highly complicated to perform. Proper packing of glass s/General_Chemistry/Book%3A_Chem1_(Lower)/
wool and glass beads inside the column must be done 08%3A_Solutions/8.09%3A_Distillation
accurately – not too tight nor too loose – because it serves
as the heart of fractional distillation. Packing it loosely PubChem.(n.d.). Toluene. https://pubchem.ncbi.nlm.nih.go
allows both fractions of the volatile liquid mixture evaporate v/compound/Toluene
and condense at the same time. Consequently, packing it
tightly condenses the vapor too quickly, not letting it go up
the column. In both cases, the experiment will not yield any
results. If it does, it will be highly inaccurate. Moreover,
failure to add enough boiling chips to the round bottom flask
allow molecules with higher boiling point gain kinetic energy
before those with lower boiling point, creating impure
fractions.

It is therefore recommended for future researchers to

carefully and properly pack glass wool and glass beads in
the fractional column. There is no exact amount for this
process so it is necessary to know the concepts before the
actual experiment to avoid encountering such errors. It is
also recommended to capture all parts of the experiment for
documentation purposes, especially to serve as proof and
basis when errors occur.

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