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.

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 includes 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

Methodology

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 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
81 – 88 °C B
89 - 98 °C C
99 – 106 °C D
107 – 111 °C E

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 ℃ , 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 7 6−80 ℃ must be placed in bottle F. Turn the hot
plate off once the solution reaches 80 ℃ , 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 ℃ , 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 9 8 ℃ , 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 in it.

Then, collect distillate fraction from temperature ranges of 76 – 80 °C, 81 – 88 °C, 89 – 98 °C, and 99 –
106 °C in bottles F, G, H, and I, respectively. Turn the hot plate off once the solution reaches 106 ℃ ,
drain the remaining liquid in the 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 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, n.d.). 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.

Conclusion

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 produces purer compounds as compared to simple 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.

Overall, it can be concluded that although fractional distillation is a great technique for volatile liquid
separation, it is highly complicated to perform. Proper packing of glass wool and glass beads inside the
column must be done accurately – not too tight nor too loose – because it serves as the heart of
fractional distillation. Packing it loosely allows both fractions of the volatile liquid mixture evaporate 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.

Lab Society (n.d.) - https://labsociety.com/fractional-distillation/

PubChem - https://pubchem.ncbi.nlm.nih.gov/compound/Toluene

Lower (2022) - https://chem.libretexts.org/Bookshelves/General_Chemistry/Book

%3A_Chem1_(Lower)/08%3A_Solutions/8.09%3A_Distillation