Fractional Distillation CHM032.

2 Organic Chemistry for Teachers Laboratory

ACTIVITY No. 8

Fractional Distillation

Fractional distillation is a more efficient method of separation or purification of liquid

mixtures than simple distillation. The principle involved here is based on the use of a fractionating
column inserted vertically between the distilling flask and the condenser, allowing better separation
of the components of a liquid mixture.

There are different types of fractionating columns. The Hempel column is most commonly
used in the laboratory. It is composed of a vertical glass tube or distilling column which is filled
with some kind of packing material like glass or porcelain beads, chunks of glass tubing, glass
helices or copper turnings. In the Vigreux column, the glass tube does not contain any packing
but is composed of a series of sharp indentations. Another type of fractionating column is the
spiral wire column. The wire inside the column is inert to most materials and serves as good
conductor establishing an efficient heat exchange between column and surrounding. Some
columns are provided with heating jackets for careful control of temperature.

The packing material or indentations in the fractionating columns serve as surfaces on

which condensation of vapors can take place. As the vapors continue to ascend, the lower-boiling
component escapes through while the higher-boiling component condenses and returns to the
flask. In this manner, the lower-boiling component is steadily being “scrubbed” free of the other
higher-boiling component. Each then becomes richer in amount as distillation continues and thus
separation is achieved. When the lower-boiling component has distilled over, distillation
temporarily stops. During this time, the heating maybe cautiously increased. A sharp rise in boiling
point is then observed as the second fraction starts to distill (Mann and Saunders, 1960).

When efficiently conducted, one fractional distillation can effectively separate the
components of a mixture which by simple distillation can only be achieved by a series of separate
distillations. A mixture of methanol (Tb 66 oC) and water, for instance, can be effectively separated
into its components by a single fractional distillation even though their boiling point difference is
only 34 oC.

In this experiment, fractional distillation will be carried out using the same brand of beer
sample used in the simple distillation experiment. This process can only concentrate the mixture
by as much as 95% but cannot effectively separate pure ethanol from the sample. This is because
ethanol forms a binary azeotropic mixture with water. As an azeotrope, it gives a vapor of the

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 Fractional Distillation CHM032.2 Organic Chemistry for Teachers Laboratory

same composition (95% ethanol and 5% water) at 78.1 oC and hence cannot be further
concentrated by distillation no matter how efficient the fractionating column. One way of obtaining
absolute ethanol or 100% ethanol is by conducting several fractional distillations of an azeotropic
ternary mixture of 95% ethanol, water and benzene.
This experiment allows the students to compare the relative efficiency of simple and
fractional distillation.

Fig.1. Fractional Distillation Set-up

APPARATUS AND MATERIALS:

500-mL distilling flask T-tube condenser
adapter small pieces of broken glass long rubber tubing (2)
fractionating column pinch clamp (2) thermometer
boiling chips 100-mL beaker 50-mL beaker (2)
10-mL graduated cylinder (2) iron clamp (3) crucible cover (3)
test tube brush long-stemmed filter funnel aluminum foil
hot plate wire gauze iron stand (3)

CHEMICALS:
beer (same brand used in simple distillation)

PROCEDURE:
1. Assemble a fractional distillation set-up as shown in Figure 1. Choose the long and narrow
condenser tube as your fractionating column. Some condensers have protrusions at the
lower end, designed to hold packing materials. For condensers which are not conveniently

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 Fractional Distillation CHM032.2 Organic Chemistry for Teachers Laboratory

designed in this manner, the bottom is sealed by placing across the column a very fine
glass rod or glass wool on which the packing may rest. It is not advisable to constrict the
column at the bottom as this can cause “choking” of the column during distillation. Use
glass beads or small pieces of broken glass as your packing material.
2. By means of a filter funnel, pour 250 mL of beer into the flask. Add 2 or 3 tiny pieces of
boiling chips. Reassemble the set-up. Wrap the distilling flask, column and adapter with
aluminum foil (double the wrapping) to protect the set-up from drafts.
3. Adjust the hot plate to moderate/medium setting. Distill the mixture very slowly at a rate
of not more than 2 mL/minute.
4. Record the temperature at the first drop of distillate and in the succeeding fractions of
distillate. Note the color and odor of the distillate. Change the receiver after the collection
of each fraction.
5. Test each fraction of distillate for combustion as done in the simple distillation experiment.
Place an inverted crucible cover over a 50-mL beaker. Transfer an amount of the distillate
just enough to cover the bottom of the crucible cover. Ignite with a lighted match. Observe
closely against a black background. Note the relative intensity of the flame and indicate
results as: (+++) for blue flame, (+) for yellow flame, and (―) for no flame.

Transfer the remaining distillate into the 50-mL beaker.

6. Collect 1 mL of the distillate, note the temperature and test for combustion. Record your
observations. Transfer the rest of the distillate into the 50-mL beaker.
7. Collect the next 2 mL fraction. Note the temperature and test for combustion. Record
your observations. Transfer and combine the remaining distillate. Do the same for every
succeeding 2-mL fraction of distillate collected. Stop the distillation after a total of 15 mL
of distillate has been collected or when two consecutive fractions are no longer
combustible.
8. Plot a graph of the temperature (y-axis) versus the volume of distillate (x-axis).
9. Plot another graph showing the results of the two distillation methods using different ink
color for each type of distillation. Compare the efficiency of the two methods.

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References:
Kenneth Williamson and Katherine Masters. Macroscale and Microscale Organic Experiments.
Cengage Learning, Incorporated. 2011.

Pavia, Donald. Introduction to Organic Laboratory Techniques. 5 th International Edition. Cengage

Learning, Incorporated. 2012.

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