Distillation: Simple Organic Chemistry Lab Manual

Activity No. 9
Simple Distillation

Distillation is one of the widely used techniques for separation and purification of liquid
mixtures. The process is done by boiling the mixture and allowing the lower-boiling component of the
mixture to vaporize and condense by passing through a condenser and be collected in a receiver flask
while the higher-boiling component remains in the distilling flask. There are several distillation methods:
simple, fractional, steam and vacuum. Each has its own limitations and advantages.

Simple distillation is only effective when the components of a liquid mixture have wide
differences in boiling points, about 50o or more. To ensure maximum efficiency in carrying out the
process, superheating, irregular ebullition or bumping and temperature fluctuations must be avoided.
Therefore, the following measures must be adapted: a) use medium heat b) add a few boiling chips
and c) insulate the distilling flask and the T-tube.

In this experiment, you will carry out separation of ethanol from beer. This experiment aims
for the student to learn how to properly assemble a simple distillation set-up and to gain experience in
carrying out simple distillation by attempting to isolate ethanol from its aqueous mixture. The ethanol
which has a lower boiling point (78.5oC) than water will vaporize and condense prior to water.

Fig. 1. Simple Distillation Set–up.

Dept. of Chem, MSU-IIT 2016-2017 Page 47

Distillation: Simple Organic Chemistry Lab Manual
The results of this experiment shall be plotted in a graph (temperature versus volume of
distillate). A successful separation is achieved when the first component is removed completely at its
boiling point before the second component distills over. From the graph, the student can gauge
whether simple distillation is effective for the separation. The result of this experiment will be compared
to the result of the next activity which fractional distillation using the same brand of beer.

APPARATUS AND MATERIALS:

500 ml distilling flask t-tube 10 mL graduated cylinder (2)
condenser adapter 100-ml graduated cylinder
iron clamp (3) long rubber tubing (2) pinch clamp (2)
aspirator crucible tong aluminum foil
boiling chips (3) iron stand (2) 50 mL beaker
crucible cover hot plate matches
thermometer long-stem funnel test tubes (9)

CHEMICALS :
beer sample ( any brand )

PROCEDURE:
1. Assemble a distillation set-up as shown in the kit manual, with the help of the laboratory
technician. Laboratory equipment for distillation set-up have different sizes, e.g. 19/24, the
number referring to the diameter and length in mm of the ground glass joint. Choose ground-
glass joint fittings of the same specifications. To ensure vacuum tightness, place a small amount
of grease in every glass joint connections (to do this, apply thinly at the center). Use rubber
tubing as inlet and outlet of water. Be sure to open the water source before starting the
distillation. The whole condenser must be filled with water and there must be a continuous flow
of water from the source.
2. By means of a clean, dry funnel, introduce 100 mL of the beer sample into the distilling flask and
add a few (2 or 3) tiny boiling chips. Reassemble the set-up. The position of the thermometer
must be such that the 70oC mark can be seen above the rubber connector. At this position also,
the tip of the mercury bulb must be at the same level the opening of the side arm of the adapter.
Cover the distilling flask and adapter with aluminum foil.
3. Set the hotplate at medium heating and distill the mixture using a 10 mL graduated cylinder as
your receiver.

Dept. of Chem, MSU-IIT 2016-2017 Page 48

Distillation: Simple Organic Chemistry Lab Manual

4. Note the color and odor of the distillate. Distill the mixture slowly at a rate of not more than 2
mL/minute.
5. Record the temperature at the first drop of distillate and in the succeeding volumes of distillate.
Change the receiver after the collection of each fraction. Transfer 6 drops of the collected
fraction to a crucible cover and ignite using a match. Observe closely against a black background.
Note relative intensity of the flame and indicate results as:
( - ) , (+) , ( ++), or ( +++). Transfer the remaining distillate to another container.
6. Continue the distillation and record the temperature for every 2 mL fraction collected thereafter.
For each fraction, test for combustion. Transfer the remaining distillate in the receiver after
every test for combustion.
7. Stop the distillation after 15 mL of distillate has been collected.
8. Graph temperature (y-axis) versus volume of distillate (x-axis).

Dept. of Chem, MSU-IIT 2016-2017 Page 49