PETE218 Atmospheric Distillation Spring 2015-2016

Atmospheric Distillation
Distillation is the most common method used to separate and purify liquids. The process
consists of heating a liquid to its boiling point, conducting the vapors to a cooling device where they
are allowed to condense, and collecting the condensate. Also, simple distillation is a reasonable way
to determine boiling point. One can load the pot with a pure unknown liquid and very carefully and
slowly distill it. The still head temperature will quickly level off. The range of temperatures observed
at the still head during the temperature plateau is the boiling range of the unknown liquid. Since the
boiling point is related to the structure of the compound, knowing the boiling point can be useful in
identifying the compound.

To understand distillation, first consider what happens upon heating a liquid. At any temperature,
some molecules of a liquid possess enough kinetic energy to escape into the vapor phase (evaporation)
and some of the molecules in the vapor phase return to the liquid (condensation). An equilibrium is
set up, with molecules going back and forth between liquid and vapor. At higher temperatures, more
molecules possess enough kinetic energy to escape, which results in a greater number of molecules
being present in the vapor phase.

A liquid is boiling when the vapor pressure of the liquid equals that of the atmosphere giving the liquid
the maximum rate of escape into the vapor phase. If a liquid has a low boiling point, its intermolecular
forces are low and less energy is needed for molecules to escape into the vapor phase at their
maximum rate. So, if a liquid has a low boiling point, it has a higher vapor pressure at any
temperature, but the maximum rate of escape can be achieved at a relatively low temperature. It is
important to realize that like other phase changes, boiling is an equilibrium process. When a liquid is
boiling the escaping tendency of the liquid into the gas phase equals that of the gas into the liquid
phase.

The preceding discussion also opens up the idea that there is a relationship between the atmospheric
pressure and the boiling point. That is, the more the atmosphere weighs down on the liquid, the
greater the energy input must be to have those molecules escape at a high rate. On a high-pressure
day, boiling point of a compound will go up and on a low pressure day it will go down.

The key step is to raise the temperature of the mixture to a point above that of the compound with
the lower boiling point. But you also have to make sure it's below that of the compound with the higher
boiling point. The compound with the lower boiling point will then evaporate, leaving behind the
compound with the higher boiling point. If the vapor is then condensed, you're only going to have the
compound with the lower boiling point, since you separated the two compounds.

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PETE218 Atmospheric Distillation Spring 2015-2016

Note that simple distillation is effective only when separating a volatile liquid from a nonvolatile
substance or when separating two liquids that differ in boiling point by 30-40 degrees or more. If the
liquids comprising the mixture that is being distilled have boiling points that are closer than 30-40
degrees to one another, the distillate collected will be richer in the more volatile compound but not to
the degree necessary for complete separation of the individual compounds.

Experimental Set-up

Essential elements of an atmospheric distillation setup are:

• Thermometer
• Heating mantle
• Condenser
• Cooling Water
• A Pot
• Distillate/Receiver flask

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PETE218 Atmospheric Distillation Spring 2015-2016

Experiment Procedure
1. Fill the distillation flask. The flask should be no more than two thirds full because there needs
to be sufficient clearance above the surface of the liquid so that when boiling commences the
liquid is not propelled into the condenser, compromising the purity of the distillate.
2. Put the container with liquid inside into the heating mantle, and dip the sensor into heating
liquid.
3. Switch on the power accords with the machine, then the equipment screen will show the
current temperature of heating liquid.
4. Always keep cold water running through the condenser, enough so that at least the lower half
is cold to the touch. Remember that water should go in the bottom and out of the top.
5. Heat the distillation flask slowly until the liquid begins to boil. Vapors will begin to rise through
the neck of the distillation flask. As the vapors pass through the condenser, they will condense
and drip into the collection receiver. An appropriate rate of distillation is approximately 20
drops per minute. Distillation must occur slowly enough that all the vapors condense to liquid
in the condenser. Many organic compounds are flammable and if vapors pass through the
condenser without condensing, they may ignite as they come in contact with the heat source.
6. When the displayed temperature reaches the setting point, the red indicator light will be
lighten, then it gets into constant temperature state.
7. Adjust the RST knob to the left side, where is the smaller value position; wait until the
temperature does not rise anymore, for example, when the displayed temperature is lower
than the setting temperature, then turn it to right side gradually.
8. Collect each compound in receiver flasks.