Simple Distillation
Introduction
(Adapted from Mohrig, pp. 109-112.)
The boiling point of a pure organic liquid is a physical property of that liquid. It is defined as the
temperature at which the vapor pressure of the liquid exactly equals the pressure exerted on it. Boiling
points can be determined using the technique of simple distillation. Distillation is a technique that is used
to purify a mixture of liquids or to obtain a boiling point of a pure liquid (in the case of this course).
Essentially, the liquid is heated to boiling and the vapors condensed above the boiling liquid.
Distillation is probably the most common technique for purifying organic liquids. In simple
distillation, a liquid is boiled and the vapors work through the apparatus until they reach the
condenser where they are cooled and reliquify. Liquids are separated based upon their
differences in boiling point. Two important things to note: 1) the tip of the thermometer must be
correctly positioned slightly below the center of the condenser to accurately reflect the
temperature of the vapors (see above left) and 2) the water supply should be connected to the
lower port in the condenser and the drainage tube connected to the upper (in the picture on the
right the right tube is connected to the water supply and the red tube is a drainage tube). Also be
sure to use the thin-walled tubing and not the heavy walled vacuum tubing. Be very careful that
your water lines do not come in direct contact with your hot plate, as the lines could melt
resulting in a flood. Be sure to clamp both the round bottom boiling flask and the collection tube.
Knocking over your collection tube at the end of the experiment if VERY frustrating. Below is a
diagram of assembly: Generally, boiling stones will be added to the boiling flask to ensure even
boiling. It is also wise to use some type of clamps to connect the various pieces of the distillation
apparatus together. For low boiling liquids, enough heat may be provided simply by resting your
flask on the hot plate (as shown above). You can also insulate your boiling flask and Claisen
adaptor with aluminum foil. For higher boiling liquids it may be necessary to use an oil or sand
bath to reach higher temperatures. The individual pieces of glassware needed for a simple
distillation are diagrammed below.
Simple Distillation
Introduction:
Simple distillation is used to purify a liquid mixture by a single vaporization-condensation step.
Simple distillation uses the differences in higher or lower boiling point of the liquid to separate
and purify the mixture.
The apparatus for a standard-scale simple distillation consists of a boiling flask attached to a still
head, thermometer adapter and a thermometer. Attached to the side of the still head is the
condenser, vacuum adaptor and the receiver flask, it is important to note that the water goes out
from the top and in through the bottom of the condenser. Also it is significant to make sure that
the tip of the thermometer is right above the opening of the boiling flask to ensure that the
correct temperature is being recorded. To ensure that the majority of the purified liquid is being
recovered, the correct size of the boiling flask should be used. For example if the theoretical
yield of final solution is 2.0 mL it would decrease the loss of product if a 50mL boiling flask
were used instead of a 250mL boiling flask.
When heating up a simple distillation apparatus either a hot plate or mantle are most commonly
used since they provide a constant temperature unlike a steam bath. Before starting to heat up a
simple distillation apparatus an approximate boiling point range should be noted to know what
temperature to keep constant. However, if there are multiple boiling point ranges it is best to
keep several receiver flasks to exchange during the different boiling point ranges. The best way
to determine optimal distillation rate is to count the drops going from the vacuum adapter into
the receiver flask. A good and stable distillation rate would be 1 to 3 drops per second into the
receiver flask. By having a significantly constant temperature and distillation rate it reduces the
amount of purified product lost. Finally, it is critical not to let the liquid mixture in the boiling
flask heat to the point that all of the liquid is gone. This is significant because if the boiling flask
is completely dry it might form either a solid that is extremely hard to clean off or an explosive.
