This experiment is a technique lab on

separating and purifying compounds by

distillation and on using GC to analyze
samples.
Distillation is a frequently-used technique
involving boiling and condensing and is
used for mixtures of liquid compounds that
have different vapor pressures (different
boiling points). When a liquid mixture is
boiled. the vapors above the liquid are
richer in the lower-boiling component.
Condensing these vapors results in a
purified sample. Figure 1 shows a typical
laboratory setup for a simple distillation.
When the difference in boiling points of the
components is large
(40-60 °C), a fairly good separation often
can be made with a simple distillation
(Figure 2b). When the difference in boiling
points of the components is small, then a
simple distillation cannot achieve a good
separation (Figure 2a). If a better
separation is desired when the
components have similar boiling points,
then a fractional distillation can be done.
The simple distillation setup in Figure 1 can
be converted to a fractional distillation
setup by inserting a fractionating column at
number IT in the figure. The fractionating
column can be thought of as a place where
the vapors condense and then boil again.
Each time a very small sample condenses
and then boils again, the vapor is even
more enriched in the more volatile (lower
boiling) component. Thus, fractional
distillation can produce samples that are
much purer. This increase in purity comes
with a cost of more complex equipment
and more distillation time.
Chemists use four basic methods of
distillation: Simple distillation, fractional
distillation, steam distillation, and vacuum
distillation. You will learn steam distillation
in the next experiment (Experiment # 7).
Chromatography is another method used
to purify the solids as well as liquids.
Simple Distillation. Simple distillation is
used to purify a single liquid. When a single
liquid is boiled, the liquid is converted into
vapor. The vapor rises from the distillation
flask and touches the thermometer, which
records the vapor temperature. The vapor
then goes through the condenser where it
is liquefied by cold circulating water. The
liquid then passes from the condenser into
the receiving flask. The thermometer reads
the constant temperature (boiling point
within 1-2° C range) throughout the
distillation. A liquid boils when its vapor
pressure equals to the external pressure
(acting on the surface of the liquid). The
normal boiling point (b.p) of a liquid at 1
atmosphere is defined as the temperature
at which (a liquid boils) when its vapor
pressure equals to 1 atmospheric pressure.
Simple distillation can be used to purify
single compounds or a liquid mixture
containing two components with widely
differing boiling points. For a pure
compound, the temperature remains the
same throughout the distillation where as
for a liquid mixture; the temperature most
often does not remain the same. That is
because the composition of the distilling
vapor varies continuously during the
distillation. Three types of temperature
behavior during simple distillation are
shown in Figure 6.1. First, for a pure liquid
X, the temperature remains constant.
Second, for a liquid mixture X+Y with a
narrow b.p. difference of 1-15° C the
temperature gradually increases. Third, for
a liquid mixture X+Y with a larger b.p.
difference of 100° C, the temperature
remains constant until one of the low
boiling components 'X' distills over; then
suddenly temperature jumps to a higher
temperature when the higher boiling
component 'Y' distills over and remains
constant.