Experiment 6

Experiment 6
Title: Simple and Fractional Distillation
Objective:
The main objective of this project is to separate and purify the liquid compounds
by simple and fractional distillation and hence to learn the technique of
distillation.
Theory:
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 the external pressure (acting on the surface of the liquid).
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 whereas
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,
Fractional Distillation. As it is not possible to separate components in a mixture of

pure
form and desired quantities by simple distillation, it is necessary to perform a
Fractional Distillation. Fractional distillation must be used to achieve good
separation when boiling point differences between the components in a mixture
are not large, and highly pure components are desired. In fractional distillation, a
fractionating column is introduced between the distilling flask and the still head.
The fractionating column is packed with suitable material such as a stainless
steel sponge. Alternatively, Vigreux Column can be used. When heated, the
vapors generated from the boiling flask move up through the packing material in
the fractionating column, where the components in the liquid mixture are
subjected continuously to many vaporization-condensation cycles. The rising
vapors that have low boiling liquid components are passed on to the condenser,
cooled to provide the liquid. The higher boiling component is then returned to the
boiling flask. The highly volatile or lower boiling component ascends the
fractionating column in the vapor stream whereas the low volatile or higher
boiling liquid descends in the condensate stream in the fractionating column. In
effect, vapor and condensate are passing through the fractionating column in
opposite directions.
Procedure:
So firstly, we heat the liquid mixture of methanol and water.

As the liquid heats, components with the lower boiling points will begin to
vaporize and rise through the column. Here in our case methanol will boil off first
(BP 65° C, compared to water (BP 100° C). However, the vapor rising will still
contain some molecules of the other substances.
Vapor gets purer the higher it rises in the column, as heavier molecules “fall off”
and turn back to liquid.
As vapor rises in the distillation column, heavier molecules will condense back
into liquid and “rain” back down. At any given point in a fractionating column,
vapor will be rising, the liquid will be falling, and molecules will be mixing.
Columns naturally have certain “stages”; a stage is an area in the column with a
similar amount of molecules of each type of substance (i.e. a general certain
percentage of water and methanol). Columns are designed to be tall enough to
achieve a certain percentage separation, by finding the minimum number of
required stages.
Vapor reaching the top of the column (distillate) is collected into an industrial
condenser (a big chiller), which cools the vapor back into a liquid, and is piped to
a tank or storage.
Substances remaining in the column continue the process of distillation until the
desired purity is reached. Some columns are a continuous process (most
common), where the new base solution is added continually. Others are batch
systems, where the base is removed when the desired separation is achieved. In
many systems, the solution is recirculated several times to make sure
substances are properly separated.
Observations
Simple Distillation Fractional Distillation

Post Laboratory Questions.
1. Describe the behavior on the fractional distillation of 50% methanol (X=
methanol; Y = water) through an efficient column. Refer to Figure 6.3.
It has been observed that during the fractional distillation, in quite a few readings
the temperature lies between the boiling point of the individual substances.
Compared to simple distillation, fear in fractional distillation the range of such
values is broad, this is mainly because at 50% liquid concentration equilibrium
with the paper containing 80% of methanol.
2 Why is it dangerous to heat an organic compound in a closed container or in a

distilling assembly (simple or fractional distillation) that is closed at every point
(no vent or opening) to the atmosphere?
Ans: We know that while we heat a compound in a distilling assembly the

compound starts to boil. After boiling the compound goes to the vapor phase.
Thus with the increase in heating, more vapors are formed. As a result, the vapor
pressure increases by multiple times than the previous compound. Hence, the
vapor tries to lessen its pressure by expand and forms a severe strain on the
walls of the pipes or containers. Hence, if this is done in a system without a vent
or opening, this may lead to an explosion. Hence, heating a compound in a tight
chamber without a vent or openings is very dangerous.
3. Explain the terms:
Simple distillation: Simple distillation is a process in which a mixture of organic

substances are separated if their boiling points differ by more than 40 °C.
Ideal solution: An ideal solution may be defined as one which obeys Raoult's law
over all concentration range at a given temperature.
4. Comment on the green chemistry of this experiment. That is, the nature
and amount of solvent (for example water, etc.), and atom economy
(number of atoms in the reactants versus products) in this experiment
Ans: In this particular experiment of distillation used a mixture of water and

methanol in equal proportion. Since the main purpose of this experiment is
to separate the mixture we can easily term that none of the reactance is
wasted, hence we can turn this experiment completely green.

Experiment 6 - Distillation

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Title: Simple and Fractional Distillation

Simple Distillation. Simple distillation is used to purify a single liquid. When a

Fractional Distillation. As it is not possible to separate components in a mixture of

So firstly, we heat the liquid mixture of methanol and water.

Simple Distillation Fractional Distillation

2 Why is it dangerous to heat an organic compound in a closed container or in a

Ans: We know that while we heat a compound in a distilling assembly the

3. Explain the terms:

Simple distillation: Simple distillation is a process in which a mixture of organic

Ans: In this particular experiment of distillation used a mixture of water and

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