DISTILLATION

PROCESS
Distillation:-
An important organic process used to separate two or more than two
liquids having different boiling points from a liquid mixture.

• Distillation is a method of separating mixtures based on differences in volatility

(vapourpressure) of the components in a boiling liquid mixture

• It is used in pharmacy either to extract volatile active principles from vegetable

drugs or to separate volatile substances from less volatile impurities.

An organic process used to separate a liquid

organic compounds from a solid substance.
 Definition
Ø Distillation An important organic process used to

separate two or more than two liquids having different

boiling points from a liquid mixture.

ØDistillation is a physical separation process, not a chemical

reaction to purify an impure liquid.
 Principle of distillation
1) Distillation method basis on the difference in boiling point of the
components of the mixture at standard pressure conditions.
2) At any boiling temperature a liquid is in equilibrium with its vapor.
3) This equilibrium is described by the vapor pressure of the liquid. The
vapor pressure is the pressure that the molecules at the surface of
the liquid exert (try) against the external pressure, which is usually
the atmospheric pressure.
 How does it work
1) As the mixture is heated, the temperature rises until it reaches the
temperature of the lowest boiling substance in the mixture,
2) The other components of the mixture remain in their original phase
in the mixture.
3) The resultant hot vapor passes into a condenser and is converted to
the liquid, and then collected in a receiver flask.
4) The other components of the mixture remain in their original phase
until the most volatile substance has all boiled off.
5) Then the temperature of the gas phase rises again until it reaches
the boiling point of a second component in the mixture, and so on.
 distillation techniques depends on several factors

1) The difference in vapor pressure (related to the difference in the

boiling points) of the components present.

2) the size of the sample.

3) The distillation apparatus.
 Application of distillations
Distillation is used to:
Separation of volatile oils- cloves(Eugenol comprises 72- 90%, Vanilin, acetyl eugenol).

Separation of drugs obtained from plant and animal sources- Vit. A from fish liver oil.
Purification of organic solvents-absolute alcohol (100%).
Purification of drugs obtained from chemical process.
Manufacture of official preparations -sprit of nitrous ether,
sprit of ammonia, D.water and water for inj.
Quality control methods- Alcohol content in elixir(4-40%).
Refining of petroleum products- Petroleum ether 60,80.
Recovery of solvents- synthesis.
 According to the differences in boiling
points between the liquids, distillation process
classified into four types:-

1-Simple distillation. 3-Steam distillation.

2-Fractional distillation. 4-destructive

distillation.
Simple distillation:-
Simple distillation is the process of converting a liquid into its vapour,
transferring the vapours to another place, and recovering the liquid by
condensing the vapours
Under atmospheric pressure
1. Under reduced pressure
Example:-
Separation diethyl ether (B.P=34°C), from dioxane (B.P=101°C).
Separation chloroform (B.P=60°C), from an oil (B.P=220°C).

* Separation of a liquid substances from the

solid substances in a mixture.
Example:-
Separation H2O (B.P=100°C), KMnO4 (B.P ≥ 240°C).
Simple distillation components:-
Any simple distillation system composed from the following main parts:-

1-Heating source.

2-Distillation flask (Still).

3- Thermometer.
4- Condenser.
5- Receiving flask .
Separation of liquid mixture by simple distillation:-
1. A mixture composed of (acetone) and (water) with boiling point (56 &
100) °C respectively is heated.
2. The lowest boiling point (acetone) will vaporized and ascended
(elevated) from the solution till it reach the top of the system, with
recording its real b.p. with the help of thermometer.
3. The ascended (rises) vapor (acetone) will converts to the liquid form by
the action of the condenser, then collect at the receiver.
4. Finally the highest boiling point (water) will remain in the distillation
flask.
As a result, simple distillation is effective only when the liquid boiling points differ greatly (rule
of thumb is 25 °C or when separating liquidsfrom non-volatile solids or oils.
 Simple distillation under reduce pressure

• Liquid boils when vapour pressure is equal to the atmospheric

pressure, i.e., pressure on its surface. If the external pressure is
reduced by applying vacuum, the boiling point of liquid is
lowered.
• Therefore, the liquid boils at a lower temperature. This principle is
illustrated using an example of water.

• Thermolabile liquids, the liquids which are unstable at their

boiling point under atmospheric pressure , are distilled at a
much lower temperature under reduce pressure with less
likelihood of decomposition.
• Also used for concentrating thermo-labile substances.
• This process is used in the purification of vitamins
 Distillation apparatus for simple distillation
under reduce pressure

Vacuum distillation is mostly carried

out in Claisen flask, which has two
necks
• Second neck prevents splashing of
the violently agitated liquid.

•Vacuum pumps, suction pumps, etc. are

used to reduce the pressure on the liquid
surface.
FRACTIONAL
DISTILLATION
Fractional Distillation:-

Second technique of the distillation process, used to separate two

liquids having close (near) boiling points (Lower than 25 °C).

Example:-
Separation of ethanol (78) °C from
water (100) °C
.
Fractional distillation components:-
Fractional distillation system composed from the following main parts:-

1- Heating source.
2- Distillation flask.
3- Fractional column.
4- Thermometer.
5- Condenser.
6- Receiving flask .
Fractional Distillation Set-up
FRACTIONAL DISTILLATION

• This method is also known as rectification, because a part of

• the vapour is condensed and returned as a liquid.

• This method is used to separate miscible volatile liquids,

whose boiling points are close, by means of a fractionating column.
Simple Distillation Vs Fractional Distillation

• In simple distillation, vapour is • In fractional distillation the

directly passed through the vapour must pass through a
condenser. fractionating column in which
partial condensation of vapour
is allowed to occur.

• Condensation takes place in the

• Condensate is collected directly
into the receiver, fractionating column, so that a
part of the condensing vapour r
eturns to the still.
 Principle:

• When a liquid mixture is distilled, the partial condensation of the

vapour is allowed to occur in a fractionating column.

• In the column, ascending vapour from the still is allowed to come

in contact with the condensing vapour returning to the still.
• This results is enrichment of the vapour with the more volatile
component.
• By condensing the vapour and reheating the liquid repeatedly,
equilibrium between liquid and vapour is set up at each stage, which
ultimately results in the separation of a more volatile component.
The liquid with higher boiling point is condensed first and vapour becomes richer
with the liquid having the lower boiling point which gets
• Applications:
• Fractional distillation is used for the separation of volatile miscible
liquids with near boiling point such as
• •Acetone and water
• •Chloroform and benzene
Fractionating columns

• In fractional distillation, special type of still-heads are required so that

condensation and re-vaporisation are affected continuously.
• These are known as fractionating columns.
• A fractionating column is essentially a long vertical tube in which the
vapour passes upward and partially condensed. The condensate flows down
the column and is returned eventually to the flask.
• The columns are constructed so as to offer the following advantages
simultaneously.
• (1) It offers a large cooling surface for the vapour to condense.
• (2) An obstruction to the ascending vapour allows easy condensation.
Steam Distillation (Distillation of two immiscible
liquids)

• Steam distillation is a special type of distillation for temperature

sensitive materials like natural aromatic compounds.
• • Many organic compounds tend to decompose at high sustained
temperatures.
• Separation by normal distillation would then not be an option, so
water or steam is introduced into the distillation apparatus.
• By adding water or steam, the boiling points of the compounds are
depressed, allowing them to evaporate at lower temperatures,
preferably below the temperatures at which the deterioration of the
material becomes appreciable.
• A mixture immiscible liquids boils when sum of their VP= ATM
• BP Water 100 c, turpentine is 160C, mix BP 95.5
• At 95.5 C = VP(647 water+ 113 turpentine) =760mm which is atm
• • If the substances to be distilled are very sensitive to heat, steam
distillation can also be combined with vacuum distillation.
• • After distillation the vapors are condensed as usual, usually yielding
a two phase system of water and the organic compounds, which can
be
• separated because they are immiscible
• • Conclusion:
• • Steam is used to reduce the boiling point of a liquid to be distilled
Steam distillation apparatus
Application of steam distillation

• Steam distillation is employed in the manufacture

• of essential oils, for use in perfumes, for example. In this
• method, steam is passed through the plant material
• containing the desired oils.
• • Eucalyptus oil and orange oil are obtained by this method
• on the industrial scale.
• • Steam distillation is also sometimes used to separate
• intermediate or final products during the synthesis of
• complex organic compounds.
• • Steam distillation is also widely used in petroleum
• refineries and petrochemical plants.
Azeotropic mixture

• An azeotrope is a mixture of two or more liquids in such a ratio that

its composition cannot be changed by simple distillation.
• This occurs because, when an azeotrope is boiled, the resulting vapor
has the same ratio of constituents as the original mixture.
• • Because their composition is unchanged by distillation, azeotropes
are also called constant boiling mixtures.
• • Thus a mixture behaves like a pure liquid
• • Such a mixture cannot be separated into pure liquid.
DESTRUCTIVE DISTILLATION (DRY DISTILLATION)
• This is also known as Dry Distillation. The dried organic matter is
heated in the absence of air, in a suitable apparatus, until all the
volatile substances are driven off and the residue is left behind.
• The residue is subjected to carbonisation.
• Destructive distillation is mainly used in industry for obtaining many
valuable products from wood and coal.
• Destructive distillation of wood gives acetone, menthol, cresol, wood
tar etc. while charcoal remains in the still.
• Destructive distillation of coal gives burning gases the ammonia, and
the coke remains in the still.
• Destructive distillation of animal bones gives ammonia, amines and
• hydrocarbons.