Distillation

Asif Massud
 Definition
Distillation is the process of separating the constituents
of a liquid by vaporizing the liquid and passing the
vapors through a cold surface thereby converting the
vapors again to the liquid.

It is the process of separating components of a

mixture based on different boiling points.

Distillation involves a change of state

from liquid to vapor and again to liquid
 Condenser
• The selection of suitable condenser is necessary for the success of many
distillation processes. An ideal condenser should have the following
characteristics:
• The construction of the condenser should be such that it can easily be
cleaned to remove even traces of previous product.
• The broken parts may be easily replaced so that the cost of a new
condenser is saved.
• It should provide the maximum cooling surface because the rate of
condensation is directly proportional to the cooling area.
• Condensing surface should be good conductor of heat therefore where
practicable metal condenser are preferred that glass container.
• The water used for cooling the surface must leave the condenser
quickly to provide space for fresh water to get in and provide cold
surface. The cooling water must flow in the opposite direction to that
of vapors to be condensed so that the condensed liquid should leave
the condenser in as cool a condition as possible.
 Different types of distillation are
• Simple distillation

Types of distillation • Fractional distillation

• Steam distillation
• Vacuum distillation
• Destructive distillation
Simple distillation
Explanation
• Simple distillation is the process of converting a
liquid into its vapors which are passed through a
cooling surface to condense the vapours.
• The condensed vapours are reformed into a liquid
which is collected in a receiver.
• The apparatus generally used for simple
distillation consist of still, the condenser and the
receiver depending on the suitability the apparatus
may consist of glass or metal.
Applications
• Simple distillation is mainly used for the
purification of organic liquids and for the
separation of liquids from non-volatile solids such
as recovery of alcohol in the preparation of dry
extracts.
• This process is also used in the preparation of
ether, amyl nitrate and spirit of nitrous ether.
• Distilled water is an important product which is
prepared by simple distillation process.
Fractional distillation
• Fractional distillation process is used to separate miscible volatile liquid's having different boiling points such as a
mixture of alcohol and water.
• Alcohol is more volatile than water therefore will evaporate at a faster rate than water. It is quite easy to separate a
liquid from non-volatile solids by simple distillation, but it is very difficult to separate two volatile liquids completely
from each other by a simple distillation.
• Such type of miscible liquids can be separated by using fractionating columns in between the still and the condenser.
A fractionating column is a device which increases the process of fractional distillation by condensing most of
vapours of less volatile component of the mixture and return it to the still whereas the vapors of more volatile
components of the liquid are allowed to pass to the condenser.
• The vapours are condensed there to reform the liquid which is collected in the receiver the liquid collected in the
receiver may not be a pure liquid therefore repeated distillation of the distillates may have to be carried out to get a
pure product.
Diagram
 • Fractional distillation process is used in the separation of two
miscible liquids having different boiling points. It is also used in the
Applications manufacture of alcohol by means of a special form of a still known as
Coffey's still .
 Steam distillation
• Steam distillation is used for the distillation of two immiscible liquids one of which is water.
• An immiscible liquid and water independently boils at high temperature but when steam is passed through a
mixture of these liquids it boils at a much lower temperature than the boiling point of pure water.
• The turpentine which has a boiling point of about 160 c° when mixed with water can be distilled at about
95.6 c° if a current of steam is passed through it.
• On laboratory scale the distillation apparatus consists of a steam generator fitted with a rubber bung having
two holes through one hole a long safety tube is passed which permits the expulsion of some water if
excessive pressure is generated inside the steam generator. Escape of steam from the safety tube indicates
that the steam can is almost dry.
• Through the other hole a bent tube is passed which carries the steam to the flask containing the liquids(
volatile liquid and small quantity of water) to be distilled.
 Steam distillation
• This tube must dip almost to the bottom of the flask the steam can and flask
containing the liquids are heated simultaneously so that a rapid current of
steam passes through the boiling mixture in the flask. The vapours are
allowed to pass through the condenser and condensed liquids are collected in
Florentine receiver.
• The distillate which forms two layers one aqueous another non-aqueous are
separated from each other as completely as possible. For this purpose, either
Florentine receivers or separating funnels are used.
• Florentine receiver is specially designed receiver meant for collecting the oil
and water in the same receiver. They are of two types; one type is used for
separating oils lighter than water and the other one is used for separating oils
heavier than water.
 Steam distillation is used for the extraction of most of volatile oils such as
global oil anise oil and eucalyptus oil etc. The extraction is done on the
same principle that when steam is passed through a mixture of
immiscible liquids, the mixture boils below the normal boiling point of
Applications of either component.
Steam distillation
Steam distillation is used for the distillation of water immiscible liquids of
high boiling points turpentine and aniline. It is also used for the
extraction of volatile oils from their crude drugs such as clove, anise and
eucalyptus. Steam distillation is also used for the purification of volatile
substances.
 Vacuum Distillation/ Distillation under reduced pressure
• Distillation under reduced pressure or vacuum distillation works on the principle that a liquid boils when its
vapor pressure is equal to the atmospheric pressure or external pressure.
• From this it is clear, the liquids which are decomposed at their boiling point under atmospheric pressure can be
distilled at a much lower temperature than its boiling point if the pressure is reduced on the surface of the liquid.
• Boiling under reduced pressure will also increase the rate of distillation.
• distillation under reduced pressure is carried out in a specially designed flask known as Claisen flask.
• This flask has two necks. Through one neck a thermometer is inserted and is attached to the condenser through
the other neck a very fine capillary is introduced which completely dips in the boiling liquid. During distillation
under reduced pressure bumping occurs very readily which can be easily prevented by introducing a stream of
air bubbles into the liquid through the capillary.
 The side tube of receiver is connected to a vacuum pump to provide suitable vacuum.

During vacuum distillation, a small pressure gauge (manometer) should be inserted in between the receiver

Vacuum
and the vacuum pump.

distillation For distillation, heating of the flask should not be started until the required vacuum has been obtained
above the surface of the liquid otherwise foaming of the hot liquid will result in the receiver.

Preferably heating up the flask should be done on water bath or oil bath maintained at about 20 C° higher
than the boiling point of the liquid. During vacuum distillation thin-walled glass apparatus like ordinary
flat bottom flasks and conical flasks should never be used otherwise collapsing of such apparatus may
result.
Applications of vacuum distillation

This process is used for the distillation of thermolabile

substances and is also commonly used for the concentration and
drying of extracts which get destroyed at high temperatures.
Destructive distillation

During destructive distillation process the Though it is not a pharmaceutical process but
decomposition of a usually natural products is is used in the destructive distillation of wood
carried out by heat and volatile products of and coal to produce tars which are ultimately
decomposition are condensed and collected. used in the preparation of certain medicines