Distillation may be defined as the separation of the
constituents of a mixtures including a liquid by partial
vaporization of the mixture and separate collection of the vapour. This process include- * The separation of one liquid from non-volatile impurities. * The separation of one liquid from one or more other liquids, with which it may be miscible, partially miscible or immiscible. • Distillation may be of four types:- a) Simple distillation:- Simple distillation is the process of converting a liquid into it’s vapor, recovering the liquid by condensing the vapor, usually leading it into contact with a cold surface. b) Fractional distillation:- (Rectification) Fractional distillation is the process employed to separate miscible volatile liquids having different boiling points. c) Steam distillation:- Steam distillation is used for the distillation of water immiscible liquids of high boiling points. Ex. turpentine, aniline etc. d) Destructive distillation:- Destructive distillation is used to describe the decomposition of a substance, usually a natural product by heat, followed by the condensation and collection of the volatile product decomposition. A condenser is fundamentally a heat exchanger. The surface of a condenser is kept cold by a stream of water on one side.
۩ A large volume of cooling water is required on account of
the latent heat of vaporization evolved on condensing the vapor.
♪ In cooling 1 gm of steam (100˚C), approximately 2.27KJ
heat are evolved. ۩ For liquids boiling point above 150˚C; simple air cooling is used. Fig: Steam – jacketed still ♫ The condenser must be constructed as to be easily cleaned. ♫ The cooling surface must be large. ♫ The condensing surface must be a reasonably good conduction of heat. ♫ The film of condensed liquid is bad conductor and must be removed quickly. ♫ The warmer water in contact with the condensing surface must be quickly carried away and it’s place taken by fresh cold water. ¶ Recovery of alcohol in the preparation of dry extracts.
¶ Preparation of purified water, BP and water for injections,
BP by simple distillation.
♫ Purification of water by distillation is a special case
because, ☻Gases including CO2 dissolved in the raw water must be removed. ☻The residue of solids must not be concentrated to a point where hydrolysis occurs. Fig: Distillation unit for purified water The general arrangement of a Fractional distillation unit is known here:- ۩ The mixture to be distilled is fed to the boiler and heated, usually by a steam coil. ۩ The vapor is taken to a condenser at the top of the column. ۩ The condensed liquid is split in a reflux divider, a suitable quantity being returned to the column as reflux and the remainder taken off as product. ۩ The ratio of reflux/product is known as reflux ratio. ۩ Distillation will continue until all the MVC (More Volatile Component) has been distilled off and forms the top product and the LVC (Less Volatile Component) is left in the boiler to provide the bottom product. • Fractional distillation depends upon ----- ♠ heating the mixture ♠ repeatedly condensing the vapor ♠ re-heating the liquid ♠ equilibrium between liquid and vapor state
♣ From the operational point of view, Fractional distillation is a
mass transfer process.
Application: Vaccum fractionation is extensively used
for the separation of the mixed fatty acids derived from oils and fats. Fig: Fractional distillation column THEORY • A mixture of immiscible liquids begins to boil when the sum of their vapor pressure is equal to the atmospheric pressure.
A. A high boiling point substances (turpentine 160°c) may be distilled
with water at a temperature much below its boiling point under reduced pressure.
B. Substances of low volatility can be steam distillated when molecular
weight is considerably higher than that of water. Here, the following equation is followed---
W1 /W2 =ρ1M1 /ρ2M2 Where,
ρ1, ρ2 = Vapor pressure of two molecules M1, M2 = molecular weight W1, W2 = proportion by weight • The safety tube in the steam generator permits the expulsion of some water if excessive pressure is developed. • The distillate separates into two layers (water and other component) that are separated in a separating funnel. • The actual yield is greater than the calculated yield since minute particles are carried over mechanically by the steam. Fig: Steam distillation apparatus • It has a jacket and contains manholes in the top and side for charging and discharging. • Most volatile oils are lighter than water and will separate from the distillate as an upper layer. • Some volatile oils are heavier than water, here the process is reversed. When specific gravity = 1, separation does not take place; then it is necessary to collect the whole of the distillate and extract it with a volatile solvent and subsequently distilling off the solvent from the oil. Fig: Still for steam distillation of volatile oils. THANKS GOOD BYE… • For the determination of volatile oils in drugs. • Distillation with toluene is used for the determination of moisture in drugs. • For extracting volatile oils like clove, aniseed, eucalyptus.