Distillation

contents
• Introduction

• Types of Distillation processes

• preparation of purified water I.P.

• water for Injection I.P. construction and working

of the still used for the same
 Introduction
Distillation is the process of converting a liquid
into its vapours by heating and the
subsequent condensation of the vapours back
into the original liquid

Liquid Heating
Cooling Vapour
• It is a method of separating substances which
differ in their vapour pressure

Acetone

Acetone Water
Water
 Uses of Distillation
• It is used as separation of mixture of two
miscible liquids

• To separate volatile substances from non-

volatile impurities
• Boiling point of water is 100 degree celsius

• Boiling point of acetone is 56 degree celsius

• As there is sufficient difference between their

boiling points, these components can be
separated by Distillation
 Types of Distillation Processes
Simple Distillation
(Boiling Point difference- more than 300C)

Distillation under reduced pressure or Vaccum Distillation

(The liquid which decomposed below its boiling point
Ex: Glycerine)

 Fractional Distillation
(Boiling Point difference- less than 300C)

Steam Distillation
(For liquids which are insoluble in water but soluble in Steam
Ex: Aniline , Nitrobenzene)

Destructive Distillation
Simple Distillation
 Simple distillation does not work properly
when difference between 2 boiling point is
less than 30 degree celsius
 .This is because the components do not get
separated and purified completely
 If we repeat this process multiple times, we
will be able to separate these 2 components
 However , as this is very time consuming , a
special type of distillation called fractional
distillation is used
 Applications of Simple Distillation

• Preparation of distilled water

• Purification of organic solvents

• Concentration of liquids

• Seperation of Non-volatile solid from volatile

liquids such as acetone, alcohol , ether etc.
Distillation under reduced pressure or Vaccum
Distillation
 Distillation under reduced pressure:This process is carried out for such
liquids which get decomposes below its boiling point

• Glycerine • So the Boiling point of

• Boiling Point:2900C Glycerine should be
reduced.
Pressure Temprature
• Pressure: • As pressure decreases ,
1atm=760mmhg temprature also decreases.
• So we apply the vaccum to
• But at this temprature reduce pressure
Glycerine get decomposes • Temprature:180
• Pressure:12 mmgh
 Fractional Distillation
• Fractional distillation is employed when the
difference of Boiling point of two liquids is
less than 300C
• Fractionating column is used to separate and
purify the liquids
• EX: Acetone 560c
Methanol 650c
 Steam Distillation

Density
Aniline-
1.02gm/cm3

Water-
1gm/cm3

For liquids which are insoluble in water but soluble in

Steam
 Purified water IP
• Water which is free from Volatile and non-volatile
impurities is called Purified water

• It is liable to get contaminated by microbes , hence

purified water should not be used in preparation meant
for parentral administration.

Specifications of Purified water as per IP

• Description : Clear,Colourless, odourless and tasteless

liquid.
• pH: 5-7
• Conductivity:Not more than 1 µS/cm
 Acidity / Alkalinity
• On addition of Methyl red solution the resulting
solution should be not red.
• On addition of Bromo thymol blue solution the
resulting should not blue.

Heavy metals Total bacterial Count

Not more than 0.1ppm Not more than 100 cfu/ml

Total Fungal Count Residue on evaporation

Not more than 10 cfu/ml Not more than 0.001%
 Water for Injection IP
• Water which is free from Volatile,non-volatile
impurities,Microorganisms and pyrogens is called Water for Injection

• Highly purified water used for injectives,which will be subsequently

sterilised

• Specifications of water for injections are same as that of Purified water

• WFI is prepared by using potable water, purified water and distilled

water

• WFI must pass the Pyrogen test

Pyrogen is a substance, typically produced by a bacterium, which
produces fever when introduced or released into the blood
Preparation of Purified water IP and water
for Injection IP
 Consrtruction and workinng of apparatus

Construction
• It consist of boiler which is made of cast iron.

• It is connected to the condenser tubes through the baffles.

• The condenser tubes and baffles are made of stainless steel.

• Baffles are provided over the top of the condenser tubes to

avoid water drops entry with water.

• The baffles are provided to avoid carry-over of pyrogen and

other water soluble materials.
 working
• The cooling water enters at the bottom of the
condenser
• Water is heated by the condensing vapours
• The flow rate is adjusted in such a way that water
gets heated at 90-950 c befor it enters the boiler.
• The top of condenser jacket is open , so that gases
from the water can escape into the atmosphere.
• Storage: water for Injection is stored in tightly
closed natural glass containers