Evaporation and Distillation

EVAPORATION and DISTILLATION
Industrial Pharmacy
Samia Ghani
M.Phil Pharmaceutics

CONTENTs
• DEFINITION OF EVAPORATION
• MECHANISM/PRINCIPLE
• THEORY OF EVAPORATION
• FACTORS AFFECTING EVAPORATION
• MODES OF EVAPORATION
• EVAPORATORS
• EVAPORATION UNDER REDUCE PRESSURE
• ADVANTAGES
• APPLICATIONS

MECHANISM OF EVAPORATION:
When heat applied in solution the motion of
molecules increase and molecules present in
the surface overcome the surface tension of
the liquid and it evaporates because surface
molecules have less cohesive force than
others.

FACTORS AFFECTING
EVAPORATION
• There are seven factors to affect evaporation.
1. Temperature
2. Surface area
3. Agitation
4. Atmospheric aqueous vapour pressure
5. Atmospheric pressure on the liquid under evaporation
6. Type of product required
7. Economic factors

FACTORS AFFECTING
EVAPORATION
1) Temperature: The rate of evaporation is directly
proportional to the temperature.
2) Surface area: The rate of evaporation is directly
proportional to the surface area of the vessel exposed to
evaporation.
3) Agitation: is necessary for evaporation.
4) Atmospheric aqueous vapour pressure: The rate of
evaporation is inversely proportional to the atmospheric
aqueous vapour pressure.

FACTORS AFFECTING
EVAPORATION
5) Atmospheric pressure on the liquid under evaporation: The
rate of evaporation is inversely proportional to the
atmospheric pressure on the liquid under evaporation.
6) Type of product required: The selection of the method and
apparatus to be used for evaporation depends upon type of
product required.
7) Economic factors: When selecting the method and apparatus
the economic factors are important

EVAPORATION UNDER
REDUCED PRESSURE

ADVANTAGES
1. Evaporation occurs at low temperature, with less risk of
damage to heat sensitive materials.
2. A lower operating temperature gives higher
temperature gradients, without the need of excessive
steam pressures.
3. The lower the operating, temperature the lower the steam
pressure that can be used.

Method of operation of
evaporation
Single effect evaporator
Forward feed multiple effect evaporator
Backward feed multiple effect evaporator
Parallel feed multiple effect evaporator
Mixed feed multiple effect evaporator

Single effect evaporator
Required capacity of operation is relatively small

Forward feed multiple effect evaporator
Feed should be near the B.P. of
the solution at the pressure in the
1st effect
Previous unit vapour serves as a
heating medium for the next
effect
Here latent of the vapour can be
reused and recovered again
Uses when feed is hot or when
the concentration product might
be damaged at high temperature
B.P decreases from effect to effect
Pressure is 1 atm at 1st effect and
under vaccum in other effects

Backward feed multiple effect evaporator
Uses when fresh feed is
cold
Flows from low to high
pressure for this to happen
we apply pumps at certain
places
Temperature increases
from effect to effect
Used when concentrated
product is highly viscous
High temperature and low
viscosity gives high heat
transfer coefficient

Parallel multiple effect evaporator
Adding and withdrawal
of concentrated product
from each effect
Feed almost saturated
and solid crystals are the
product
Eg- evaporation of brine
to make salt

Mixed multiple effect evaporator
When feed moves
forward with fresh feed is
entering at the 2nd or 3rd
effect k/a mixed type
Used in solutions having
considerable change in
viscosity with
temperature over
concentration range

EQUIPMENT USED FOR
EVAPORATION
• Equipments which are used for evaporation are
called Evaporators.
 Types of Evaporator:
• Evaporators are divided mainly into three groups.
 1. Natural circulation evaporator
 Types:
i) Evaporating pans (solar evaporators)
ii) Evaporating stills
iii) Short tube evaporator.

EQUIPMENT USED FOR
EVAPORATION
2) Forced circulation evaporator.
3) Film evaporator
Types:
i) Wiped Film evaporator
ii)Long Tube Evaporator
a) Climbing film evaporator
b) Falling film evaporator

1) NATURAL CIRCULATION
EVAPORATORS
• Working principle:
• The movement of the liquid results from
convection currents set up by the heating
process.
• Convection currents: The process in which
heat moves through a gas or liquid as the
hotter parts rises and the cooler part sinks.

Evaporating Pans
• “On a manufacturing scale, liquid extracts containing water are
evaporated in open pans called evaporating pans.”
Construction:
• The evaporating pan consists of
 Hemispherical shallow made of
Copper Stainless
steel Alluminium
Enameled iron
 Steam jacket
• The hemispherical shape gives the best surfacevolume
ratio for heating and the largest area for the disengagement
of vapour.
• Paddles and scrappers are used for agitation. Heat is
supplied by condensation of stream

• Working:
• The dilute solution is
taken in the pan. Steam is
introduced through the
steam inlet into the jacket
to heat the pan. In these
evaporators the
movement of the liquid
results from convection
currents set up by the
heating process. The
concentrated liquid is
collected through the
outlet placed at the
bottom of the pan.

Diagram of Batch pan Evaporators

Advantages
1) They are simple, easy and cheap to construct.
2) They are easy to use and clean.
3) Stirring of the evaporating liquids can be
done easily.

Disadvantage
1) The whole of the liquid is heated all the time
which may lead to decomposition of the
components.
2) On the evaporating surface foam is rapidly
formed which decreases evaporation. Solids may
be deposited at the bottom which make the
stirring necessary.
3) This pan can only be used for evaporating
aqueous and thermostable liquid extracts.
4) They can not be used for evaporating extracts
containing organic solvents like alcohol etc.

ii) Evaporating still
• Construction
• It consists of a jacketed-evaporating pan with
a cylindrical cover that connects it to a
condenser. The over all assembly is called still.
The cover is clamped with the evaporating
pan.

Working :
• The dilute liquid is fed
into the still, the cover is
clamped. Steam is
introduced into the
jacket. The liquid is
evaporated and
condensed in the
condenser and collected.
The product (i.e.
concentrated liquid) is
collected through the
product outlet.

Advantages:
• Easy to clean and maintain.
• Allow the equipment to be used for slovents
other than water. E.g. ethanol.
Disadvantages:
• All the liquor is heated all the time.
• The heating surface is limited.

iii) Short tube evaporator
Construction:
1 – 2 m
40 – 80 mm
2.5 m
1000
• The evaporator is a cylindrical vessel. The lower
portion of the vessel consists of a nest of tubes with
the liquor inside and steam outside– this assembly is
called calendra.
• The specifications of calendria are as follows:
• Tube length:
• Tube diameter:
• Diameter of evaporator:
• Number of tubes:
• The feed inlet is at the top of the calendra. The product
outlet is placed at the bottom of the evaporator. Steam
inlet and outlet is placed from the side of the calendria.

Vertical type natural circulation
evaporator
Types are basket type(liquid
inside ) and standard
type(liquid outside )
Velocity :1-3 fps
Boiling increases de
Boiling increases density
liquid rises in the tube by
natural circulation and flows
downward through a large
central open space or
downcomer
Natural circulation increases
heat transfer coefficient
Not for viscous liquid
Also called as short tube
evaporator

Working:
• The liquor in the tubes is
heated by the steam and
begins to boil, when the
mixture of liquid and
vapor will shoot up the
tubes (in a similar manner
to that of a liquid that is
allowed to boil to
vigorously in a test-tube).
• The product is collected
through the product
outlet.

• Advantages
• 1. Use of tubular calendria increases the heating area,
possibly by a factor of 10 to 15 compared to that of an
external jacket.
• 2. Increasing the rate of heat transfer.
• 3. Condenser and receiver can be attached to run the
evaporation under vacuum with nonaqueous solvents.
• Disadvantages
• 1. Since the evaporator is filled to a point above the level of
the calendria, a considerable amount of liquid is heated for a
long time. The effect of this continual heating can be reduced
to some extent by removing concentrated liquor slowly from
the outlet at the bottom of the vessel.
• 2. Complicated design, difficult for cleaning and
maintenance.

2) Forced circulation
evaporators
Construction:
• The evaporator consists of a short tube calendria and a
large cylindrical vessel (body of the evaporator) for
separation of vapor and liquid takes place.
• The liquor inlet is provided at the side of the cylindrical
vessel.
• A pump is fitted in between the calendria and the body
of the evaporator.
• A tangential inlet for liquid under high pressure is
placed at neck of the body of the evaporator.
• The vapor outlet is placed at the top of the body and it
may be passed through a condenser to collect the
condensed liquid.

Working principle:
• Feed is introduced through the
liquor inlet. Pump will force the
liquid through the calendria.
Steam heats the liquid inside
the calendria. As it is under
pressure in the tubes the
boiling point is elevated and no
boiling takes place. As the
liquor leaves the tubes and
enters the body of the
evaporator through the
tangential inlet there is a drop
in pressure and vapor flashes
off from the superheated
liquor. The concentrated liquid
is pumped out through the
product outlet and the vapor is
collected through the vapor
outlet.

4) These evaporators are mainly used for
thermolabile materials.
5) These can also be used in practice for the
concentration of insulin and liver extracts.
Disadvantage:
• Corrosion-erosion can occur, due to high
circulation velocities.
• Salt deposits detach and accumulate at the
bottom.

Example of Forced Circulation Evaporator

3) FILM
EVAPORATORS
• Film evaporators spread the material as a film over the heated
surface, and the vapor escapes the film.
• Following are the types of film evaporators.
i) Wiped Film
evaporator ii)Long
Tube Evaporator
a) Climbing film evaporator
b) Falling film evaporator

i) Wiped film
evaporators
• Construction:
• A form of film evaporator coming into increasing use is
the wiped film evaporator or rotary film evaporator,
which contains of a single, short tube of wide diameter,
better described as a narrow cylindrical vessel,1 or 2
meters in length.
• A section across the evaporator is shown here where it
will be seen that the vessel is surrounded by a heated
jacked. Through the vessel is a bladed rotor, with a
clearance of the order of 1mm between the tips of the
rotor blades and the wall of the vessel.

Working:
• The liquor is introduced at the
top of the vessel and spread
as a film over the heated wall
by the action of the rotor.
• Evaporation occurs as the
liquor passes down the wall,
vapour is taken to a
condenser and the
concentrated liquor
withdrawn at the bottom of
the vessel.
• The evaporator is therefore a
form of single tube, falling
film evaporator in which the
film is formed and agitated
mechanically.

ii) Long tube evaporators
(Climbing film evaporators)
Construction:
• The heating unit consists of steam-jacketed
tubes, having a length to diameter ratio of about
140 to 1, so that a large evaporator may have
tubes 50 mm in diameter and about 7 m in
length.
• The liquor to be evaporated is introduced into the
bottom of the tube, a film of liquid forms on the
walls and rises up the tubes, hence it is
called climbing film evaporator.

Working
:
• At the upper end, the mixture of vapor
and concentrated liquor enters a
separator, the vapor passes to a
condenser, and the concentrated liquid
to a receiver.
• Cold or pre heated liquor is introduced
into the tube.
• Heat is transferred to the liquor from
the walls and boiling begins.
• Ultimately sufficient vapor has been
formed for the smaller bubbles to unite
to a large bubble,
• filling the width of the tube and
trapping a ‘slug’ of liquid above the
bubble.
• As more vapor is formed, the slug of
liquid is blown up the tube, the tube is
filled with vapor, while the liquid
continues to vaporize rapidly, the vapor
escaping up the tube and, because of
friction between the vapor and liquid,
the film also is dragged up the tube upto
a distance of 5 to 6 metres.

Example of Rising-film Evaporators

long tube vertical type evaporator or
kestner evaporator
Heat transfer on stream side is
very high as compare to
evaporating liquid side so high
liquid velocities are desirable
Liquid run inside the tube
Length of 12-20 ft.
3-10 mm tubes
Formation of vapours inside the
tube causing pumping action
which gives quite high liquid
velocities
Not re circulated (contact time is
low )
Can be adapt for foamy liquids
Not for scaling and not for
liquids of high viscosity

ii) Long tube evaporators
(Falling film evaporators)
Construction:
• The heating unit consists of steam-jacketed
tubes, having a length to diameter ratio of
about 140 to 1, so that a large evaporator may
have tubes 50 mm in diameter and about 7 m
in length.

Working principle
• The liquor to be
evaporated is introduced
at the top of the
evaporator tubes and the
liquor comes down due to
gravity.
• The concentrate and
vapor leaves the bottom.
They are separated in a
chamber where the
concentrate is taken out
through product outlet
and vapor from vapor
outlet.

Advantages:
• Because of obtaining good heat transfer the
method being especially useful with liquids that
are too viscous to be processed in units in which
the film is formed naturally.
Disadvantages:
• A major disadvantage of falling film evaporators is
the potential instability of the falling film
• Expense to manufacture and install the
instrument is high.
• Difficult to clean and maintain.

APPLICATION OF
EVAPORATION
• Evaporation is one of the most important
processes in the manufacture of
pharmaceuticals.
• It is used in the preparation of
1. Liquid extracts, soft extracts & dry extracts.
2. In the concentration of blood plasma &
serum.
3. It is also used in the manufacture of drugs
containing, antibiotics, enzymes, hormones &
many other substances.

APPLICATIONS OF
EVAPORATION
4) Used in purification of vitamins.
5) Concentration of proteins.
6) Concentration of biological products.
7) Stripping of solvents from vegetable & plant or herbal
extracts.
8) Removal of water & solvents from
fermentation broths.
9) Concentration of penicillin & related products

DEFINITION
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 “Distillation is an unit operation which involves separation
of a vaporizable component from a multi-component
system and subsequent condensation of vapours.”
 “Distillation is a process of separating the component
substances from a liquid mixture by selective evaporation
and condensation.”
 “Distillation is defined as the separation of the
components of a liquid mixture by a process involving
vaporization and subsequent condensation at another
place.”

APPLICATIONS:
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 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.

Difference between Evaporation
& Distillation
Evaporation Distillation
1.It is the process of
vapourisation of solvent from
a solution to get
concentrated product.
1.It is the separation of
constituents of a liquid
mixture by vapourisation &
again condensation.
2.Vapours are not collected. 2.Vapours are condensed &
collected.
3.Concentrated product is
obtained after evaporation.
3.Distillate is obtained after
distillation.
4.Used for obtaining
concentrated products &
removing impurities.
4.Used for separation &
purification of liquids from
mixtures.

TERMINOLOGY
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 Binary Mixture
When two liquids mixed together, they may be miscible
with each other in all proportion, such miscible liquid are
known as binary mixtures of liquid.
Example:
- Ethanol + Water
- Acetone + Water
- Benzene + Carbon tetrachloride

TERMINOLOGY
 Ideal Solution (Perfect solution)
Ideal solution is defined as the one in which there is no
change in the properties of components other than
dilution, when they mixed to form a solution.
Property of ideal solution
 T
otal volume of solution is equal to sum of volumes of
each component
 No heat absorbed and No heat evolved
 No Chemical reaction in-between
 Final volume of solution represents additive property of
individual components
 Follow Raoult’s low 5

TERMINOLOGY
 Real Solution
Most system shows varying degree of deviation from
raoult’s law, depending on nature of liquids and
temperature. These solution are known as real solution.
Property of Real solution
 Heat may absorbed or evolved
 Chemical reaction occurs in-between
 Final volume of solution represents additive property of
individual components
 Don’t Follow Raoult’s low
Example
 Carbon tetra-chloride + Cyclohexane
 Choroform + Acetone
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TERMINOLOGY
 Volatility
The volatility of any substance in solution may be defined as the
equilibrium partial pressure of substance in vapour phase divided by the
mole fraction of substance in the solution.
For example, a substance A in a liquid mixture has partial pressure PA
and its concentration in the mixture is XA on mole fraction scale.
Partial vapour pressure of A
Volatility of component A, =
Mole fraction XA of A insolution
vA = PA/XA
The volatility of a material in the pure state is equal to the vapour
pressure of the material. 7

TERMINOLOGY
 Relative Volatility
Consider a liquid mixture containing two component A and
B, In such case, the volatility of one component is
expressed in terms of second as below,
Volatility of component A(VA)
Relative Volatility =
Volatility of component B (VB)
= VA/VB 8

TERMINOLOGY
Vapor pressure
 It is defined as the pressure exerted by a vapor in
thermodynamic equilibrium with its condensed phases (solid
or liquid) at a given temperature in a closed system.
 The equilibrium vapor pressure is an indication of a liquid's
evaporation rate.
Thermodynamic Equilibrium
 It is the systematic study of transformations of matter and
energy in systems as they approach equilibrium.
 The word equilibrium implies a state of balance. 9

TERMINOLOGY
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Azeotropic Mixture(Constant boiling Mixture)
Mixture of special composition giving minimum or maximum
boiling point than individual component with minimum or
maximum boiling point respectively.
 Examples
 Mixture with Maximum Boiling point:
Mixture containing 20.2 ml HCl + 79.8 ml water
 Mixture with Minimum Boiling point
Mixture containing 95.5 ml Alcohol + 4.5 ml water

RAOULT’S LAW
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 It express a quantitative relationship between the
concentration and vapour pressure.
 It states that partial vapour pressure of each volatile
constituent is equal to vapour pressure of the pure
constituent multiplied by its mole fraction in the solution at
a given temperature.

 Suppose Homogeneous mixture of liquid A and B
Partial vapour pressure of component A in Mixture
= PA = P°A*XA
Mole fraction of A in solution = XA
Vapour pressure of A in pure state = P°A
Partial vapour pressure of component B in Mixture =
PB = P°B *XB
Mole fraction of B in solution = XB
Vapour pressure of A in pure state = P°B
 Total Vapor pressure of Mixture
PT = PA+ PB
PT = P°A *XA + P°B*XB
RAOULT’S LAW
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POSITIVE DEVIATION & NEGATIVE DEVIATION
(REAL SOLUTION)
 Positive Deviation:
In some liquids systems, the total vapor pressure is greater
than the sum of the partial pressures of the individual
components
Ex: benzene and ethanol.
Differ in their polarity, length of hydrocarbon chain and
degree of association.
 Negative Deviation:
In some liquid systems, the total vapor pressure is lower
than that of the sum of the partial pressures of the
individual components.
Ex: Chloroform and acetone
Due to hydrogen bonding, salt formation and hydration
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POSITIVE DEVIATION & NEGATIVE DEVIATION
(REAL SOLUTION)
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GENERAL EQUIPMENT FOR DISTILLATION:
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STILL :
 It is a vaporizing chamber and used to place the material
to be distilled.
 The still is heated by a suitable means for vaporization of
the volatile constituents.
 On laboratory scale round bottom flasks made of glass
are used so that the progress of the distillation can be
noticed.
 A condenser is attached to the still using appropriate
joints. A trap is inserted between distillation flask and
condenser.

CONDENSER :
 Used to condense the vapor
It is kept cold by circulating water/air through jacket.
Types:
 Single-surface condensers
- Straight Tube
- Bulb type
- Spiral
- Coiled type
 Double-surface condensers
 Multi-tubular condensers
The condenser is connected to a receiver through a suitable
adapter.
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CONDENSER :
Bulb type
Straight
Tube
type
Spiral type Coiled type
Cold finger,
Spiral type
Lucas’s
Double Surface
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RECEIVER :
 It is used to collect the distillate.
 It may be a simple flask.
 It immersed in ice-bath to minimize loss of volatile
matter.
 Florentine receivers are used for the separation of
oil and water.
Types of Florentine receivers :
 Type-I :- for separation of oil heavier than water.
 Type-II :- for separation of oil lighter than water.

RECEIVER :
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CLASSIFICATION OF DISTILLATION METHODS
I. Simple Distillation (Differential distillation)
II. Flash Distillation (Equilibrium distillation)
III. Vacuum distillation (distillation under reduced pressure)
IV. Molecular Distillation (Evaporation distillation or short path
distillation.)
V. Fractional Distillation (Rectification)
VI. Aezotropic and extractive Distillation
VII. Steam Distillation
VIII. Destructive Distillation
IX. Compression Distillation
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1. SIMPLE DISTILLATION
 Simple distillation is a process of converting a single
constituent from a liquid (or mixture) into its vapour,
transferring the vapour to another place and recovering
the liquid by condensing the vapour, usually by allowing it
to come in contact with a cold surface.
 This process is known differential distillation, as
distillation is based on the differences in volatilities and
vapour pressures of the components in the mixture.
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Principle:
 Liquid boils when its vapour pressure is equal to atmospheric
pressure. Simple distillation is conducted at its boiling point.
 The higher the relative volatility of a liquid, the better is the
separation by simple distillation. Heat is supplied to the liquid so
that it boils. The resulting vapour is transferred to a different
place and condensed.
CONSTRUCTION:
 It consists of a distillation flask with a side arm sloping
downwards.
 Condenser is fitted into the side arm by means of a cork.
 The condenser is usually water condenser, i.e., jacketed for
circulation of water.
 The condenser is connected to a receiver flask using an adapter
with ground glass joints.
 On a laboratory scale, the whole apparatus is made of glass. 24

WORKING:
 The liquid to be distilled is filled into the flask to one-half to
two-third of its volume. Bumping is avoided by adding
small pieces of porcelain before distillation.
 A thermometer is inserted into the cork and fixed to the
flask. The thermometer bulb must be just below the level of
the side arm.
 Water is circulated through the jacket of the condenser.
The contents are heated gradually.
 The liquid begins to boil after some time. The vapour
begins to rise up and passes down the side arm into the
condenser.
 The temperature rises rapidly and reaches a constant
value.
 The temperature of the distillate is noted down, which
is equal to the boiling point of the liquid. The vapour is
condensed and collected into the receiver.
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 The flame is adjusted so that the distillate is collected at
the rate of one to two drops per second. Distillation should
be continued until a small volume of liquid remains in
the flask.
Applications:
 For the preparation of distilled water and water for injection.
 Volatile and aromatic waters are prepared.
 Organic solvents are purified.
 A few official compounds are prepared by distillation.
Examples are spirit of nitrous ether and aromatic spirit of
ammonia.
 Non-volatile solids are separated from volatile liquids.

2. FLASH DISTILLATION
 Flash distillation is defined as a process in which the
entire liquid mixture is suddenly vaporized (flash) by
passing the feed from a high pressure zone to a low
pressure zone.
 Flash distillation is also known as equilibrium distillation,
i.e., separation is attempted when the liquid and vapour
phases are in equilibrium. This method is frequently
carried out as a continuous process and does not involve
rectification.

Principle:
 When a hot liquid mixture is allowed to enter from a high-
pressure zone into a low-pressure zone, the entire liquid
mixture is suddenly vaporised.
 This process is known as flash vaporisation. During
this process the chamber gets cooled. The individual
vapour phase molecules of high boiling fraction get
condensed, while low boiling fraction remains as
vapour.
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Working:
 The feed is pumped through a heater at a certain pressure.
 The liquid gets heated, which enters the vapour-liquid separator
through a pressure-reducing valve.
 Due to the drop in pressure, the hot liquid flashes, which
further enhances the vaporisation process.
 The sudden vaporisation induces cooling. The individual
vapour phase molecules of high boiling fraction get
condensed, while low boiling fraction remains as vapour.
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 The mixture is allowed for a sufficient time, so that
vapour and liquid portions separate and achieve
equilibrium.
 The vapour is separated through a pipe from above and
liquid is collected from the bottom of the separator.
 By continuously feeding into the still, it is possible to
obtain continuous flash distillation.
 The operating conditions can be adjusted in such a way
that the amount of feed exactly equals the amount of
material removed.
 Therefore, vapour and liquid concentrations at any
point remain constant in the unit.
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Uses:
 Flash distillation is used for separating components, which
boil at widely different temperatures. It is widely used in
petroleum industry for refining crude oil.
Advantages:
 Flash distillation is a continuous process.
Disadvantages:
 It is not effective in separating components of comparable
volatility.
 It is not an efficient distillation when nearly pure components
are required, because the condensed vapour and residual
liquid are far from pure.
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3. VACUUM DISTILLATION
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• The distillation process in which the liquid is distilled at a
temperature lower than its boiling point by the application
of vacuum. Vacuum pumps, suction pumps, etc. are
used to reduce the pressure on the liquid surface.
Distillation under the reduced pressure is based on the
principle of the simple distillation with some
modifications.

1
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vapour.
Principle:
• 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.
• Water boils at an 100°C at an atmospheric pressure is 101.3I
kPa (760 mm Hg). At 40°C, the vapour pressure of water is
approximately 9.33 kPa (70 mm Hg). Hence, the external
pressure is reduced to 9.33 kPa (70 mm Hg) where water boils at
40°C. The net result is the increase in rate of mass transfer into

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1
The important factor in evaporation is:
Mass of vapour formed ά vapour pressure of evaporating liquid
external pressure
According to this formula, water is allowed to evaporate at
40°C and 9.33 kPa (70 mm Hg) pressure, the mass of
vapour formed in unit time is approximately 11 times, i.e.
760/70 for water.

Assembling of apparatus:
 It consists of a double-neck distillation flask known as Claisen flask .
 Thick walled glass apparatus with interchangeable standard glass joints are used for
vacuum distillation.
 In one of the necks of the Claisen flask, a thermometer is fitted. The second neck prevents
splashing of the violently agitated liquid.
 Bumping occurs readily during vacuum distillation. Placing a fine capillary tube in the
second neck of the flask can prevent bumping.
 The capillary tube is dipped in the boiling liquid, so that a stream of air bubbles is drawn
out.
 Water bath or oil bath is used for heating.
 The Claisen flask is connected to a receiver through a condenser.
 Vacuum pump is attached through an adapter to the receiver. A small pressure gau3g8e
(manometer) should be inserted between the pump and the receiver.

 Applications:
 Preventing degradation of active constituents (≈ 55◦C)
 Enzymes - malt extract, pancreatin
 Vitamins-thiamine,ascorbic acid
Glycosides - anthraquinones
Alkaloids - hyocymine to
atropine
 Disadvantages:
 In vacuum distillation, persistent foaming occurs. This may
be overcome by adding capryl alcohol to the liquid or by
inserting a fine air capillary tube in the second neck of
the Claisen flask.
 The stream of air is drawn in and breaks the rising foam. The
above method is not suitable for the preparation of
semisolid
or solid extracts by distillation under vacuum.
39

4. MOLECULAR DISTILLATION
 It is defined as a distillation process in which each
molecule in the vapour phase travels mean free path
intermolecular
and gets condensed
collisions on
individually without
application of vacuum.
Molecular distillation is based on the principle of the
simple distillation with some modifications. This is
also called Evaporation distillation or Short path
distillation.
40

Principle:
 The substances to be distilled have very low vapour pressures.
examples are viscous liquids, oils, greases, waxy materials and
high molecular weight substances.
 These boil at very high temperature. In order to decrease the
boiling point of the liquids, high vacuum must be applied.
 The pressure exerted by vapors above the liquid is much
lower. At very low pressure, the distance between the evaporating
surface and the condenser is approximately equal to the mean free
path of the vapour molecules.
 Molecules leaving the surface of the liquid are more likely hit the
condenser surface nearby. each molecule is condensed individually.
the distillate is subsequently collected.
41

Applications:
Molecular distillation is used for the purification and separation of chemicals
of low vapour pressure.
1. Purification of chemicals such as tricresyl phosphate, dibutyl phthalate
and dimethyl phthalate.
2. More frequently used in the refining of fixed oils.
3. Vitamin A is separated from fish liver oil. Vitamin's is concentrated by this
method from fish liver oils and other vegetable oils.
4. Free fatty acids are distilled at 100°C.
5. Steroids can be obtained between 100°C and 200°C,
6. Triglycerides can be obtained from 200°C onwards.
Proteins and gums will remain as nonvolatile residues. Thus, the above
mixture can be separated by molecular distillation. 42

Theory:
The mean free path of a molecule is defined as the average distance through
which a molecule can move without coming into collision with another.
The mean path (λ.) can be expressed mathematically as:
where. p = vapour pressure, kPa
ρ = density, kg/m3
η = viscosity, Pa's
λ = mean path length, m
For example, mean path (heavy molecules) of butyl phthalate is about 30 mm and of
olive oil is 20 mm when measured at a pressure of 0.1 pascal.
The mean free path can be increased by decreasing the viscosity which can be
obtained at high temperature and low pressure. Thus, nonvolatile substances
may become volatile and distillation is possible.
1
0
7

1
0
8
Requirements for design the equipment:
• The evaporating surface must be close to the condensing
surface. This ensures the molecules to come in contact with the
condenser as soon as they leave the evaporating surface. For
this reason, this process is also known as short path distillation.
• The molecular collisions should be minimized because they
change the direction of the path of molecules. In other words,
intermolecular distances should be fairly high. It can be
achieved under very high vacuum, usually of the order of 0.1 to
1.0 pascals.
• The liquid surface area must be as large as possible as so that
the vapour is evolved from the surface only, but not by boiling.
Thus this process is also called evaporation distillation.

1
0
9

Principle:
 In this method, liquid feed is introduced into a vessel, which is
rotated at very high speed (centrifugal action).
 On account of heating, vaporisation occurs from a film of liquid
on the sides of the vessel.
 The vapour (molecules) travels a short distance and gets
condensed on the adjacent condenser.
 Each molecule is condensed individually. The
subsequently collected.
distillate is
46

Construction:
 It consists of a bucket-shaped vessel having a diameter of about 1
to 1.5 m.
 It is rotated at high speed using a motor.
 Radiant heaters are provided externally to heat the fluid in the
bucket.
 Condensers are arranged very close to the evaporating surface.
 Vacuum pump is connected to the entire vessel at the top.
 Provisions are made for introducing the feed into the centre of the
bucket, for receiving the product and residue for re-circulation.

Working:
 Vacuum is applied at the centre of the vessel.
 The bucket shaped vessel is allowed to rotate at high speed.
 The feed is introduced from the centre of the vessel.
 Due to centrifugal action of the rotating bucket, liquid moves outward over the
surface of the vessel and forms a film.
 Since, the radiant heaters heat the surface, the liquid evaporates directly from
the film.
 The vapour (molecules) travels its mean tree path and strikes the condenser.
 The condensate is collected into another vessel.
 The residue is collected from the bottom of the vessel and is recirculated
through the feed port for further distillation.
48

Construction:
 The vessel has a diameter of 1 m.
 The walls of the vessel are provided with suitable means of heating
(jacket).
 Wipers are provided adjacent to the vessel wall. Wipers are
connected to a rotating head through a rotor.
 The condensers are arranged very close to the wall (evaporating
surface).
 Vacuum pump is connected to a large diameter pipe at the
centre of the vessel.
 Provisions are made for collecting the distillate and the undistilled
liquid residue at the bottom.
50

 Vacuum is applied at the centre of the vessel and wipers are allowed to rotate.
 The feed is entered through the inlet of the vessel.
 As the liquid flows down the walls, it is spread to form a film
1
1
5
by PTFE
(polytetrafluoroethylene) wipers, which are moving at a rate of 3 m per second.
 The velocity of the film is 1.5 m per second.
 Since the surface is already heated, the liquid film evaporates directly.
 The vapour (molecules) travels its mean free path and strikes the condenser.
 The condensate is collected into a vessel.
 The residue (undistilled or mean free path not travelled) is collected from the bottom
of the vessel and re-circulated through the feed port for further distillation. Capacity is
about 1000 L / hour.
Working:
 The vessel is heated by suitable means.

8. 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.
Fractional distillation is a process in which vaporisation of liquid
mixture gives rise to a mixture of constituents from which the
desired one is separated in pure form.
64

1
1
8
In simple distillation,
vapour is directly passed
through the condenser.
Condensate is collected
directly into the receiver,
 In fractional distillation the vapour
must pass through a fractionating
column in which partial condensation
of vapour is allowed to occur.
Condensation takes place in the
fractionating column, so that a part of
the condensing vapour returns to the
still.
Simple Distillation Vs Fractional Distillation

1
1
9
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.

1
2
0
Applications:
Fractional distillation is used for the separation of volatile miscible liquids with
near boiling point such as
•Acetone and water
•Chloroform and benzene
Disadvantage:
Fractional distillation cannot be used to separate miscible liquids, which form
PURE azeotropic mixtures.

Fractionating columns
 In fractional distillation, special type of still-heads are required so
condensation and re-vaporisation are affected continuously.
 These are known as fractionating columns.
that
 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.
68

1
2
2
Fractionating columns Types
A. Packed columns and
B. Plate columns

A] Packed columns
1
2
3

A. Packed columns
Some form of packing is used in the column to affect the
necessary liquid/vapour contact. The packing may consistof
single turn helices (spirals) of wire or glass, glass rings,
cylindrical glass beads, stainless steel rings etc.
Construction: Packed column consists of a tower containing a
packing that becomes wetted with a film of liquid, which is
brought into contact with the vapour in the intervening spaces.
(a)A long fractionating column is necessary when theboiling
points of the constituents are lying fairly close together.
(b) A short fractionating column is necessary when theboiling
point of the constituents differ considerably.
Applications: Packing must be uniform so as to obtain proper
channels. If packing is irregular, mass transfer becomes less
effective.
71

B] Plate columns
1
2
5

B] Plate columns (Bubble cap)

1
2
7
B. Plate columns
Many forms of plates are used in the distillation using different columns. It can be divided into
two types, which are commonly used in pharmacy.
(a) Bubble cap plates
(b) Turbo grid plates
Bubble cap column is used in large distillation plants and is describedbelow.
Construction: The column consistsof a number of plates mounted one above the other. Caps
are present on each plate, which allow the vapour to escape by bubbling through the liquid.
Working: Ascending vapour from the still passes through the bubble-caps on plate A and the
rising vapour will be richer in the more volatile component. This vapour passes through the
liquid on plate B and partially condensed. The heat of condensation partially vaporizes the
liquid. The process of condensation and vaporisation will be repeated at plate C and so on all
the way up the column. Each bubble-cap plate has the same effect as a separate still.

1
2
8
B. Plate columns (Bubble cap)
Advantages:
The bubble cap plate is effective over a wide range of vapour-
liquid proportions. There is excellent contact as the vapour
bubbles through the liquid.
Disadvantages:
(I) A layer of liquid on each plate results in considerable
hold-up of liquid over the entire column.
(2)The need to force the vapour out of the caps, throughthe
liquid, led to a large pressure drop through the column.
(3) The column does not drain when it is not in use.
(4)The structure is complicated making construction and
maintenance expensive.

1
2
9
Theory:
Fractional distillation is suitable for a system when the boiling point of the
mixture is always intermediate between those of pure components.
 There is neither a maximum nor a minimum in the composition curves.
These systems are known as zeotropic mixtures.
 Examples
Benzene and toluene
Carbon tetrachloride and cyclohexane

Distillation Process
Liquid-Vapor Composition Diagram
• When a mixture AB of a specific
composition is heated, the total
vapor pressure (composed of the
contributions of PA and PB) will rise
until it is equal to the external vapor
pressure. The mixture will begin to
boil.
• The vapor which first forms is
enriched in the more volatile
component. This behavior is shown
at right,
•Assume a two component mixture with a composition of 30%A:70%B (point W). The
boiling point of this mixture is found by drawing a vertical line from W to where it
intersects the lower curve (point X). A horizontal line drawn from X to where it intersects
the vertical axis (the temperature) gives the bp of composition W. From the point (Y) where
this horizontal line intersects the upper curve (vapor) drop a vertical line to intersect the
lower axis (the composition). Point Z gives the composition of the vapor which is in
equilibrium with a liquid of composition W at its boiling point.
13
0

Fractional Distillation
AB at composition of 5% A boils at temperature L1 and the vapors with composition V1 enter the column at
that temperature. The vapor will condense to a liquid with composition V1. The condensate L2 has a
lower boiling point (because it has more of the lower boiling liquid A) and will thus vaporize at a lower
temperature (warmed up by coming in contact with the additional vapors from below) to give vapors of
composition V2. These vapors will condense somewhat farther up the column to give a condensate L3.
If the column is long enough or contains sufficient surface area that many successive vaporization-
condensation steps (theoretical plates) can occur, the distillate that comes over the top is nearly pure A.
Distillation yielding pure A continues until all of A is removed, after which the temperature atthe
thermometer rises to the boiling point of B.
13
1

8. AZEOTROPIC AND EXTRACTIVE
DISTILLATION
Azeotropic distillation:
In which azeoptorpic mixture is broken by the addition of third
substance, which forms a new azeotrope with one of the components.
Extractive distillation:
The third substance added to the azeoptorpic mixture is relatively
nonvolatile liquid compared to the components to be separated.

8. AZEOTROPIC AND EXTRACTIVE
DISTILLATION
Azeotropic distillation:
Azeotropic Mixture(Constant boiling Mixture)
Mixture of special composition giving minimum or
maximum boiling point than individual component with
minimum or maximum boiling point respectively.

 Steam distillation is method of distillation carried out with
aid of steam.
 It is used to separate:
 High boiling substances from non-volatile impurities
 Separate immiscible liquids
1
3
6
5. STEAM DISTILLATION

Example:
Boiling point of Turpentine = 160 °C
Boiling point of Water + Turpentine Mixture = 95.6 °C
At this temperature Vapour pressure of
Water
Turpentine
= 86.245 kPa (647 mmHg)
= 15.06 kPa (113 mmHg)
Sum of vapour pressure = 101.31 kPa (760 mmHg)
Which is normal atmospheric pressure and thus high boiling liquid may be
distilled with water at a temperature much below its boiling point.

Principle:
A mixture of immiscible liquids begins to boil when sum of their vapour
pressure is equal to atmospheric pressure.
In case of mixture of water and turpentine, mixture boils below the boiling
point of pure water, though the turpentine boils at a much higher temperature
than that of water.

1
3
9
Application:
 Used to separate immiscible liquids. Ex- Water + Toluene
Extraction at much lower temperature to protect from
decomposition without loss of aroma
 To extract volatile oils like clove, anise and eucalyptus oils.
 Purification of essential oils like almond oil.
 Camphor is distilled by this method.
 Aromatic water are prepared.
Limitation:
Not suitable when two immiscible liquids reacts with each other.

 Provision are made to heat both steam can and flask separately.
Construction of assembly:
 Metallic steam can fitted with cork having two holes.
 Safety tube inserted up to bottom through one hole to maintain pressure
in side stem can, more over when steam comes out from safety tube
indicates that can is empty.
 Through other hole band tube is passed and other end of this tube is
connected to flask containing non-aqueous liquid in which tube is dipped.
 Flask and condenser is connected with delivery tube.
 Condenser is connected to receiver with help of adopter.

 Provision are made to heat both steam can and flask separately.
Working:
 Metallic steam can fitted with cork having two holes.
 Safety tube inserted up to bottom through one hole to maintain pressure
in side stem can, more over when steam comes out from safety tube
indicates that can is empty.
 Through other hole band tube is passed and other end of this tube is
connected to flask containing non-aqueous liquid in which tube is dipped.
 Flask and condenser is connected with delivery tube.
 Condenser is connected to receiver with help of adopter.

6. DESTRUCTIVE DISTILLATION (DRY DISTILLATION)
 Distillatilate is decomposition product of constituents of
the organic matter burnet in absence of air.
 Not used in lab practices but very useful in industrial
process to obtain valuable product from wood, coal and
animal matter.
 It involve the heating of dry organic matter in suitable
vessel in absence of air, until all volatile substances are
driven off.
 The distillate is the decomposition product of
constituents.
 Wood distillation industry and coal carbonation indust6r0y
provides many useful fuel material with this method

Compression distillation method was developed to meet the
need of navy and army for fresh water from sea-water.
Product obtained is quite pure and pyrogen-free, there for it
meets the requirement of pharmaceutical industry.
It is economical from the standpoint of consuption of fuel and
water
7. COMPRESSION DISTILLATION
61

 The feed water is heated in an evaporator for boiling.
 The vapour produced in tubes is separated from entrained
distilland in separator.
 The vapour is than conveyed to compressor, which
compresses it and raises its temperature to about 118 c.
 It than flows to the steam chest where it is condensed on the
outer surface of tube.
 During condensation, heat is released which is allowed for
heating of fresh feed in the tube.
62
 The vapour condensed and drained off as distillate.
7. COMPRESSION DISTILLATION

Evaporation and Distillation

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