SEPARATION TECHNIQUES

Chemist/ Emad Ashmawy

DEFINITION:

Separation techniques are those techniques that can be used to

separate two different states of matter such as liquids and solids.

Separation processes or a separation method or simply a separation

is methodology to attain any mass transfer phenomenon that
convert a mixture of substances into two or more distinct product
mixtures.

Separation is an important asset to purify component of interest

from a mixtures.
NEED OF SEPARATION
TECHNIQUES:

TO IDENTIFY WHAT TO BE TO OBTAIN IMPORTANT AND TO REMOVE UNWANTED

SEPARATED FROM MIXTURE. PURE SUBSTANCES. PARTICLES.
TYPES OF SEPARATION
TECHNIQUES:
• Separation techniques are classified based on type of
mixtures:
Separation techniques

For solid in liquid mixtures For liquid in liquid mixtures

Heterogenous:
1. Sedimentation /
Homogenous: gravitation Homogenous: Heterogenous:
1. Evaporation 2. Filtration 1. Simple or 1. Partition
2. Distillation fractional distillation. separation using
3. Magnetic
3. centrifugation separation 2. Chromatography funnel
4. Fractional
distillation
 This method involves the separation of magnetic
substances from non-magnetic substances by
means of magnet.

Takes advantage of physical property of

magnetism, so it useful only for certain
substances such as ferromagnetic (materials
MAGNETIC strongly affected by magnetic fields) and
paramagnetic (materials that are less affected,
SEPARATION: but the effect is still noticeable).

This method involves the separation of magnetic

substances from non-magnetic substances by
means of magnet.
• Applications:
• Waste management, low-magnetic field separation in water purification
and separation of complex mixtures.
• To remove metal contaminants from pharmaceutical product streams.
• Magnetic cell separation. It is currently being used in clinical therapies,
more specifically in cancer and hereditary diseases researches.
• These techniques are combined with PCR (polymerase chain reaction), to
increase sensitivity and specificity of results.
DECANTATION:
Decantation is a process for the separation of
mixtures of immiscible liquids or of a liquid and a solid
mixture such as a suspension.

Immiscible liquid separation:

• Takes advantage of differences in density of the liquids.
• A separatory funnel is an alternative apparatus for separating
liquid layers. It has a valve at the bottom to allow draining off the
bottom layer. It can give a better separation between the two
liquids.
• Example: separation of mixture of oil and water.
 • Takes advantage of gravity/sedimentation of
solids in case solid-liquid separation.
• Sedimentation: The tendency
of particles in suspension to settle down in the
fluid due to certain forces like gravity, centrifugal
acceleration, or electromagnetism is called as
sedimentation.
Liquid-solid • The solid that gets settled down is called as
separation: sediment.
• In laboratory it can be done in test tubes. To
enhance productivity test tubes should be placed
at 45° angle to allow the sediments to settle at
the bottom of the apparatus.
• A decanter centrifuge may be used for
continuous solid-liquid separation.
 Examples/applications:
• Decantation is frequently used to purify a liquid by separating it
from a suspension of insoluble particles.
• Decantation is also present in nanotechnology. In the synthesis of
high-quality silver nanowire (AgNW) solutions and fabrication
process of high-performance electrodes, decantation is also being
applied which greatly simplifies the purification process.
• Fat is determined in butter by decantation.
• In sugar industry, processing of sugar beets into granular sugar
many liquid - solid separations are encountered.
 Takes advantage of physical property of state of matter,
its size and solubility in liquid.

Mechanical,
physical or • The substance which is
biological left behind in the
operations that
FILTRATION: separates solids filtration medium is
from fluids called residue.
(liquids or gases ) • The liquid which passes
by adding a
medium through through the filtration
which only the medium is called
fluid can pass can
be called as filtrate.
filtration.
 Applications:
Most important techniques used by
chemists to purify compounds.

HEPA filters in air conditioning to remove

particles from air.
In the laboratory, a Büchner funnel is often
used, with a filter paper serving as the
porous barrier.
 CENTRIFUGATION:

Centrifugation is a
technique which
It is used to separate
involves the application
mixtures where the A centrifuge is a
of centrifugal force to
solid particles don’t device that separates
separate particles from
settle faster and which particles from a solution
a solution according to
are of very small size through use of a rotor.
their size, shape,
and can't be separated
density, viscosity of the
by filtration.
medium and rotor
speed.
 The rate of centrifugation is
More-dense components of the specified by the angular
mixture migrate away from velocity usually expressed
the axis of as revolutions per
the centrifuge (move to the minute (RPM), or acceleration
outside), while less-dense expressed as g. The
components of the mixture conversion factor between
migrate towards the axis, i. e., RPM and g depends on
move to the center. the radius of the
centrifuge rotor.
Applications/examples:
Microcentrifuges are used to process small volumes of
biological molecules, cells, or nuclei.

Used in diagnostic laboratories for blood and urine tests.

Aids in separation of proteins using purification

techniques such as salting out.
Differential Centrifugation used to separate organelles
and membranes found in cells.
EVAPORATION:
Evaporation is type of vaporization that occurs on the surface of liquid as it
changes into gas phase.
This separation technique can be used to separate solutes that are
dissolved in solvent, by boiling the solution. The solvent gets vaporized
leaving back the solute.
Factors affecting:

• Concentration of the substance evaporating in the air.

• Flow rate of air, pressure, temperature.
• Surface area.
• Intermolecular forces.
 Evaporation
equipment:

Natural Forced
Film
circulation circulation
evaporators:
evaporators: evaporators.

Evaporating Climbing
still and film
pans. evaporators.

Horizontal
Evaporating
film
short tubes.
evaporators.
 Applications/examples:

• Recovering salts from solution.

• The use of evaporation to dry or concentrate samples
is a common preparatory step for many laboratory
analyses such as spectroscopy and chromatography.
• Demineralization of water.
 DISTILLATION:
Distillation is a
Distillation is an
purification process
effective method to The separation of a
where the
separate mixtures mixture of liquids
components of a
comprised of two or based on the physical
liquid mixture are
more pure liquids property of boiling
vaporized and then
(called point.
condensed and
“components”).
isolated.
The mixture is heated until one of the
components boils (turns to a vapor). The
vapor is then fed into a condenser, which
cools the vapor and changes it back into a
liquid that is called distillate. What
remains in the original container is called
the "residue".
 Simple
distillation:
 Fractional
distillation:
 Types:

Fractional: Fractional distillation is used for the

Simple: Used to separate liquid mixtures which boil
separation of a mixture of two or more miscible
without decomposition and have enough difference in
liquids for which the difference in boiling points is
their boiling points.
less than 25K.

Applications: Applications:
The apparatus for fractional
distillation is like that of simple
distillation, except that a Separation of
Separation of fractionating column is fitted in different fractions
acetone and between the distillation flask and from petroleum
water. the condenser. products.

Separation of a
Distillation of mixture of
alcohol. methanol and
ethanol.
Other applications/examples:
Separation of volatile oils.

Separation of drugs obtained from plant or animal

sources – vitamin A from fish liver oil.

Purification of organic solvents.

Manufacture of official preparations – spirit of nitrous

ether, spirit of ammonia, distilled water, and water for
injection.

Refining petroleum products.

 CRYSTALLIZATION:

• Crystallization is the (natural or artificial)

process by which a solid forms, where the atoms
or molecules are highly organized into a
structure known as a crystal.
• Used to separate a dissolved heat-liable (will
decompose upon heating and hence can
sublime) solid (solute) from a solution.
• Most minerals and organic molecules crystallize
easily, and the resulting crystals are generally of
good quality, i.e. without visible defects.
First, the solution is heated to evaporate off most of the solvent
to make a hot and nearly saturated solution.

After which, the hot solution to is kept for cooling, naturally.

The solubility of the solute decreases as the solution is cooled,
and the excess solute which can no longer be dissolved in the
saturated solution crystallizes out of the solution.

The crystals which are formed can be separated from the

remaining solution by filtration.
 • Purification of drugs.
• Separation of crystals of alum from
impurities sample.
• Fractional Crystallization : It is
possible to separate mixtures of
Applications different ionic compounds having
/ identical chemical composition by
examples: dissolving them in water and
adjusting the temperature of the
solution so that one compound
crystallizes out and the other does
not.
• E.g. K2SO4 and KNO3
 • Sublimation is the transition of a
substance directly from
the solid to the gas phase,
without passing through the
intermediate liquid phase.
SUBLIMATIO • This technique takes the
N advantage of substance’s
SEPARATION: sublimable property.
• Separate a mixture of solids
containing one which sublimes
and one (or more than one) which
does not, by heating the mixture.
Applications/examples:
• Separate iodine from sand.
• Dye-sublimation printers help in rendering digital
pictures in a detailed and realistic fashion which helps
in the analysis of substances.
• Sublimation finds practical application in forensic
sciences.
• Chemists usually prefer sublimation as a purification
method to purify volatile compounds.
 CHROMATOGRAPHY:
• Chromatography is a separation technique used to separate
the different components in a liquid mixture.
• The mixture is dissolved in a fluid called the mobile
phase, which carries it through a structure holding another
material called the stationary phase.
• Chromatography is vast separation technique which has many
methods or has different principles of separation involved.
EXTRACTION
TECHNIQUES:

• Involves the separation of medicinally active

portions of plant or animal tissues from the
inactive or inert components by using
selective solvents in standard extraction
procedures.
• Different methods of extraction are:
Method Solvent Temperature Pressure Time Volume of organic Polarity of natural
solvent consumed products extracted

Maceration Water, aqueous and non-aqueous Room temperature Atmospheric Long Large Dependent on extracting
solvents solvent

Percolation Water, aqueous and non-aqueous Room temperature, Atmospheric Long Large Dependent on extracting
solvents occasionally under heat solvent

Decoction Water Under heat Atmospheric Moderate None Polar compounds

Reflux extraction Aqueous and non-aqueous solvents Under heat Atmospheric Moderate Moderate Dependent on extracting
solvent

Soxhlet extraction Organic solvents Under heat Atmospheric Long Moderate Dependent on extracting
solvent

Pressurized liquid Water, aqueous and non-aqueous Under heat High Short Small Dependent on extracting
extraction solvents solvent

Supercritical fluid Supercritical fluid (usually S-CO2), Near room temperature High Short None or small Nonpolar to moderate
extraction sometimes with modifier polar compounds

Ultrasound assisted Water, aqueous and non-aqueous Room temperature, or under Atmospheric Short Moderate Dependent on extracting
extraction solvents heat solvent

Microwave assisted Water, aqueous and non-aqueous Room temperature Atmospheric Short None or moderate Dependent on extracting
extraction solvents solvent

Pulsed electric field Water, aqueous and non-aqueous Room temperature, or under Atmospheric Short Moderate Dependent on extracting
extraction solvents heat solvent

Enzyme assisted Water, aqueous and non-aqueous Room temperature, or heated Atmospheric Moderate Moderate Dependent on extracting
extraction solvents after enzyme treatment solvent

Hydro distillation and Water Under heat Atmospheric Long None Essential oil (usually non-
steam distillation polar)
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