Separation Techniques Used in Chemistry

Learning Objectives
1. Identify and explain the principles behind a particular separation
technique that is used in daily life and in industry.
2. Identify an appropriate separation technique to separate a mixture based
on the physical properties of the components of the mixture. These
properties include solubility, density, melting and boiling points, thermal
stability, magnetic properties and particle size.
 Separation Techniques Used in Chemistry
Darshan Singh, Prateek Harbola*, Meenu Choniyal**
Government Inter College, Syakote
* Government Inter College, Salani
**Inter College, Quarali

Abstract
A separation process is a method that converts a mixture or solution of chemical
substances into two or more distinct products. At least one of results of the separation is
enriched in one or more of the source mixture's constituents. In some cases, a separation may
fully divide the mixture into pure constituents. Separations exploit differences in chemical
properties or physical properties between the constituents of a mixture. This study involves
various methods of separation viz. decanting, filtration, crystallization, distillation,
magnetization, chromatography.
Key Words: Chromatography, Centrifugation, Simple distillation, Fractional distillation,
Sublimation.
Introduction
Separation techniques are used to separate mixtures into its constituent elements and/or
compounds. Recall that a mixture is contains elements and/or compounds which are not
chemically combined together. By separating the constituents of the mixtures, we are able to
find out the properties of the known/unknown substances from mixtures and possibly use them
for the production of useful substances such as medicines. Depending on the physical and
chemical properties of the substances in the mixture, we can choose the most appropriate
separation technique to isolate them from the mixture.
A separation process is a method that converts a mixture or solution of chemical
substances into two or more distinct product mixtures.[1] At least one of results of the separation
is enriched in one or more of the source mixture's constituents. In some cases, a separation may
fully divide the mixture into pure constituents. Separations exploit differences in chemical
properties or physical properties (such as size, shape, mass, density, or chemical affinity)
between the constituents of a mixture. Processes are often classified according to the particular
differences they use to achieve separation. If no single difference can be used to accomplish a
desired separation, multiple operations can often be combined to achieve the desired end.
With a few exceptions, elements or compounds exist in nature in an impure state. Often these
raw materials must go through a separation before they can be put to productive use, making
separation techniques essential for the modern industrial economy.
The purpose of a separation may be analytical, can be used as a lie component in the
original mixture without any attempt to save the fractions, or may be preparative, i.e. to
"prepare" fractions or samples of the components that can be saved. The separation can be done
on a small scale, effectively a laboratory scale for analytical or preparative purposes, or on a
large scale, effectively an industrial scale for preparative purposes, or on some intermediate
scale. In some cases, separations require total purification, as in the electrolysis
refining of bauxite ore for aluminium metal, but a good example of an incomplete separation
technique is oil refining. Crude oil occurs naturally as a mixture of various hydrocarbons and
impurities. The refining process splits this mixture into other, more valuable mixtures such
as natural gas, gasoline and chemical feedstocks, none of which are pure substances, but each
of which must be separated from the raw crude. In both of these cases, a series of separations
is necessary to obtain the desired end products. In the case of oil refining, crude is subjected to
a long series of individual distillation steps, each of which produces a different product or
intermediate.
Methods
Following separation methods are used for the separation of mixtures:
Decanting: A crude way of separating insoluble solids from liquids, as the liquid is poured
away and collected in another container. Note that the insoluble solid should be able to settle
down on standing and this method is not effective for obtaining clear liquid from the mixture
especially when the insoluble solid is very fine and light.

Fig. 1. Decantation.
Filtration: Separation of solids or groups of solids from the liquid in a mixture, using a
medium through which the liquid can pass. The medium which we are using over here is the
filter paper. The filter paper is folded and placed onto the filter funnel.
The liquid-solid mixture is poured onto the filter paper. Using a filter paper with pores of a
smaller size than the solid particles (and is larger than the size of the liquid molecules), the
liquid (or solvent) should pass through the filter paper, and is collected by a collection container
placed at the bottom of the filter funnel.

Fig. 2. Filteration.
The liquid that passes through the filter paper is called the filtrate while the solid left on the
filter paper is called the residue.
Separating Funnel
Separating funnel is used mainly to segregate two immiscible liquids. The mechanism
involves taking advantage of the unequal density of the particles in the mixture. Oil and water
can be easily separated using this technique.
Evaporation: In the case which we do not need to collect the solvent. The solvent is boiled off
and escape into the air while the solute is left behind in the holding container. Note that this
method is not suitable for use on solutes which can decomposed by heating (e.g. Copper II
sulfate).

Fig. 3. Evaporation.
 Separation of salt by evaporation
Crystallisation: Used to separate a dissolved heat-liable (will decompose upon heating and
hence can sublime) solid (solute) from a solution. You will need a saturated solution to being
with. A saturated solution is a solution that contains the maximum amount of solute dissolved
in a given volume of solvent at a particular temperature. Do not mix this up with a concentrated
solution, which is a solution that contains lots of solute dissolved in it. The amount of solute in
a concentrated solution may/may not be the maximum amount which can be dissolved in the
solution. First, you will need to heat to evaporate off most of the solvent from a solution to
make a hot and nearly saturated solution. Else, if you already have a saturated solution, heat it
up slightly such that the solution becomes hot. After which, allow the hot solution to coll
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.

Fig. 4. Crystallisation.

Seeding: Using a small crystal of salt (the “seed”) to collect the solid solute crystals in a
saturated solution. No heat is required but will take a long time.

Fig. 5. Seeding.
As the saturated solution continues to evaporate overtime, there is an increasing amount of
solute which will crystallise out from the solution. These solid solute crystals will attach itself
to the “seed”, resulting in a grow in size of the “seed” overtime. The enlarged “seed” can then
be removed from the solution at the end of the procedure (or when it is large enough for use in
other applications).
Simple Distillation:
Simple distillation is a method used for the separation of components of a mixture containing
two miscible liquids that boil without decomposition and have sufficient difference in their
boiling points.
The distillation process involves heating a liquid to its boiling points, and transferring
the vapours into the cold portion of the apparatus, then condensing the vapors and collecting
the condensed liquid in a container. In this process, when the temperature of a liquid rises, the
vapor pressure of the liquid increases. When the vapor pressure of the liquid and the
atmospheric pressure reach the same level, the liquid passes into its vapor state. The vapors
pass over the heated portion of the apparatus until they come into contact with the cold surface
of the water-cooled condenser. When the vapor cools, it condenses and passes down the
condenser and is collected into a receiver through the vacuum adapter.
To separate and collect solvent from a solution of solutes, or in a mixture of two
different liquids (with different boiling points), with the use of heat. The logic behind how
simple distillation works is actually the same as that of evaporation. The only difference is that
a closed neck container (distillation flask) is used to hold the mixture to be heated, with a
opening/tube by the side (of the container) connected to a condenser. The setup for simple
distillation should look something like this:

Fig. 6. Simple distillation.

As the sea water mixture is heated, water boil and changes into water vapour gas. Since hot air
rises and cold air sinks, the hot water vapour moves to the top of the flask and passes into the
condenser. The tubes on the condenser are attached to a water source, with the water flowing
in through the lower end and flowing out through the higher end of the condenser. This creates
a cooler surface for the hot water vapour to condense on. As the condenser is tilted downwards,
towards the collecting container at the end of the setup, the condensed water flows and drips
into the collecting container.
Fractional Distillation:
Fractional distillation is used for the separation of a mixture of two or more miscible liquids
for which the difference in boiling points is less than 25K. The apparatus for fractional
distillation is similar to that of simple distillation, except that a fractionating column is fitted
in between the distillation flask and the condenser.

A simple fractionating column is a tube packed with glass beads. The beads provide surface
for the vapors to cool and condense repeatedly. When vapors of a mixture are passed through
the fractionating column, because of the repeated condensation and evaporation, the vapors of
the liquid with the lower boiling point first pass out of the fractionating column, condense and
are collected in the receiver flask. The other liquid, with a slightly higher boiling point, can be
collected in similar fashion in another receiver flask.
This method is used to separate miscible liquids with different but very close boiling point.
This method is more efficient than simple distillation. A fractionating column is introduced
between the distillation flask and the condenser. The upper portion of the column, which is
closer to the condenser, is cooler than the lower portion and hence, only gases with the same
temperature as the upper portion are allowed to pass on to the condenser. On the other hand,
the gases with higher boiling points will condense and flow back to the bottom into the
distillation flask, and is heated into a gas again. At the end, liquid with the lowest boiling point
will be the first to boil and hence the first to be distilled out and collected.
Fig. 7. Fractional distillation.

Sublimation: To separate a mixture of solids containing one which sublimes and one
(or more than one) which does not, by heating the mixture. A cotton-stoppered inverted funnel
is placed over the mixture. When the mixture is heated, the heat-liable solid sublime and turn
into a gas, and travel to the top of the inverted funnel. Once the hot gas touches the cooler
funnel, it solidifies back into a solid. The solid can then be scrapped off and collected in another
container from the funnel.
 Fig. 8. Sublimation.

Magnetization or Magnetic Attraction: This method involves the separation of magnetic

substances from non-magnetic substances by means of a magnet.

Fig. 9. Magnetization.
Chromatography:
Chromatography is a separation technique used to separate the different components in a liquid
mixture. It was introduced by a Russian Scientist Michael Tswett. Chromatography involves
the sample being dissolved in a particular solvent called mobile phase. The mobile phase may
be a gas or liquid. The mobile phase is then passed through another phase called stationary
phase. The stationary phase may be a solid packed in a glass plate or a piece of chromatography
paper. The various components of the mixture travel at different speeds, causing them to
separate. There are different types of chromatographic techniques such as column
chromatography, TLC, paper chromatography, and gas chromatography.
Paper Chromatography: Paper chromatography is one of the important chromatographic
methods. Paper chromatography uses paper as the stationary phase and a liquid solvent as the
mobile phase. In paper chromatography, the sample is placed on a spot on the paper and the
paper is carefully dipped into a solvent. The solvent rises up the paper due to capillary action
and the components of the mixture rise up at different rates and thus are separated from one
another. This method is used to separate a mixture of solutes (or liquid) with different solubility
and degree of adsorption. This method uses a porous or absorbent medium (e.g. paper or jel)
and a solvent which can move over the material. This method is commonly used for separating
a mixture of dyes in ink or different types of sugars (e.g. glucose, fructose, sucrose).
In particular, to carry out paper chromatography, get a rectangular piece of filter paper and
draw a pencil line 2 cm away from the bottle edge of the paper. Note that pen cannot be used
to draw the line here as its ink mixture will be resolved and there will be no reference line left
at the end of the experiment.

Place a drop of sample ink or mixture on the line. Let the sample dry before placing more
sample on the same spot. Place the other known components (e.g. red, blue and green dye if
we are separation an ink sample) on the line, with a distance away from the first ink sample,
for comparison.

Place the chromatography paper on a suitable solvent (e.g. ethanol). The solvent will “run” up
the chromatography paper after some time.
As the solvent travels up the paper, the dyes are dissolved in the solvent. Since some dyes are
more soluble, they travel up the paper faster than the rest. The less soluble dyes are absorbed
more strongly on the paper near the pencil line. This means that identical dyes will travel the
same distance along the length of the paper.
When the solvent reaches near the top of the paper, remove the paper and mark the location
where the solvent stops running. By comparing the ink sample with the colour dyes, we know
the composition of the ink sample. For this case, we can conclude that the ink sample contain
red, blue and green dyes.

A separating funnel is used for the separation of components of a mixture between two
immiscible liquid phases. One phase is the aqueous phase and the other phase is an organic
solvent. This separation is based on the differences in the densities of the liquids. The liquid
having more density forms the lower layer and the liquid having less density forms the upper
layer.
Thin-layer chromatography (TLC) (a) The solution is applied near one end of a plate coated
with silica or alumina. (b) The plate is then immersed in a solvent, which rises up the plate by
capillary action.
Discussion
Everybody hates capsicum, right? So, what do we do when our mother mixes capsicum with other
vegetables to get us to eat it? That’s right, we separate it out. Every day we see instances where one
substance is separated from the other.
 Mixtures can be separated using a variety of techniques.
 Distillation takes advantage of differences in boiling points.
 Evaporation removes a liquid from a solution to leave a solid material.
 Filtration separates solids of different sizes.
 Chromatography involves solvent separation on a solid medium.
Acknowledgment
The authors are grateful to DIET, Bageshwar for providing this opportunity of
presenting this paper.
References
1. Wilson, Ian D.; Adlard, Edward R.; Cooke, Michael; et al., eds. (2000). Encyclopedia of
separation science. San Diego: Academic Press. ISBN 978-0-12-226770-3.
2. https://en.wikipedia.org/wiki/Separation_process
3. https://chemistrynotesblog.wordpress.com/seperation-techniques/introduction-to-
separation-techniques-2/
4. NECRT note book class XII Chemistry Part 2.