CHAPTER 3

Separation Techniques

2013 Marshall Cavendish International (Singapore) Private Limited

Learning Outcomes
At the end of this chapter, you should be able to:

describe methods of separation and purification by:

i.
the use of a suitable solvent
ii.
filtration
iii. crystallisation
iv. evaporation
v.
sublimation
vi. distillation and fractional distillation (with particular references to the fractional
distillation of crude oil, liquid air and fermented liquor).
vii. use of separating funnel
viii. paper chromatography.
describe paper chromatography and interpret chromatograms including comparison with
known samples and the use of R f values.
explain the need to use locating agents in the chromatography of colourless compounds.
suggest suitable methods of purification, given information about the substances involved to
separate the following types of mixtures: i) solid-solid, ii) solid-liquid, iii) liquid-liquid
(miscible and immiscible).
deduce from the given melting point and boiling point the identities of substances and their
purity, as well as to describe heating and cooling graphs/curves.
explain that the measurement of purity in substances used in everyday life, e.g. foodstuff
and drugs, is important.
describe methods associated with the drying and collection of gases.
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Chapter 3 Separation Techniques

3.1 Obtaining Pure Substances from Mixtures
3.2 Separating a Solid from a Liquid
3.3 Separating Solids
3.4 Separating a Liquid from a Solution
3.5 Separating Liquids
3.6 Chromatography
3.7 Determining Purity
3.8 Methods for Collecting Gases
3.9 Methods for Drying Gases

3.1

Obtaining Pure Substances

from Mixtures

Pure Substance
A pure substance is made up of one single element or
compound. It is not mixed with any other substance.

Diamond
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3.1

Obtaining Pure Substances

from Mixtures

Mixture
A mixture is made up of two or more substances that are
not chemically combined together.

Air
Orange juice

3.2 Separating a Solid from a Liquid

Filtration
Filtration is a process of separating an insoluble
solid from a liquid.
A filter funnel and a filter paper are usually used.
Examples of mixtures:
sand and water
chalk powder and water (suspension)
clay and water
a mixture where solid particles
are found throughout the liquid

3.2 Separating a Solid from a Liquid

Filtration

mixture of
insoluble solid
in a liquid

Large insoluble
solid particles are
trapped by the
filter paper in the
filter funnel.

small particles of
liquid pass through

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3.2 Separating a Solid from a Liquid

Separation of Sand and Water
Upon filtration, the solid that
remains on the filter paper is
called the residue.
(sand)

The liquid or solution that

passes through the filter paper
is called the filtrate.
(water)
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3.2 Separating a Solid from a Liquid

Evaporation to Dryness
This is a process of obtaining a soluble solid from
a solution by heating the solution until all the water
has boiled off.
Example:
salt (sodium chloride) and water

3.2 Separating a Solid from a Liquid

Separation of Salt from Water

URL

Water in the
solution is lost to
the atmosphere.

salt solution

evaporating dish

Salt remains as a
white residue in the
evaporating dish.
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3.2 Separating a Solid from a Liquid

Evaporation to Dryness
Not all soluble substances can be obtained by
evaporation to dryness.
Example: Sugar
decomposes on heating
The solid obtained by
evaporation to dryness is
not always pure. Any
soluble impurities will be
left together with the solid
after heating.

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3.2 Separating a Solid from a Liquid

Crystallisation
Process of obtaining pure solid sample
(soluble solid) from its solution.
Examples:

hydrated copper(II)
sulfate crystals

sodium carbonate
crystals
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3.2 Separating a Solid from a Liquid

Preparation of Pure Copper(II) Sulfate Crystals
by Crystallisation
Step 1
The solution is heated
to remove most of the
solvent (water).

impure
copper(II) sulfate
solution

Heating is stopped
when a saturated
solution is formed.
URL

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3.2 Separating a Solid from a Liquid

Preparation of Pure Copper(II) Sulfate Crystals
by Crystallisation
Step 2

a solution that contains as much dissolved

solute as it can at a given temperature

The hot, saturated solution is allowed to cool.

The dissolved copper(II) sulfate appears as pure crystals.
Rapid cooling produces small
crystals while slow cooling
produces large crystals.
copper(II) sulfate crystals
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3.2 Separating a Solid from a Liquid

Preparation of Pure Copper(II) Sulfate Crystals
by Crystallisation
Step 3
The cold solution is removed by filtration. The residue
of pure crystals is washed with cold distilled water.
filter paper
pure copper(II)
sulfate crystals

The crystals are then dried by pressing them between

pieces of filter paper.

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3.3

Separating Solids
Using a Suitable Solvent
To separate a mixture of two solids, we use a solvent
in which one solid is soluble. (The other solid is
insoluble in that solvent.)
Different solids dissolve in different solvents. Some
common solvents are water and ethanol.

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3.3

Separating Solids

Example:
Separating sodium chloride and sand
Mixture of sodium chloride
and sand
Add water to dissolve
sodium chloride

sodium chloride solution + sand

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3.3

Separating Solids

Example:
Separating sodium chloride and sand
sodium chloride solution + sand
Filter the mixture

filtrate
sodium chloride
solution

residue
sand
+
traces of sodium
chloride solution

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3.3

Separating Solids

Example:
Separating sodium chloride and sand
filtrate
sodium chloride
solution
Evaporate
to dryness

sodium chloride

residue
sand
+
traces of sodium
chloride solution
Wash with
distilled water

sand
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3.3

Separating Solids

Sublimation
Sublimation is used to separate a solid that
sublimes from one that does not.
Some substances, such as ammonium chloride
and iodine, sublime.

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3.3

Separating Solids
Using Sublimation to Separate Two Solids
We can make use of this property to separate a
substance that sublimes from one that does not
e.g. salt and iodine.
solidified
iodine

wet cloth
to cool

iodine
vapour

mixture of
iodine and sand

heat

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3.3

Separating Solids
Using a Magnet
A magnet can be used to separate a
magnetic substance from a non-magnetic
substance.
Examples of magnetic materials:
Iron
Steel
Nickel
Cobalt
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3.3

Separating Solids
Using Magnets to Separate Two Solids
Some metals are
magnetic.
We can use this property
to separate these metals
(e.g. iron, nickel, cobalt,
steel) from mixtures.

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3.4

Separating a Liquid from

a Solution
Obtaining the Solvent from a Solution
SOLUTION
Evaporation
Crystallisation
SOLUTE

Simple distillation

SOLVENT

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3.4

Separating a Liquid from

a Solution
Simple Distillation
Simple distillation is used to separate a pure
solvent (liquid) from a solution.
Examples:
Extraction of water from:
sea water
salt (sodium chloride) solution
sugar solution

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3.4

Separating a Liquid from

a Solution
Setting Up the Distillation Apparatus
Thermometer
bulb should be
just beside the
side arm
leading to the
condenser.

Boiling chips
are placed in
the flask to
ensure smooth
boiling.

water out

Water enters the

condenser from the
bottom and leaves
from the top.
Condenser must be
sloping downwards.

water in

Volatile liquids can be kept in the

liquid state by placing receiver on ice.

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3.4

Separating a Liquid from

a Solution
Simple distillation of salt solution

4. The salt solution

becomes more
concentrated as
distillation
continues. Salt will
be collected as
residue.
1. Boiling chips
are added to
ensure smooth
boiling. Water
vaporises, rises
and enters the
condenser.

2. Water boils and becomes

vapour. Thermometer measures
temperature of the vapour.
3. Water vapour
is cooled and
condenses into
pure liquid
(distillate).

5. Pure water
is collected
as distillate.

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3.5

Separating Liquids
Using a Separating Funnel
This method can be used to separate immiscible
liquids. Liquids that do not dissolve in each other
are described as immiscible.
Example:
Oil and water

separating
funnel
oil
water

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3.5

Separating Liquids

Using a Separating Funnel to Separate

Immiscible Liquids
Step 1

Pour the mixture of oil and water

into the separating funnel.
(Make sure the tap is closed.)

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3.5

Separating Liquids

Using a Separating Funnel to Separate

Immiscible Liquids
Step 2
Support the separating funnel using a
retort stand.
Then, place a clean beaker
below the separating funnel.

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3.5

Separating Liquids

Using a Separating Funnel to Separate

Immiscible Liquids
Step 3

Allow the liquids to separate

completely. This may take some
time. The denser liquid (water) will
be the bottom layer.

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3.5

Separating Liquids

Using a Separating Funnel to Separate

Immiscible Liquids
Step 4
Open the tap of the funnel to
allow the bottom layer to drain
into the beaker.
Close the tap before the top
layer of liquid runs out.

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3.5

Separating Liquids

Using a Separating Funnel to Separate

Immiscible Liquids
Step 5
Place another beaker below the
funnel. Open the tap to allow a little of
the top layer of liquid into the beaker.
Dispose of the liquid collected.
Now, the separating funnel contains
only oil while the beaker from Step 4
contains only water.
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3.5

Separating Liquids
Fractional Distillation
This method can be used to separate a mixture of
miscible liquids with different boiling points.
Liquids that mix together completely to form a
solution are described as miscible.
Examples:
Ethanol and water
Purified air
Crude oil
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3.5

Separating Liquids
Comparing Simple
Distillation with Fractional
Distillation
A fractionating column is attached
to the round-bottomed flask and the
condenser for fractional distillation.

simple distillation

Glass beads/plates/spiral in the

fractionating column provide a large
surface area for vapour to
condense on.
fractional distillation
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3.5

Separating Liquids
Fractional Distillation

2. The water vapour

condenses in the
fractionating column
and falls back into the
flask.
1. Ethanol vapour and
water vapour rise up
the column as the
solution is heated.

3. Ethanol, which has a

lower boiling point than
water, reaches the
upper part of the column
and is distilled over.

4. At this stage, the

thermometer shows a constant
temperature of 78oC, which is
the boiling point of ethanol.

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3.5

Separating Liquids
Fractional Distillation

7. When all the ethanol

has distilled over, the
temperature rises
rapidly to 100oC, which
is the boiling point of
water. At this
temperature, water
distils over and can be
collected separately.

5. In this condenser,
hot ethanol vapour condenses
as running water cools it;
liquid ethanol flows down the
inner tube of the condenser
and into the receiver.

6. Ethanol is collected as the

distillate in the receiver.

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3.5

Separating Liquids
Fractional Distillation

Graph showing how

temperature changes
as a solution of ethanol
and water is
fractionally distilled

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3.5

Separating Liquids

Industrial Applications of Fractional Distillation

To separate:
the various components of crude oil such as petrol,
kerosene, diesel in oil refineries.
nitrogen, oxygen and argon in liquid air.
ethanol from the fermentation mixture of water,
glucose and malt in breweries.
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3.6

Chromatography

Chromatography is the method of separating two or

more components that dissolve in the same solvent.
Examples:
Pigments in plants

Dyes in paints Colouring in food

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3.6

Chromatography

The chromatography paper with the separated

components is called a chromatogram.

lid
glass tank
chromatogram

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3.6

Chromatography

Separating Dyes Found in Green

Food Colouring
Chromatography
paper
Green food
colouring
Pencil line
Ethanol or water
as solvent

1. Place a spot of green food

colouring on the paper.
2. Dip the paper into a
solvent such as ethanol or
water. Ensure that the
coloured spot is above the
solvent level.
3. The components will
separate as the solvent
travels up the paper.
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3.6

Chromatography

Principle Behind Paper Chromatography

Separation of a substance into its different components
depends on the relative solubility of the component.
The more soluble component travels faster and further
up the paper than the less soluble components.
Identical dyes travel up the same distance and produce
the same colour on the paper when the same solvent is
used.
The chromatography paper with the separated
components is called a chromatogram.

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3.6

Chromatography
Interpretation of a Chromatogram
This food colouring
is not pure.
It consists of 2
component dyes.
This is a pure
substance. Why?

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3.6

Chromatography
What is
Rf value?
The positions of the
solvent front
(position reached by
solvent) and spot on
a chromatogram
depend on how long
the experiment was
allowed to run.

Chromatogram
after a period
of time.

Chromatogram
after a longer
period of time.

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3.6

Chromatography

What is Rf value?
The ratio between the
distance travelled by
the substance
and
the distance travelled by
the solvent is a
constant.
This ratio is called
the Rf value of the
substance.

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3.6

Chromatography

Rf value of substance is the same regardless

of distance travelled on chromatogram.

3 cm
Rf =
4.5 cm

3.5 cm
Rf =
5.2 cm

= 0.67

= 0.67

Chromatogram
after a period
of time.

Chromatogram
after a longer
period of time.

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3.6

Chromatography
Rf Value
The Rf value of a substance does not change
as long as chromatography is carried out under
the same conditions (i.e. same solvent and
same temperature).
This property allows us to easily identify
a substance on a chromatogram.

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3.6

Chromatography

Example: Comparison with known samples

Chromatography was performed on a sample of food

colouring (X) and 4 banned dyes (A, B, C and D).
If X contains any of the 4 banned dyes, it is not safe to
be consumed.

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3.6

Chromatography

Example: Comparison with known samples

Conclusions that can be drawn from the chromatogram:

Identical dyes produce spots at the same height.
Sample X does not contain the banned dyes A, B and D.
However, X contains the banned dye C. Therefore, it
must not be consumed.

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3.6

Chromatography

Example: Comparison with known samples

Other conclusions that can be drawn from the chromatogram:

Dyes A and D are pure.
Both dye B and dye C are mixtures of two different dyes.
Sample X is a mixture of three dyes.

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3.6

Chromatography
How do we identify colourless substances?
Chromatography can also be used for
colourless substances such as amino acids.
To separate and analyse colourless
substances, we apply a locating agent on a
chromatogram.
The locating agent reacts with the colourless
substances to form coloured spots.

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3.6

Chromatography
Uses of Chromatography
Given a sample, chromatography can be used to:
separate the components in a sample;
identify the components present in a sample;
identify substances;
determine its purity.

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3.7

Determining Purity

Importance of Purity
Impurities in drugs must be
detected as they may cause
undesirable side effects.
Chemicals are often added to
food and beverages. It is
important to ensure that our food
contain only chemicals that are
safe for consumption.
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3.7

Determining Purity

Determination of a Pure Substance

By doing one of the following:
Checking for exact and constant (or fixed) melting
point of a solid
Checking the exact and constant (or fixed) boiling
point of a liquid
Performing chromatography
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3.7

Determining Purity

Determining Purity by Melting and

Boiling Points
A pure solid has an exact and constant melting point.

A pure liquid has an exact and constant boiling point.

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3.7

Determining Purity
Effect of Impurities on Melting Points
Impurities decrease the melting point of a solid.

The greater the amount of impurities, the lower the

melting point of the substance.
Impurities cause melting to take place over a range
of temperatures.

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3.7

Determining Purity
Effect of Impurities on Boiling Points
Impurities increase the boiling point of a liquid.

The greater the amount of impurities, the higher

the boiling point of the substance.
Impurities cause boiling to take place over a range
of temperatures.

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3.7

Methods for Collecting Gases

The method of collection of gas depends on:

solubility of the gas in water;
density of the gas, compared to air.

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3.7

Methods for Collecting Gases

Downward displacement of water

For collecting gases that are insoluble
or slightly soluble in water
E.g. carbon dioxide,
hydrogen, oxygen
delivery tube

gas jar
gas

gas

URL

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3.7

Methods for Collecting Gases

Downward delivery of gas

For collecting gases that are soluble in water
and denser than air
gas

E.g. chlorine,
hydrogen chloride
gas jar

delivery
tube

gas
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3.7

Methods for Collecting Gases

Upward delivery of gas

For collecting gases that are soluble
in water and less dense than air
gas

E.g. ammonia

gas jar

delivery
tube
gas

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3.7

Methods for Collecting Gases

If we need to collect and measure the volume of

a gas, we can also use a gas syringe.

barrel
plunger

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3.8

Methods for Drying Gases

Drying with Concentrated Sulfuric Acid
moist
gas in

dry gas
out

Note the
positions of the
delivery tubes
Concentrated sulfuric
acid used to dry most
gases except ammonia

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3.8

Methods for Drying Gases

Drying with Quicklime (Calcium Oxide)
dry gas
out

Quicklime used for

drying ammonia
moist
gas in
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3.8

Methods for Drying Gases

Drying with Fused Calcium Chloride
moist
gas in

dry gas
out

Fused calcium
chloride used for
drying most gases

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