CHAPTER 3

Separation and Purification

© 2013 Marshall Cavendish International (Singapore) Private Limited

© 2014 Marshall Cavendish Education Pte Ltd
(Formerly known as Marshall Cavendish International (Singapore) Private Limited)
Chapter 3 Separation and Purification

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

2
3.1 Obtaining Pure Substances
from Mixtures

Learning Outcome
At the end of this section, you should be able to:

• understand the difference between pure

substance and mixtures.

3
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.

A white diamond

4
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 5
Chapter 3 Separation and Purification

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

6
3.2 Separating a Solid from a Liquid

Learning Outcome

At the end of this section, you should be able to:

• describe methods of separating and purifying

mixtures of a solid and a liquid.

7
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 8
3.2 Separating a Solid from a Liquid

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

mixture of
insoluble solid
in a liquid small particles of
liquid pass through

9
URL
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)
10
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

11
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.
12
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.
13
3.2 Separating a Solid from a Liquid

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

Examples:

hydrated copper(II) sodium carbonate

sulfate crystals crystals
14
3.2 Separating a Solid from a Liquid

Preparation of Pure Copper(II) Sulfate Crystals

by Crystallisation
Step 1
impure copper(II)
• The solution is heated sulfate solution
to remove most of the
solvent (water).

• Heating is stopped
when a saturated
solution is formed.

URL 15
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

16
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.
17
Chapter 3 Separation and Purification

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

18
3.3 Separating Solids

Learning Outcome
At the end of this section, you should be able to:

• describe methods of separating and purifying

mixtures of solids.

19
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.

20
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

21
3.3 Separating Solids

Example:
Separating sodium chloride and sand
sodium chloride solution + sand

Filter the mixture

filtrate residue
sodium chloride sand
solution +
traces of sodium
chloride solution
22
3.3 Separating Solids

Example:
Separating sodium chloride and sand

residue
filtrate
sand
sodium chloride
+
solution
traces of sodium
chloride solution
Evaporate
to dryness Wash with
distilled water
sodium chloride
sand
23
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.

24
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
wet cloth
iodine
to cool

iodine
mixture of vapour
iodine and sand

25
heat
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

26
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.

27
Chapter 3 Separation and Purification

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

28
3.4 Separating a Liquid from
a Solution

Learning Outcome
At the end of this section, you should be able to:

• describe a method to separate and purify a

solvent from a solution.

29
3.4 Separating a Liquid from
a Solution

Obtaining the Solvent from a Solution

SOLUTION

Evaporation
Simple distillation
Crystallisation

SOLUTE SOLVENT

30
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

31
3.4 Separating a Liquid from
a Solution

Setting Up the Distillation Apparatus

Thermometer Water enters the
bulb should be condenser from the
just beside the bottom and leaves
side arm water out from the top.
leading to the Condenser must be
condenser. sloping downwards.

Boiling chips
are placed in
the flask to water in
ensure smooth
boiling.
Volatile liquids can be kept in the
liquid state by placing receiver on ice. 32
3.4 Separating a Liquid from
a Solution
Simple distillation of salt solution
4. The salt solution 2. Water boils and becomes
becomes more vapour. Thermometer measures
concentrated as temperature of the vapour.
distillation
continues. Salt will
3. Water vapour
be collected as
is cooled and
residue.
condenses into
pure liquid
1. Boiling chips (distillate).
are added to
ensure smooth
boiling. Water
vaporises, rises 5. Pure water
and enters the is collected
condenser. as distillate. 33
Chapter 3 Separation and Purification

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

34
3.5 Separating Liquids

Learning Outcome
At the end of this section, you should be able to:

• describe methods of separating and purifying

mixtures of liquids.

35
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.
separating
Example: funnel
• Oil and water oil

water

36
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.)

37
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.

38
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.

39
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.

40
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.

41
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

42
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
43
3.5 Separating Liquids

Fractional Distillation
3. Ethanol, which has a
lower boiling point than
water, reaches the
2. The water vapour upper part of the column
condenses in the and is distilled over.
fractionating column
and falls back into the
flask.

1. Ethanol vapour and

water vapour rise up
the column as the
solution is heated.
4. At this stage, the
thermometer shows a constant
temperature of 78oC, which is 44
the boiling point of ethanol.
3.5 Separating Liquids
5. In this condenser,
Fractional Distillation • hot ethanol vapour condenses
as running water cools it;
• liquid ethanol flows down the
inner tube of the condenser
and into the receiver.
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.

6. Ethanol is collected as the

distillate in the receiver.
45
3.5 Separating Liquids

Fractional Distillation

Graph showing how

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

46
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.

47
Chapter 3 Separation and Purification

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

48
3.6 Chromatography

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

• describe chromatography and interpret

chromatograms;

• explain the use of a locating agent in the

chromatography of colourless compounds.

49
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

50
3.6 Chromatography

The chromatography paper with the separated

components is called a chromatogram.

lid

glass tank

chromatogram

51
3.6 Chromatography

Separating Dyes Found in Green

Food Colouring
1. Place a spot of green food
colouring on the paper.
Chromatography
paper 2. Dip the paper into a
solvent such as ethanol or
Green food water. Ensure that the
colouring coloured spot is above the
solvent level.
Pencil line
3. The components will
Ethanol or water separate as the solvent
as solvent travels up the paper.
52
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.
53
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?

54
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 Chromatogram
after a period after a longer
of time. period of time. 55
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. 56
3.6 Chromatography

Rf value of substance is the same regardless

of distance travelled on chromatogram.

Rf = Rf =
= 0.67 = 0.67

Chromatogram Chromatogram
after a period after a longer
of time. period of time. 57
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.

58
3.6 Chromatography

Example: Comparison with ‘known’ samples

X A B C D

• 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. 59
3.6 Chromatography

Example: Comparison with ‘known’ samples

X A B C D
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
60
must not be consumed.
3.6 Chromatography

Example: Comparison with ‘known’ samples

X A B C D

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.
61
• Sample X is a mixture of three dyes.
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.

62
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.

63
Chapter 3 Separation and Purification

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

64
3.7 Determining Purity

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

• explain the importance of determining purity of

substances in our daily lives;

• identify substances and their purity, given

melting and boiling points.

65
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.
66
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

67
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.

68
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.

69
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.

70
Chapter 3 Separation and Purification

Concept Map

71
Chapter 3 Separation and Purification

The URLs are valid as at 15 November 2014.

Acknowledgements
(slide 4) AEW diamond solo white © Black Moon |
Wikimedia Commons | CC BY-SA 3.0
(http://creativecommons.org/licenses/by-sa/3.0/deed.en)
(slide 5) oranges and orange juice © Scott Bauer |
Wikimedia Commons | Public Domain
(slide 5) hot air balloon and moon © Tomascastelazo |
Wikimedia Commons | CC BY-SA 3.0
(http://creativecommons.org/licenses/by-sa/3.0/deed.en)
(slide 13) © Marshall Cavendish International (Singapore)
(slide 14) copper(II)sulfate © H. Zell | Wikimedia Commons |
CC BY-SA 3.0
(http://creativecommons.org/licenses/by-sa/3.0/deed.en)
(slide 14) Uhličitan_sodný © Ondřej Mangl | 72
Wikimedia Commons | Public Domain
Chapter 3 Separation and Purification

Acknowledgements
(slide 27) © Marshall Cavendish International (Singapore)
(slide 50) main vegetables © Malakwal City |
Wikimedia Commons | CC BY-SA 3.0
(http://creativecommons.org/licenses/by-sa/3.0/deed.en)
(slide 50) Indian dyes © Sarah and Iain | Wikimedia Commons |
CC BY 2.0
(http://creativecommons.org/licenses/by/2.0/deed.en)
(slide 50) butterscotch candies © Evan-Amos | Wikimedia Commons |
CC BY-SA 3.0
(http://creativecommons.org/licenses/by-sa/3.0/deed.en)
(slide 66) 30 mg Vyvanse capsules © Sardaukar Blackfang |
Wikimedia Commons | Public Domain
(slide 66) lush cupcakes © Tracy Ducasse | Wikimedia Commons |
CC BY 2.0
(http://creativecommons.org/licenses/by/2.0/deed.en) 73