V.

Separation Technique Page 1

Topic V. Separation Technique

Reading Integrated Chemistry Today (2nd Ed.), L.H.M Chung, Book 1A, pg 202 – 215
Assignment

Objectives 0.5 - 0.6

Methods of separation
Test of purity

Notes A. Methods of separation

Most naturally occurring materials are mixtures. e.g. sea water is a mixture of water and salt, air is a mixture of
different kinds of gas. Usually, a material must be purified before it can be used. e.g. sea water is not drinkable but
distilled water is.

Different kinds of purification technique / separation methods are required to purify different mixture. They also
provide us the opportunity to experience different kinds of laboratory technique.

In a mixture, different substances still retain their own physical properties. By using these differences in physical
properties, different components may be separated.

e.g. salt solution - salt NaCl (b.p. 1413 ºC) and water H2O (100 ºC) have very different boiling points. Therefore,
they can be separated by either evaporation, distillation or fractional distillation.

However, before you can choose an appropriate method, you must be very familiar with the properties of
individual components in the mixture.

Method of Apparatus required The difference in Applicable example

separation physical properties of
individual component
that the separation rely
on.
Filtration Essential : Filter funnel, filter paper Particle size of solid water (small particles) and
sand (big particles)
Decantation Essential : Nil Big difference in density water (low density) and
Optional : Glass rod sand (high density)
Centrifugation Essential : Centrifuge, centrifuging Small difference in density water (low density) and
tube flour (high density)
Using separating Essential : Separating funnel Density of immiscible water (higher density) and
funnel liquid peanut oil (lower density)
Evaporation Essential : Bunsen burner, evaporating Big difference in boiling water (low b.p. 100 ºC) and
dish / basin / Watch glass point salt (high m.p. 1413 ºC)
Optional : Steam bath
Distillation Essential : Bunsen burner, water Big difference in boiling water (low b.p. 100 ºC) and
condenser, thermometer point salt (high m.p. 1413 ºC)
Fractional Essential : Bunsen burner, water Small difference in boiling alcohol (low b.p. 78 ºC)
distillation condenser, thermometer, point and water (high b.p. 100
fractionating column ºC)
Sublimation Essential : Evaporating basin, funnel Sublimation point of solid iodine (low s.p. 187 ºC)
and sand (high s.p. 2230
ºC)
V. Separation Technique Page 2

Method of Apparatus required The difference in Applicable example

separation physical properties of
individual component
that the separation rely
on.
Crystallization Essential : Nil Solubility sugar (high solubility when
Optional : Steam bath hot, low solubility when
cold)
Paper Essential : Filter paper, a suitable Solubility in the solvent Colour A is more soluble in
chromatography carrying solvent water but Colour B is less
soluble in water.

Sometimes, more than one method would be used together to separate a mixture. For example, to separate a
mixture of sand and salt, dissolution, filtration and evaporation would be required to obtain the pure salt.

1. Filtration

The holes on a filter paper is so small that it can trap

any particles bigger than bacteria.

The big particles will be retained on the top of the filter

paper as residue. The solution passing through the filter
paper is called filtrate.

2. Decantation

Since sand is denser than water, upon standing, sand

will settle at the bottom of the beaker. The water can
then be decanted carefully from the beaker.

Decantation is only a kind of preliminary purification.

It cannot purify the water completely.
V. Separation Technique Page 3

3. Centrifugation

Although mud is denser than water, the difference is so small that mud does not settle down by itself upon
standing. A centrifuge creates a gravity larger than normal. By putting the mud solution into a rotating centrifuge,
the mud particles will settle down at the bottom.

4. Using separating funnel

Separating funnel is used to separate two immiscible

liquids with different density.

5. Evaporation

Since salt (1413 ºC) has a much higher boiling point than water (100 ºC), when salt solution is heated, only the
water will evaporate and the salt will be left behind.
V. Separation Technique Page 4

6. Distillation

Distillation is similar to evaporation. The only

difference is that the vapour is collected by
condensation.

The bulb of the thermometer is fixed just next to the

delivery tube to measure the temperature of the vapour
to be condensed. The condensed liquid is called
distillate.

Antibumping granules are usually added to ensure

smoother heating.

Distillation setup using Quickfit apparatus

7. Fractional distillation

A mixture of water and alcohol cannot be separated

satisfactorily by simple distillation. This is because they
have only small difference in boiling point.
(b.p. of water 100 ºC, b.p. of alcohol 78ºC)

When the mixture is heated, say 70ºC, both water and

alcohol will evaporate.

The presence of the fractionating column provides cool

surfaces to condense the less volatile component
(water) in the vapour. Eventually, only the more
volatile component (alcohol) can reach the top of the
fractionating column and pass through the condenser.
V. Separation Technique Page 5

8. Sublimation

A few solids turn directly into gas upon heating without

going through the liquid state.

This kind of solid can be separated from the mixture by

heating the mixture above the sublimation point of the
solid and providing a cool surface for it to condense.

In a mixture of iodine and sand, iodine has a

sublimation point 187ºC and sand has a sublimation
point 2230 ºC. Upon heating, only iodine will sublime.

Other examples : ammonium chloride,

iron(III) chloride.

9. Crystallization
A. Crystallization by cooling of saturated solution
The amount of solute that can be dissolved is
depending on the temperature of the solvent and the
volume of solvent.

In general, the higher the temperature and the larger

the volume of the solvent, more solute can be dissolved.

A solution which holds the maximium amount of solute

that it can hold is called saturated solution.

If a saturated solution is cooled down or evaporated, the

B. Crystallization by cooling of saturated solution
solution will not be able to hold the original amount of
solute and the solute will crystal out. Meanwhile, the
impurities in the solution remain in solution form and
will not mix with the pure crystal. Pure crystal will be
obtained.

Furthermore, the slower the rate of crystallization, the

bigger will be the crystal.

10. Paper chromatography

Paper chromatography can be

used to separate a mixture of
dyes.

Because different dyes have

different solubility in a given
solvent, they will move at
different speeds in the rising
solvent.

The chromatogram obtained

can be used to identify the
components in a mixture. DNA Chromatogram
fingerprinting is a technique
using chromatography.
V. Separation Technique Page 6

B. Testing of purity

1. Determination of melting point

A pure substance has a sharp melting point but a mixture

does not melts sharply. According to this behaviour, the
purity of a substance can be tested. Furthermore, the
presence of impurity will also lower the melting point of the
mixture.

Example 1
Pure ice melts at 0ºC but a mixture of salt and ice melts at
about -20ºC to 25ºC . This phenomenon is called
depression of melting point by an impurity.

Example 2
Pure octadecan-1-ol melts at 58ºC and pure napth-1-ol
melts at 120ºC.
Experimentally, pure octadecan-1-ol will start to melts at
57.5ºC and when the temperature reaches 58.5ºC, all solid
will be melted.
If it is mixed with a little napth-1-ol, the mixture will start
to melts at 50ºC and will melts completely at 55ºC.

By knowing whether a substance melts sharply or not, the purity of the substance can be tested. A pure substance
only has a very narrow melting range.

2. Determination of boiling point

Unlike melting point determination, a sharp boiling

point may not represent a pure sample. (This will be
discussed in A-Level).

However, boiling point can be used as a kind of positive

confirmation of the identity of an unknown sample.

For example, if the boiling point of the liquid is 103ºC,

the liquid must not be water.

Glossary mixture physical properties filtration residue filtrate decantation centrifugation

centrifuge centrifuging tube separating funnel immiscible evaporation
evaporating basin distillation antibumping granules water condenser Quickfit apparatus
fractional distillation volatile fractionating column sublimation sublimation point
ammonium chloride iron(III) chloride solvent extraction saturated solution solubility
crystallization paper chromatography chromatograph adsorption activated charcoal
V. Separation Technique Page 7

Past Paper
Questions

90 30
A 30 Which of the following methods can be used to obtain
sodium chloride from a solid mixture containing sodium
chloride and ammonium chloride?
A. heating
B. adding water and filtering
C. adding sodium hydroxide solution and filtering
D. adding silver nitrate solution and filtering

93 42
B 42

Which of the following solids can be purified using the

above set-up ?
A. potassium iodide
B. ammonium chloride
C. lead(II) bromide
D. sodium hydrogencarbonate

98 26
B 26 Some physical properties of a compound X are listed below:
melting point : 82°C
boiling point : 221 °C
solubility in water: soluble
Which of the following is the most appropriate method to
obtain X from a solution of X in water ?
A. decantation
B. crystallization
C. fractional distillation
D. paper chromatography