Methods of Purification

(a)Describe methods of separation for the components of the

following types of mistures:
(i)solid-solid
(ii)solid-liquid
(iii)liquid-liquid(miscible)
Techniques to be covered for separations and purification include:
(i)Use of a suitable solvent, filtration and crystallization or
evaporation
(ii)Distillation and fractional distillation
(iii)Paper chromatography
(b)

Pure Substances &

Mixtures
A pure substance contains only one
type of substance, and is not
mixed with any other substance.
Are the following pure substances or
mixtures?
Clean tap water mixture
100% orange juice mixture
Distilled water
Pure
substance

Methods of Purification
Some terms :

Solute - the solid that dissolves

Solvent - the liquid that does the dissolving
Solution - solid + solvent
Residue - the insoluble solid trapped in the
filter paper
Filtrate - the liquid that passes through the
filter paper
Sublimate - the condensed solid produced
during sublimation

Methods of Purification
The particular method used for
separating any given mixture
depends on the nature (eg.
solubility, physical state) of its
constituents.

Filtration
Used to separate a solid from a
liquid in which the solid is
insoluble
mixture of
solid and
liquid

residue

filter funnel
filter paper

filtrate

Principle of Filtration
The separation works only if the particles
concerned are of different sizes, such as larger
particles of an insoluble solid and smaller
particles of a liquid or solution.

Principle of Filtration
The filter material acts as a sieve which
allows the smaller particles to pass
through and keeps the bigger particles
behind.

Principle of Filtration
Can a mixture of common salt and
water be separated by filtration?
Why?

Filtration - large scale use

Sand filters used in water treatment
plants to remove solid impurities
Dissolved substances and bacteria will
not be removed

Decanting
Separates an insoluble solid from a liquid
liquid is carefully poured away from the
solid which is usually heavier and settles
at the bottom of the container.

Evaporation (Heating )to

Dryness
used to recover a soluble solid from its
solution
Only for solids that will NOT
decompose on heating.
Eg. sodium chloride (common salt) from
salt solution

Crystallisation
used to recover a soluble solid from its solution
for solids that decompose on heating
Eg. Copper(II) sulphate and most other salts
Steps :
The solution is heated (evaporated) to
saturation point OR heated to remove most of
the solvent
The saturated solution is left to cool; crystals
are formed.
The crystals are removed by filtration. To purify
the crystals, they can then be washed with cold
distilled water and dried between filter papers.

Crystallisation - the Principle

behind
Substances are usually more soluble in hot
water than cold water eg. more copper(II)
sulphate will dissolve in water at 80C than at
30 C.
When the hot saturated solution is cooled, the
cooled solution is unable to hold as much
solute as when it was hot. The extra solute
that cannot remain dissolved appears as
crystals.

Solubility & Crystallisation

Solubility data for NH4Cl in grams/100 mL H2O
30oC- 41.4 g
50oC- 50.4 g
70oC- 60.2 g
90oC- 71.3 g
If the water was heated to 90C, how much of
the solute will be able to dissolve?
If this hot solution is then cooled to 30 C, how
much solute can the water contain now?
Hence what is the mass of crystals you would
expect to obtain?

Separating a mixture of
solids
Method used depends on the nature of the
solids :(1) If the mixture of solids behave differently in a
particular solvent , that is, one component is
soluble in it while the other is insoluble
carefully choose a solvent that will dissolve only
one of the solids
Use water as solvent

Egs. common salt and sand;

naphthalene and sandUse methylated

spirits as solvent

Separating a mixture of
solids
Basic Steps :
Dissolutio
n

Filtration

Evaporation
to dryness

OR
Crystallisation

Separating a mixture of
solids
(2) Sublimation
used when one of the
solid sublimes
Eg.
mixture of iodine +
copper;
mixture of ammonium
chloride +
sodium chloride

Separating a mixture of
solids
(3) Other methods :
make use of the special properties
of the substance
Eg. mixture of iron filings and sulphur .
use a magnet
Bring a magnet to the mixture.
The iron filings will be attracted to the
magnet while the sulphur will be left
behind.

Separating the Solvent from the

Solution
Crystallisatio
n
Evaporatio
n to
dryness

solute

Distillation

solvent

solution

Simple Distillation
Some Terms Used :
Distillate - the liquid that distils
over
Miscible liquids - liquids that mix
completely to form a single layer
Immiscible liquids - liquids that do
not mix
A solvent can be separated from a
solution and collected by simple
distillation.

Principle of Distillation
A liquid boils and turns into vapour at its
boiling point.
When the vapour is condensed, the
(pure) liquid is obtained again.

Simple Distillation
2...vapourise.
Thevapourrises
uptheflask

3.thecondenseris
cold,sothevapour
thermometer condensestoliquid
water.

flask
seawater

condenser

Boiling chips
1.Solutionis
heated,causingthe
solventto

distillate

4.Purewater
dripsintothe
beaker.Itis
distilled
water.

Simple Distillation
thermometer
Water out

flask
seawater
Boiling chips
Tomaintaineven
boiling,withnot
toomuchbumping

condenser

Water in

Liebig Condenser
Vapour enters

Condensed vapour in liquid

form (distillate) leaves

Direction of water flow

Water
out

Cold
water in

Water flows in anti-current to the flow of vapour.

Liebig Condenser
Vapour enters

Condensed vapour in liquid

form (distillate) leaves

Direction of water flow

Water
Cold
Thisout
is to make sure the coldest part
of the
water
in

condenser is just before the vapour escapes.

Simple Distillation
Simple

distillation can be used to obtain

water from salt solution
water from copper(II) sulphate solution
ether from a solution of sugar in ether

Note :
The liquid that distils over is called the
distillate .
The solid that remains in the flask is called the
residue .

Simple Distillation
Qns. : Where is the thermometer
placed? What is the reason for this?
thermometer
flask
seawater

condenser

Boiling chips
distillate

Simple Distillation
Thermometer placed at the side arm of the flask so
that it records the temperature of the vapour as it
enters the condenser.

thermometer
flask
seawater

condenser

Boiling chips
distillate

Separating miscible liquids Fractional distillation

miscible liquids can only be
separated by fractional distillation
if they have different boiling
points .
Eg. mixture of ethanol and water.

Separating miscible liquids Fractional distillation

Fractionating
column

flask
Boiling chips

thermometer
Water out
condenser

Water in
mixtureofethanol
andwater

distillate

Separating miscible liquids Fractional distillation

2.Thefractionating
columnispackedwith
glassbeadstoincrease
itssurfacearea.
Vaporisationfollowedby
condensationtakesplace
manytimesasthe
vapourisswept
upwards.

3.Eventually,the
liquidwiththe
lowerboilingpoint
reachesthetopand
distilsover.

1.Whenheated,the
liquidwiththelower
boilingpointwill
vaporizemorereadily.

Separating miscible liquids Fractional distillation

4.Thetemperature
staysconstantat
78C.Whenallthe
ethanolhasdistilled
over,the
temperaturereading
risesabove78C.
At100C,water
startstodistilover.

5.Thereceiveris
changedtocollecteach
distillateseparately.

Separating miscible liquids Fractional distillation

Sketch a graph of temperature versus time
to show the changes in temperature
readings throughout the distillation.
temperature

100
C
78
C

time

Separating miscible liquids Fractional distillation

Note :
The glass beads in the
fractionating column
provides a large surface
area so that condensation
occurs more readily.
The liquid with the lower
boiling point distils over
first, followed by the liquid
with the next higher boiling
point.

glass
bead
s

Separating miscible liquids Fractional distillation

Note :
If the liquids in the mixture
have the same boiling
point, fractional distillation
is not possible.
If the difference in boiling
point is great, fractional
distillation occurs readily.

glass
bead
s

Fractional distillation applications

Fractional distillation can be used
to separate : nitrogen and oxygen from liquid air
the components of crude oil
ethanol from fermented liquor

Fractional distillation of crude

oil

Separating immiscible
liquids
A separating funnel
can be used to separate
two immiscible liquids.
Eg. water and petrol.
This method can be
used to separate :
a mixture of petrol
and water
engine oil and water

The main points so far

Mixture
s
solid +
(Solid INSOLUBLE
in
liquid
liquid)

Filtration

Residue
(solid)

Filtrate
(liquid)

liquid + liquid
solid +
solid

The main points so far

Mixture
s
solid +
(Solid
SOLUBLE
liquid
in liquid)

Simple
Distillation

Residue
(solid/
solute)

Distillate
(liquid/
solvent)

liquid + liquid
solid +
solid

The main points so far

Mixture
s
solid +
solution
Filtration

Residue
(insoluble
solid)

Filtrate
(solution)

YES
Add
suitable
solvent

liquid + liquid
solid +
solid
Difference
in
solubility?

Crystallisatio
n

Crystals
(soluble
solid)

The main points so far

Mixture
s
solid +
solution
Filtration
Crystallisatio
n

YES
Add
suitable
solvent

liquid + liquid
solid +
solid
Difference
in
solubility?

NO
Other physical
difference?

Sublimatio
n
Egs.

Using
magnet

The main points so far

Mixture
s
Fractional
distillation

liquid + liquid
miscible
liquids
(different
boiling
pts.)

immiscible
liquids

Separating
funnel