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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 le& to cool; crystals are
formed.
The crystals are removed by ltration. To purify
the crystals, they can then be washed with cold
distilled water and dried between lter 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
Egs. common salt and sand; Use
water as solvent

naphthalene and sand


Use methylated
spirits as solvent

Separating a mixture of solids


Basic Steps :
Dissolution

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 lings 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


Crystallisation!
Evaporation
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.
The vapour rises
up the flask

3. the condenser is
cold, so the vapour
thermometer condenses to liquid
water.

flask
sea water

condenser

Boiling chips
1. Solution is
heated, causing the
solvent to

distillate

4. Pure water
drips into the
beaker. It is
distilled water.

Simple Distillation
thermometer
Water out

flask
sea water

condenser

Boiling chips
To maintain even
boiling, with not
too much bumping

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
This out
is to make sure the coldest partwater
of thein

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
sea water

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
sea water

condenser

Boiling chips
distillate

Separating miscible liquids -


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

Separating miscible liquids -


Fractional distillation
Fractionating
column

flask
Boiling chips

thermometer
Water out
condenser

Water in
mixture of ethanol
and water

distillate

Separating miscible liquids -


Fractional distillation
2. The fractionating
column is packed with
glass beads to increase
its surface area.
Vaporisation followed by
condensation takes place
many times as the
vapour is swept
upwards.

3. Eventually, the
liquid with the
lower boiling point
reaches the top and
distils over.

1. When heated, the


liquid with the lower
boiling point will
vaporize more readily.

Separating miscible liquids -


Fractional distillation
4. The temperature
stays constant at
78C. When all the
ethanol has distilled
over, the
temperature reading
rises above 78C.
At 100C, water
starts to distil over.

5. The receiver is
changed to collect each
distillate separately.

Separating miscible liquids -


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

100C!
78C!

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
beads!

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
beads!

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


Mixtures!
solid + liquid!

Filtration!

Residue!
(solid)!

Filtrate!
(liquid)!

liquid + liquid!
solid + solid!

The main points so far


Mixtures!
solid + liquid!

Simple
Distillation!

Residue!
(solid/
solute)!

Distillate!
(liquid/
solvent)!

liquid + liquid!
solid + solid!

The main points so far


Mixtures!
YES!

solid + solution!
Filtration!

Residue!
(insoluble
solid)!

Add suitable
solvent!

Filtrate!
(solution)!

liquid + liquid!
solid + solid!
Difference
in
solubility?!

Crystallisation!

Crystals!
(soluble
solid)!

The main points so far


Mixtures!

solid + solution!
Filtration!

liquid + liquid!
solid + solid!

YES!
Add suitable
solvent!

Difference
in
solubility?!

NO!

Sublimation!

Crystallisation!
Other physical
difference?!

Egs.!

Using
magnet!

The main points so far


Mixtures!

Fractional
distillation!

liquid + liquid!
miscible
liquids
(different
boiling
pts.)!

immiscible
liquids!

Separating
funnel!

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