CHAPTER 2

PURIFICATION OF SUBSTANCES
LEARNING OUTCOMES
After completing this chapter, you should be able to
• EXPLAIN, WITH EXAMPLES, WHY PURE SUBSTANCES ARE NEEDED
• DESCRIBE METHODS OF SEPARATION AND PURIFICATION FOR THE
COMPONENTS OF SOLID-SOLID, SOLID-LIQUID AND LIQUID-LIQUID (MISCIBLE)
MIXTURES

• DESCRIBE TECHNIQUES FOR SEPARATION AND PURIFICATION INCLUDING USE

OF A SUITABLE SOLVENT, FILTRATION, CRYSTALLISATION OR EVAPORATION,
SIMPLE DISTILLATION, FRACTIONAL DISTILLATION AND PAPER
CHROMATOGRAPHY
LEARNING OUTCOMES

• DESCRIBE PAPER CHROMATOGRAPHY AND INTEPRET CHROMATOGRAMS

• DEDUCE FROM THE GIVEN MELTING POINT AND BOILING POINT, THE
IDENTITIES OF SUBSTANCES AND THEIR PURITY
WHAT IS A PURE SUBSTANCE?

• A PURE SUBSTANCE IS A SINGLE SUBSTANCE NOT MIXED WITH ANYTHING ELSE.

• EXAMPLES ARE WHITE SUGAR AND COPPER(II) SULFATE CRYSTALS.
• A MIXTURE CONSISTS OF TWO OR MORE SUBSTANCES THAT ARE NOT
CHEMICALLY COMBINED TOGETHER.

• EXAMPLES ARE SEAWATER AND MILK.

SKILLS PRACTICE
 Answers
 1. (a) pure gold coins, pure silver jewellery, platinum
wedding rings, aluminium foil
(b) milk, flavoured drinks, air, tap water
 2. oxygen, carbon dioxide, nitrogen, noble gases such as
helium, argon, neon)
 3. Chemical reactions are specific. If the chemicals used are
not pure, we will not know how the reaction actually
proceeded, and whether the reactant or the contaminant was
involved in the reaction. Pure chemicals also allow reactions
to give a better yield.
HOW ARE PURE SUBSTANCES
OBTAINED?

• MIXTURES CAN BE EASILY SEPARATED INTO PURE

SUBSTANCES BY PURIFICATION.

• IT IS DONE BY USING PHYSICAL METHODS WITHOUT

CHEMICAL REACTIONS.
DECANTING
Decanting separates an insoluble solid from a liquid
by pouring off the liquid from the container.
FILTRATION
Filtration is used to separate an insoluble solid from a
liquid.
USES OF FILTRATION
• SMALL FILTER SYSTEMS ARE
USED IN THE HOME TO
FILTER TAP WATER.
• AT WATER PURIFICATION
PLANTS, LARGE FILTERS ARE
USED TO REMOVE SAND AND
MUD FROM WATER.
EVAPORATION

• EVAPORATION IS USED TO SEPARATE

DISSOLVED SOLIDS FROM A
SOLUTION.

• A MIXTURE OF TWO SOLIDS CAN BE

SEPARATED BY COMBINING
FILTRATION AND EVAPORATION IF ONE
SOLID IS SOLUBLE IN A SOLVENT AND
THE OTHER IS INSOLUBLE.
PROBLEMS WITH EVAPORATION

• SOME SOLIDS DECOMPOSE WHEN HEATED.

• WITH EVAPORATION, ANY SOLUBLE IMPURITIES WILL

ALSO BE PRESENT IN THE SOLID RESIDUE.
CRYSTALLISATION
WHY ARE CRYSTALS FORMED?
• CRYSTALLISATION OCCURS BECAUSE THE SOLUBILITY OF
MOST SOLUTES DECREASES AS THE TEMPERATURE
DECREASES.
• AS A HOT SOLUTION COOLS, IT EVENTUALLY BECOMES
SATURATED AND CAN HOLD NO MORE SOLUTE.
• THE EXTRA SOLUTE THAT CANNOT BE DISSOLVED
SEPARATES AS PURE CRYSTALS.
CRYSTALLISATION WITHOUT A
SOLVENT
• SOME SOLIDS CAN BE PURIFIED
BY MELTING THEM.
• THE HOT LIQUID IS THEN COOLED
SLOWLY.
• PURE CRYSTALS FORM AS THE
LIQUID FREEZES.
SIMPLE DISTILLATION
Simple distillation
separates a pure liquid
from a solution.
The distillation of
seawater, known as
desalination, is one way
that pure water is
obtained.
 FRACTIONAL DISTILLATION
Fractional distillation
separates mixtures of
miscible liquids with
widely differing boiling
points.
Miscible: forming a
homogeneous mixture
when added together.
TEMPERATURE CHANGES DURING
FRACTIONAL DISTILLATION
The graph below shows how the temperature changes
during the fractional distillation of a mixture of
ethanol and water.
USES OF FRACTIONAL DISTILLATION

 Three uses of fractional distillation are:

 To separate pure oxygen and pure nitrogen from
liquid air

 To separate substances in petroleum into fractions

 To produce ethanol which is used in alcoholic

drinks
USE OF A SEPARATING FUNNEL

Liquids that do not mix with

each other are said to be
immiscible.

Two immiscible liquids, such

as oil and water, can be
separated by using a separating
funnel.
USE OF A SEPARATING FUNNEL
 To separate the oil and water, we use the following steps:
 The mixture is placed in a separating funnel and allowed to
stand.
 The oil and water form two separate layers, with the less
dense oil being on top.
 The stopper is removed and the tap opened.
 The bottom layer of water is run off and collected in a
container placed under the tap.
 Another container is placed below the funnel.
 The tap is opened again and the top layer of oil is collected
in the container.
SKILLS PRACTICE
 Answers
 1. The salt particles are small enough to go through the pores in the filter paper.
 2. The small amount of impurity is insufficient to saturate the solution and form
crystals. This is the basis for the use of crystallisation for separation. However,
complete separation will only occur if the impurities are present in small amounts.
 3. (a) Similarities: Both separate a liquid from a mixture. In both, liquids boil and
vapours condense after leaving the flask.

(b) Differences: In simple distillation, one liquid is separated from a solid-liquid

mixture. In fractional distillation, two or more miscible liquids with widely
different boiling points are separated.
 4. Solid-solid: Sublimation, paper chromatography, filtration plus crystallisation
Solid-liquid: Decantation, filtration, crystallisation, simple distillation
Liquid-liquid (miscible): Fractional distillation
Liquid-liquid (immiscible): Using a separating funnel
 Answers
 5. Possible answers are:
Filtration: Filtration of water at a water treatment plant
Crystallisation: Obtaining salt from seawater
Simple distillation: Preparation of distilled water
Fractional distillation: Separation of substances in petroleum

 6. Neon will distil first as it has the lowest boiling point. Krypton will distil last as it
has the highest boiling point.
WHAT IS CHROMATOGRAPHY?
• CHROMATOGRAPHY IS A METHOD OF SEPARATING AND
IDENTIFYING MIXTURES.

• ONE TYPE OF CHROMATOGRAPHY IS PAPER CHROMATOGRAPHY

AND IT IS USED TO SEPARATE BOTH COLOURED AND COLOURLESS
MIXTURES.

• A BIG ADVANTAGE OF PAPER CHROMATOGRAPHY IS THAT IT CAN BE

USED WITH JUST VERY SMALL AMOUNTS OF MIXTURES.
USES OF CHROMATOGRAPHY
SEPARATING MIXTURES OF COLOURED
SUBSTANCES
IDENTIFYING MIXTURES OF COLOURED
SUBSTANCES
IDENTIFYING MIXTURES OF COLOURED
SUBSTANCES
 The results from this chromatogram show that:
 The colour in the sweet is made up of three dyes.
Two of the dyes are the known red and green dyes as
there are spots on the paper of the same colour and at
the same distance above the pencil line.
The sweet contains one other dye that differs from the
three known dyes and so cannot be identified.
 SEPARATING AND IDENTIFYING
MIXTURES OF COLOURLESS SUBSTANCES

• CHROMATOGRAPHY CAN BE USED TO SEPARATE AND

IDENTIFY COLOURLESS SUBSTANCES.
• THE CHROMATOGRAM IS SPRAYED WITH A LOCATING AGENT
TO SHOW WHERE THE SUBSTANCES ARE ON THE PAPER.
• A LOCATING AGENT IS A SUBSTANCE THAT REACTS WITH
THE SUBSTANCES ON THE PAPER TO PRODUCE A COLOURED
PRODUCT.
 SEPARATING AND IDENTIFYING
MIXTURES OF COLOURLESS SUBSTANCES
• AN EXAMPLE OF SEPARATING COLOURLESS SUBSTANCES IS IN
THE IDENTIFICATION OF SUGARS IN FRUIT JUICES.
• THE SAME METHOD IS USED EXCEPT THAT THIS TIME, A
DIFFERENT SOLVENT IS USED.
• AT THE END, THE CHROMATOGRAM IS SPRAYED WITH SILVER
NITRATE SOLUTION FOLLOWED BY DILUTE SODIUM HYDROXIDE.
• THE CHEMICALS MAKE THE SUGARS APPEAR AS BROWN SPOTS.
SEPARATING AND IDENTIFYING
MIXTURES OF COLOURLESS
SUBSTANCES
• A CHROMATOGRAM OF SUGARS IN FRUIT JUICE IS SHOWN BELOW:
 SEPARATING AND IDENTIFYING
MIXTURES OF COLOURLESS SUBSTANCES
 The results of the experiment show that:

 Fruit juice contains three different sugars.

 Two of the sugars are sucrose and glucose.

The fruit juice contains one other sugar different

from the three known sugars.
 RF VALUES
Distance moved by the substance
= Rf
Distance moved by the solvent

• FORANY SUBSTANCE ON A CHROMATOGRAM,

The distance is measured from the start line.

x
= Rf
y
 RF VALUES
• THE R VALUE FOR THE UNKNOWN SUGAR CAN BE
F

CALCULATED AS FOLLOWS:
 RF VALUES
• THE SUGAR IS THEN IDENTIFIED FROM THE RF VALUES FOR DIFFERENT SUGARS THAT HAVE ALREADY BEEN
CALCULATED.

• THE RF VALUES DEPEND ON THE SOLVENT AND THE TEMPERATURE.

• FROM THE TABLE, WHAT IS THE UNKNOWN SUGAR IDENTIFIED AS?

SKILLS PRACTICE
 Answers
(a) It is needed because sugars are colourless and
cannot be seen on the paper unless coloured with a
locating agent.
(b) No sucrose remained as there is no ‘spot’ for
sucrose on the paper.
(c) Suctose rose reacts to produce glucose and fructose
as their spots have Rf values of about 0.10 and 0.56,
which are close to those for the sugars.
 HOW DO WE CHECK THE PURITY OF
SUBSTANCES?
• A PURE SUBSTANCE HAS FIXED MELTING AND BOILING
POINTS.

• THE MELTING AND BOILING POINTS OF PURE

SUBSTANCES ARE UNIQUE, SO A PURE SUBSTANCE CAN
BE IDENTIFIED FROM ITS MELTING AND BOILING POINTS.
HOW DO IMPURITIES AFFECT MELTING
POINT?

 Impurities lower the melting point.

The greater the amount of impurity, the lower the

melting point.

The substance melts over a range of temperatures.

HOW DO IMPURITIES AFFECT BOILING
POINT?

 Impurities make the boiling point higher.

The greater the amount of impurity, the higher the

boiling point.

The liquid boils over a range of temperatures.

SKILLS PRACTICE