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Separation
& Purification
Secondary 3 Science (Chemistry) (5105/5107)

OBTAINING PURE SUBSTANCES FROM MIXTURES …..…………………..


…………… 2

SEPARATING A SOLID FROM A LIQUID


FILTRATION …..…………………………………………………...
………………… 3
EVAPORATION TO DRYNESS …..……………………...………….
……………… 4
CRYSTALLISATION …..………………………………………………………..
…… 5

SEPARATING SOLIDS
USING A SUITABLE SOLVENT …..
………………………………………………… 6

SEPARATING A LIQUID FROM A SOLUTION


SIMPLE DISTILLATION …..……………………………………….
………………… 8

SEPARATING LIQUIDS
FRACTIONAL DISTILLATION …..……………………………..
…………………… 9

CHROMATOGRAPHY …..………………………………………………..………………
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DETERMINING PURITY …..……………………………………………..
………………… 18

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OBTAINING PURE SUBSTANCES FROM MIXTURES

A pure substance is made up of one single element or compound. It is not mixed with any other
substance.

Most materials that occur naturally are mixtures and not pure substances. For example, seawater is a
mixture. In order to obtain water from sea water, we need to remove impurities like salt.

There are several methods to remove impurities or separate mixtures into pure substances. To decide
which method to use, we need to consider the properties of each substance in the mixture.

In the following sections, you will learn how to separate:


 a solid from a liquid – filtration, evaporation to dryness, crystallisation
 solids – using a suitable solvent
 a liquid from solution – simple distillation
 liquids – fractional distillation

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SEPARATING A SOLID FROM A LIQUID
(I) FILTRATION
Filtration is a process of separating an insoluble solid from a liquid.

A filter funnel and a filter paper are usually used. The filter paper acts as a sieve due to the pores of
the filter paper.

e.g.
 sand, clay, dust particles from water
 chalk powder and water (suspension)
 coffee grounds separated from coffee
 tea leaves from tea

(II) EVAPORATION TO DRYNESS


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This is a process of obtaining a soluble solid from a solution by heating the solution until e.g. all the
water has boiled off.

The solid obtained by evaporation to dryness is not always pure. When all the water has been
removed, any soluble impurities will be left together with the solid.

Not all soluble substances can be obtained by evaporation to dryness. Many substances
decompose (break down to form simpler substances) when they are heated strongly.

E.g. sugar decomposes to water and carbon when heated strongly

E.g. copper(II) sulfate crystals, give off water to become powders when heated.

For such substances, evaporation to dryness is not a good method of separation and purification.

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(III) CRYSTALLISATION

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

In crystallisation, water is removed by heating the solution. Heating is stopped at the stage when a hot
saturated solution is formed. If the resulting solution is allowed to cool to room temperature, the
solids will form as pure crystals.

Procedure:
 Heat the solution until it is saturated.
 Allow the hot saturated solution to cool for to crystallise.
 Filter off the crystals.
 Wash the crystals with a little cold distilled water. Dry the crystals with filter paper.

Saturated solution: a solution that contains the maximum amount of dissolved solute at a given
temperature. No more solute can be dissolved in the solution.

1 What method can be used to separate salt from seawater?

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A dissolving B filtration
C evaporation to dryness D crystallisation ( )

2 A mixture can be separated into its components using suitable separation methods. Name a suitable
method that can be used to obtain the following substances.

(a) To obtain copper(II) sulfate crystals from a dilute solution of copper(II) sulfate

crystallisation

(b) To obtain solid sodium chloride from a sodium chloride solution

evaporation to dryness

(c) To collect sand from a mixture of sand and seawater

filtration

SEPARATING SOLIDS
USING A SUITABLE SOLVENT
Solvent: the liquid that dissolves the solute.
Solute: the substances that is dissolved

E.g. sugar solution: solute = sugar, solvent = water

Different solids dissolve in different solvents. Some common solvents are water and ethanol.
 Ionic compounds are usually soluble in water and covalent substances are usually soluble in
organic substances such as ethanol.

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.)

E.g. What are the steps needed to separate a mixture of salt and sand?

1 The table below shows the information about three different substances, A, B and C.

substance heat stable solubility in water


Solid A yes no
Solid B yes no
Solid C no yes

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The following operations could be carried out to separate substance C from a mixture of these three
substances.

1 Filtration
2 Dissolving in water
3 Crystallisation

What would be the correct order of the operation to obtain substance C from the mixture?

A 2, 1, 3 B 1, 2, 3
C 3, 2, 1 D 2, 3, 1 ( )

2 Two substances, A and B, are both fine powders, which are mixed together. A is a white solid that is
insoluble in water and B is a blue solid that is soluble in water. Water is added to the mixture and filtered.

What would be obtained as the residue and filtrate?

residue filtrate
A blue solution white solid
B colourless solution blue solid
C blue solid colourless solution
D white solid blue solution
( )

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SEPARATING A LIQUID FROM A SOLUTION
SIMPLE DISTILLATION
What method can we use if we need to collect the solvent instead?

Simple distillation is used to separate a pure solvent (liquid) from a solution. Distillation involves the
process of boiling a liquid and condensing the vapour.
E.g. Extraction of water from:
• sea water
• salt (sodium chloride) solution
• sugar solution

When setting up the distillation apparatus, note the following procedures:


1 Thermometer: the bulb of the thermometer should be placed beside the side arm of the
distillation flask. It should not be dipped into the solution.
 Ensures that the thermometer measures the boiling point of the substance that is being
distilled.

2 The condenser consists of two tubes: an inner tube and an outer water jacket and should
slope downwards.
 Ensures that the liquid runs downwards into the receiver.

3 Cold running water is allowed to enter the water jacket from the bottom of the condenser
and leave from the top.
 Ensures that the water jacket is completely filled to provide a more efficient cooling
system and maintains a temperature gradient for condensation to take place.
 To allow vapours to condense into a liquid

SEPARATING LIQUIDS

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The method used for separating a mixture of two (or more) liquids will depend on whether the liquids
are miscible or immiscible.

Liquids that dissolve in each other completely to form a solution are described as miscible. E.g.
ethanol and water

Liquids that do not dissolve in each other are described as immiscible. E.g. oil and water

FRACTIONAL DISTILLATION
This method can be used to separate a mixture of miscible liquids with different boiling points.

A fractionating column is attached to the round-bottomed flask and


the condenser for fractional distillation. Glass beads/plates/spiral in the
fractionating column provide a large surface area for vapour(s) to
condense on.

During fractional distillation:


 the liquid with the lowest boiling point will distill over first;
 the vapours of liquids with higher boiling points condense along
the fractionating column and fall back into the round bottom flask.

How does the temperature change as a solution of ethanol and water undergoes fractional
distillation?

Graph showing how temperature changes as a solution of ethanol and water is fractionally distilled.

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The temperature of the mixture increases as it is heated until it reaches 78 oC. At 78 oC, ethanol distills
over. The temperature remains constant until all the ethanol has distilled out of the round-bottomed
flask.

The temperature then increases until 100 oC. At this temperature, water distills over. The temperature
remains unchanged as water is being distilled.

What are the industrial application of fractional distillation?

 the various components of crude oil such as petrol, kerosene, diesel in oil refineries.
 nitrogen, oxygen and argon in liquid air.

1 The diagram shows part of the apparatus set up for distillation.

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xc

Where does the hot vapour enter and cooled distillate leave the apparatus?

hot vapour cooled distillate


A W Y
B X Y
C Y X
D Z X
( )

2 Which is the correct sequence of processes involved in simple distillation?

A condensation, then boiling B crystallisation, then condensation


C boiling, then condensation D filtration, then boiling ( )

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3 The diagram below shows the apparatus used to obtain pure water from seawater.

thermometer

S
boiling
boiling sea
chips
chips water

heat
T

(a) What is the name of the separation technique shown in the diagram?

 simple distillation

(b) Describe what happens to the water in apparatus S.

 water boils and turns into a vapour

(c) Name apparatus X and state its function.

X is a condenser and its function is to allow vapours to condense into a liquid by


(providing a cool surface).

(d) On the diagram above, label the boxes with ‘water in’ and ‘water out’ on
apparatus X.

(e) State the temperature reading on the thermometer when water starts to be collected in
apparatus T.

100 oC

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4 The following apparatus was set up to separate a mixture of ethanol and water. The boiling points
of ethanol and water are 78 °C and 100 °C respectively.

thermometer

condenser
glass beads

mixture of R
water and
ethanol

heat
(a) Name the separation technique shown in the diagram.

 fractional distillation

(b) Which liquid will be distilled first? Explain your answer.

Ethanol will be distilled first as it is the liquid of a lower boiling point.

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CHROMATOGRAPHY
Chromatography is the method of separating two or more components that dissolve in the same
solvent (different solubilities).

E.g. 1 Draw a start line with a pencil at about 1 cm from


the bottom of a strip of filter paper or chromatography
paper.

2 Put a drop of the green food colouring on the pencil


line. Allow the drop to dry.

3 Dip the paper into a glass tank containing the solvent.


The solvent is soaked up by the paper will dissolves
start line the dye.

4 Leave the apparatus to stand for a while. Ethanol will


travel up the paper carrying the dyes along. The more
soluble the dye is in ethanol, the further it will move
up the paper.

Why is the start line drawn with a pencil?


 Pencil ‘lead’ is insoluble in many solvents and will not dissolve and interfere with the
results of chromatography.

Why must the start line be placed above the solvent level?
 To prevent sample spot(s) from dissolving in the solvent.

https://www.youtube.com/watch?v=iPpy4khqtks

https://www.youtube.com/watch?v=J05F1fdZ-Zg

How do we interpret the result of paper chromatography?


Separation of a substance into its different components depends on the relative solubility of the
component.

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 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.

Components M and N have


A pure substance is made up different solubility in the same
of only one dye - one single solvent.
spot on the chromatogram.  Component M is more
soluble in the solvent.

The dye is a mixture of three


Samples X and Y are identical.
dyes.

Too much sample is placed on


Samples X and Y are not
the starting line.
identical.
 Samples X and Y contain
A small and concentrated
2 identical component.
sample should be used.

The sample is insoluble in the


Sample X is made by the
solvent.
combination of samples Y and
 A change in solvent is
Z.
required

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How can a banned substance present in food colouring be identified?
Each dye is identified by comparing
 Its position in the chromatogram with that of a known dye on the same chromatogram;

Chemists can then check against a database of banned dyes to see if the dyes are permitted for use in
food.

Given a sample, chromatography can be used to:


 separate the components in a sample (dyes in ink, pigments in plants and amino acids from
proteins);
 identify the components present in a sample (traces of banned substances in food);
 identify substances (such as poisons, pesticides and drugs);
 determine whether a sample is pure.

1 The presence of food colourings W, X, Y and Z were tested on food products labelled P, Q, R
and S.

Which colouring was found in most of the food products?

A W B X
C Y D Z ( )

2 The chromatogram below shows the dyes present in four different soft drinks, P, Q, R and S, and
in two dyes X and Y. Both dyes X and Y are harmful.

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Which of the soft drinks contains a harmful dye?

A P and Q B R and S
C Q and S D P and R ( )

3 A sample of food colouring is made up of blue and yellow dyes. The dyes were separated by
chromatography using the apparatus shown.

rod
chromatography paper

spot of food colouring


glass tank

starting line
solvent
(a) Suggest a suitable solvent for the experiment.

water

(b)Why must the start line be drawn in pencil and not in ink?

Pencil ‘lead’ is insoluble in many solvents and will not dissolve

(c) Why must the start line, on which the spot of food colouring was placed, be above the level of
the solvent?

To prevent sample spot(s) from dissolving in the solvent.


DETERMINING PURITY
Importance of Purity

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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.

In the production of silicon chips (99.999 999% pure) for the


electronic industry, small amounts of impurities will make a
component in an electronic device less efficient.

A substance which melts / boils over a range of temperature will not be a pure substance
(mixture).
 e.g. petrol boils between 35 oC --- 75 oC

A pure substance (element/compound) have a fixed melting and boiling point.


 e.g. gold melts at 1064 oC

Methods to determine purity

 Checking for exact and constant (or fixed) melting point of a solid
 A pure solid will melt completely at one temperature.

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 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.

 Checking the exact and constant (or fixed) boiling point of a liquid
 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.

 Performing chromatography

1 A student makes some crystals.

How does the student test for the purity of the crystals?

A the melting point of the crystals B the shape of the crystals


C the size of the crystals D the solubility of the crystals in water
( )

2 Which of the following is most likely a pure compound?

A Black substance that produces three fractions when distilled.


B Colourless crystals that all melt at 58 ºC.
C Ice that melts over a range from -10 ºC to -5 ºC.
D Liquid that has particles settling to the bottom when left to stand. ( )

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