Cambridge (CIE) IGCSE Your notes

Chemistry
Separation & Purification
Contents
Paper Chromatography
Locating Agents & Rf Values
Separation & Purification Techniques

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 Paper Chromatography
Your notes
Paper chromatography
Chromatography is used to separate substances and provide information to help
identify them
The components have different solubilities in a given solvent
E.g. Different coloured inks that have been mixed to make black ink
A pencil line is drawn on chromatography paper and spots of the sample are placed on it
A pencil is used for this as ink would run into the chromatogram along with the
samples
The paper is then lowered into the solvent container, making sure that the pencil line
sits above the level of the solvent so the samples don’t wash into the solvent container
The solvent used is usually water but it can be other substances such as ethanol
The solvent travels up the paper by capillary action, taking some of the coloured
substances with it
Different substances have different solubilities so they will travel at different rates,
causing the substances to spread apart
Those substances with higher solubility will travel further than the others

How to carry out chromatography

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 Your notes

The pigments in ink can be analysed using paper chromatography

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Interpret simple chromatograms
We can use a chromatogram to compare the substances present in a mixture to known Your notes
substances and make assumptions
Pure substances will produce only one spot on the chromatogram
Impure substances will produce more than one spot on the chromatogram
If two or more substances are the same, they will produce identical chromatograms
If the substance is a mixture, it will separate on the paper to show all
the different components as separate spots
It is common practice to include a known compound as a reference spot
This can help match up to an unknown spot or set of spots in order to identify it

Example chromatogram results

The brown ink has separated showing a spot of red ink, blue ink and yellow ink

We can draw several conclusions from this chromatogram:

The brown ink is a mixture as there are three dots
Red, yellow and blue are pure as there is only one dot for each
The brown ink contains red, blue and yellow as the dots are in line with one another
horizontally

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 Your notes
Examiner Tips and Tricks
Chromatograms in exams will be in black and white so to identify whether a mixture
contains a known sample, the dots need to be in line with one another.

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 Locating Agents & Rf Values
Your notes
Locating agents
Extended tier only
For chromatography to be useful, the chemist needs to be able to see the components
move up the paper
This is not the case for colourless substances such as amino acids or sugars
Locating agents can be used to see the spots
These are substances which react with the sample and produce a visible / coloured
spot for the product(s)
The chromatogram is treated with the agent after the chromatography run has been
carried out, making the sample runs visible to the naked eye

Retention factor (Rf) values

Extended tier only
Rf values are used to identify the components of mixtures
The Rf value of a particular compound is always the same
However, it does depend on the solvent used
If the solvent is changed then the Rf value changes
Calculating the Rf value allows chemists to identify unknown substances because it can
be compared with the Rf values of known substances under the same conditions
The retention factor, Rf, is calculated by the equation:

Rf =
distance moved by substance
distance moved by solvent
The Rf value:
Is a ratio
Has no units
Will always be less than 1

Worked Example
A student obtained the following chromatogram when carrying out chromatography.

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 Your notes

Calculate the Rf value of the substance.

Answer:
The Rf value of the substances in the chromatogram above can be calculated by:

distance moved by substance 3

Rf = = = 0.5
distance moved by solvent 6

Examiner Tips and Tricks

When you calculate Rf values in exams, make sure to use your ruler carefully to
measure the distance moved by the solvent and the substance, or use any scale
provided on the diagram.
Mark schemes can be strict about the values accepted, so it's important to be as
accurate as possible when determining these distances.

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 Separation & Purification Techniques
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Filtration & crystallisation
The choice of separation technique depends on the substances being separated
All techniques rely on a difference in properties of the chemicals in the mixture
This is usually a physical property such as boiling point

Separating a mixture of solids

Differences in solubility can be used to separate solids
For a difference in solubility, a suitable solvent must be carefully chosen
Only the desired substance should dissolve in the solvent
Other substances or impurities in the mixture should not dissolve in the solvent
For example, to separate a mixture of sand and salt:
Water is a suitable solvent because salt is soluble in water, but sand is insoluble in
water

Filtration
This technique is used to separate an undissolved solid from a mixture of the solid and a
liquid / solution ( e.g. sand from a mixture of sand and water)
Centrifugation can also be used for this mixture
A filter paper is placed in a filter funnel above another beaker
The mixture of insoluble solid and liquid is poured into the filter funnel
The filter paper will only allow small liquid particles to pass through in the filtrate
Solid particles are too large to pass through the filter paper so will stay behind as a
residue

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 Filtration of a mixture of sand and water

Crystallisation Your notes

This method is used to separate a dissolved solid from a solution
A simple application of this is to heat a solution to boiling, remove the heat and leave
the solvent to evaporate
A more common application of this is sometimes called crystallisation
This is when the solid is more soluble in hot solvent than in cold, e.g. copper sulphate
from a solution of copper(II) sulphate
The solution is heated, allowing the solvent to evaporate and leaving a saturated solution
behind
You can test if the solution is saturated by dipping a clean, dry, cold glass rod into the
solution
If the solution is saturated, crystals will form on the glass rod when it is removed and
allowed to cool
The saturated solution is allowed to cool slowly
Solids will come out of the solution as the solubility decreases
This will be seen as crystals growing
The crystals are collected by filtration
They are then washed with distilled water to remove any impurities
Finally, they are allowed to dry
Common places to dry crystals are between sheets of filter paper or in a drying oven

The process of crystallisation

The solution is slowly heated to remove around half of the liquid. The remaining liquid will
evaporate slowly

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 Your notes
Examiner Tips and Tricks
In exams, you need to be specific that no more than half of the solution is removed by
direct heating or you may lose a mark.

Distillation: simple & fractional

Simple distillation
Distillation is used to separate a liquid and soluble solid from a solution (e.g. water from a
solution of saltwater) or a pure liquid from a mixture of liquids
The solution is heated and pure water evaporates producing a vapour which rises
through the neck of the round-bottomed flask
The vapour passes through the condenser, where it cools and condenses, turning into
pure water which is collected in a beaker
After all the water is evaporated from the solution, only the solid solute will be left behind

Simple distillation apparatus

Diagram showing the distillation of a mixture of salt and water

Simple distillation can be used to separate the products of fermentation, such as
alcohol and water

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 However, fractional distillation is a more effective separation technique, commonly
used when the boiling points of the liquids are close and/or a higher degree of purity is
required, such as crude oil Your notes
Fractional distillation
Used to separate two or more liquids that are miscible with one another (e.g. ethanol
and water from a mixture of the two)
The solution is heated to the temperature of the substance with the lowest boiling point
This substance will rise and evaporate first
The vapours will pass through a condenser, where they cool and condense
The condensed liquid is then collected in a beaker
All of the substance is evaporated and collected, leaving behind the other
component(s) of the mixture
For water and ethanol:
Ethanol has a boiling point of 78 ºC
Water has a boiling point of of 100 ºC
The mixture is heated until it reaches 78 ºC, at which point the ethanol distills out of
the mixture and into the beaker
When the temperature starts to increase to 100 ºC heating should be stopped as
the water and ethanol are now separated

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 Your notes

Fractional distillation of a mixture of ethanol and water

An electric heater is safer to use when there are flammable liquids present
The separation of the components in petroleum is achieved by fractional distillation on
an industrial scale
Fractional distillation of crude oil is not carried out in school laboratories due to the toxic
nature of some of the components of the crude oil, but it can sometimes be simulated
using a synthetic crude oil made specially for the demonstration

Worked Example
A student is given a mixture of calcium sulfate, magnesium chloride and water. The
table below shows some information about calcium sulfate and magnesium chloride.

substance solubility in water state at room temperature

calcium sulfate insoluble solid

magnesium chloride soluble solid

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 How does the student obtain magnesium chloride crystals from the mixture?
1. Crystallisation followed by distillation Your notes
2. Crystallisation followed by filtration
3. Distillation followed by crystallisation
4. Filtration followed by crystallisation
Answer
The correct answer is D because:
The difference in solubility in water means the first step is to make a solution
The magnesium chloride will dissolve, but the solid calcium sulfate will be left
behind
The mixture is filtered to remove the calcium sulfate and then evaporated and
crystallised to obtain magnesium chloride crystals

Examiner Tips and Tricks

You may be asked how to separate a mixture of gases:
One method involves cooling the gaseous mixture sufficiently to liquefy all of the
gases, which are then separated by fractional distillation.
They can also be separated by diffusion, where the boiling points are very close
or it is impractical or expensive to use fractional distillation.

Assessing purity
Pure substances melt and boil at specific and sharp temperatures
For example, water has a boiling point of 100°C and a melting point of 0°C
Mixtures have a range of melting and boiling points as they consist of different
substances that melt or boil at different temperatures
Therefore, melting and boiling point data can be used to distinguish pure
substances from mixtures
An unknown pure substance can be identified by experimentally determining its melting
point and boiling point and comparing them to literature values / data tables
Boiling points are commonly determined by distillation
Melting point analysis is routinely used to assess the purity of drugs for example
This is done using a melting point apparatus which allows you to slowly heat up a
small amount of the sample, making it easier to observe the exact melting point

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 Your notes

Melting point test using an oil bath

This is then compared to data tables

The closer the measured value is to the actual melting or boiling point, the purer the
sample is
If the sample contains impurities:
The boiling point may appear higher than the sample's actual boiling point
The melting point may appear lower than the sample's actual melting point

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