Paper Chromatography

• This technique is used to separate substances that 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.
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 travels up the paper by capillary action, taking some of the coloured
substances with it
• Different substances have different solubilities so will travel at different rates, causing the
substances to spread apart. Those substances with higher solubility will travel further than
the others
• This will show the different components of the ink / dye

Analysis of the
composition of ink using paper chromatography
 Interpret Simple Chromatograms

• If two or more substances are the same, they will produce identical chromatograms
• It is common practice to include a known compound as a reference spot
o This can help match up to an unknown spot or set of spots in order to identify it
• If the substance is a mixture, it will separate on the paper to show all the different
components as separate spots
• An impure substance will show up with more than one spot, a pure substance should only
show up with one spot

Locating Agents
• For chromatography to be useful the chemist needs to be able to see the
components move up the paper, which is not the case for colourless substances
such as amino acids or sugars
• Locating agents are substances which react with the sample and produce a
coloured product which is then visible
• 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

Using Rf values to identify components of a mixture

Retention Factor (Rf) Values

• These values are used to identify the components of mixtures
• The Rf value of a particular compound is always the same
• Calculating the Rf value allows chemists to identify unknown substances because it
can be compared with Rf values of known substances under the same conditions
•

Filtration & Crystallisation

• The choice of the method of separation depends on the nature of the substances being
separated
• All methods rely on there being a difference of some sort, usually in a physical property such
as boiling point between the substances being separated
 Separating a mixture of solids
• Differences in solubility can be used to separate solids
• For a difference in solubility, a suitable solvent must be chosen to ensure the desired
substance only dissolves in it and not other substances or impurities, e.g. to separate a
mixture of sand and salt, water is a suitable solvent to dissolve the salt, but not the sand

Filtration
• 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
• Filter paper is placed in a filter funnel above another beaker
• The mixture of insoluble solid and liquid is poured into the filter funnel
• 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

Filtration of a mixture of sand and water

 Crystallisation
• Used to separate a dissolved solid from a solution, when the solid is more soluble in hot
solvent than in cold (e.g. copper sulphate from a solution of copper (II) sulphate in water)
• 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
o 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 and solids will come out of the solution as the
solubility decreases, and crystals will grow
• Crystals are collected by filtering the solution
• They are then washed with distilled water to remove any impurities and then allowed to dry

Diagram showing the process of crystallisation

Distillation: Simple & Fractional

Simple Distillation
• 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

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
• However, more effective separation is to use fractional distillation where the liquids are closer
to boiling point and a higher degree of purity is required

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, and vapours will pass through a condenser, where
they cool and condense, turning into a liquid that will be collected in a beaker
• All of the substance is evaporated and collected, leaving behind the other components(s) of
the mixture
• For water and ethanol: ethanol has a boiling point of 78 ºC and water of 100 ºC. The mixture is
heated until it reaches 78 ºC, at which point the ethanol boils and distills out of the mixture
and condenses into the beaker
• When the temperature starts to increase to 100 ºC heating should be stopped. Water and
ethanol are now separated

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.
•
TEST FOR ANIONS
 the acidification with aqueous silver nitrate and aqueous barium nitrate / chloride is done to
remove ions that might give a false positive result
The most common ion that is removed is the carbonate ion
The choice of acid has to be considered so that it does not influence the results
For example, aqueous silver nitrate solution should not be acidified with hydrochloric acid as
this will form a white precipitate due to the chloride ion in the acid
For example, aqueous barium nitrate / chloride solution should not be acidified with sulfuric
acid as this will form a white precipitate due to the sulfate ion in the acid
Identification of Anions

Identification of Cations

• Metal cations in aqueous solution can be identified by the colour of the precipitate they
form on addition of sodium hydroxide and ammonia
• If only a small amount of NaOH is used then normally the resulting metal hydroxide
precipitates out of solution
• In excess NaOH some of the precipitates may re-dissolve
• A few drops of NaOH is added at first and any colour changes or precipitates formed are
noted
• Then the NaOH is added in excess and the reaction is observed again
• The steps are then repeated for the test using ammonia solution

Analysing results
• The table below contains the results for each of the cations included in the syllabus
• If a precipitate is formed from either NaOH or aqueous ammonia then it means that the
hydroxide is insoluble in water
• Zinc chloride, for example, reacts as such:
ZnCl2 (aq) + 2NaOH (aq) → Zn(OH)2 (s) + 2NaCl (aq)

• Ca2+ ions can be distinguished from Zn2+ and Al3+ as calcium hydroxide precipitate does
not dissolve in excess NaOH but both zinc hydroxide and aluminium hydroxide do
• Zn2+ ions can be distinguished from Al3+ ions as Zn(OH)2 dissolves in excess aqueous
ammonia but Al(OH)3 does not
• Most transition metals produce hydroxides with distinctive colours
 Identification of Gases

• Several tests for anions and cations produce gases which then need to be tested
• The table below indicates the tests for the gases included in the syllabus