Experimental techniques

Purity of a substance

The purity of a substance can be determined by its melting point or boiling point.

➢ A pure solid has a fixed melting point.

➢ A pure liquid has a fixed boiling point.
➢ Impurities lower the melting point of a solid and increase the boiling point
of a liquid.
➢ The boiling point of a liquid can be increased by increasing its pressure. The
boiling point of a liquid can be decreased by decreasing its pressure.

CHROMATOGRAPHY

Chromatography is used to separate colours, pigments and dyes.

This method is used in the separation of small quantities of mixtures. The mixture
is separated based on the difference in solubility of its components in a particular
solvent.
The solvent used can be ethanol or water or a mixture of ethanol and water.
Method
• A pencil line is drawn on chromatography paper and spots of the sample
are placed on it.
• Pencil is used instead of ink as ink would also separate and would interfere
with the chromatogram (the result obtained after carrying out
chromatography).
• The paper is then lowered into the solvent container, making sure that the
pencil line is above the level of the solvent so the samples don´t wash into
the solvent container.
• Solvent moves up the paper taking different components along at different
rates.
• 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

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• This will show the different components of the ink / dye

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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
• 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

Note: Number of rings/dots = number of substances

Retention Factor (Rf) Values

These values are used to identify the components of mixtures.

The Rfvalue 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
Calculation
The formula to calculate the retention factor is:
Retention factor = Distance travelled by substance

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 Distance travelled by solvent
The Rf value is a ratio and therefore has no units

Locating Agents

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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.

Separation techniques
The choice of the method of separation depends on the nature of 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.
Decantation
Decantation involves carefully pouring the liquid in another container and leaving
behind the undissolved solid. This method is suitable for separating suspension
(undissolved solid) for example sand from water.

Filtration

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Filtration is used to separate a mixture of a liquid (or solution) and an insoluble
solid. The insoluble solid is collected as the residue while the liquid is collected as
the filtrate.

Evaporation to dryness
E.g separating a mixture of salt and water. Water is heated until all the water has
evaporated leaving behind salt.

Crystallisation
This method is 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

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• Test for saturation: A clean, dry, cold glass rod is dipped 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 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

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Separating a mixture of sand and salt

Sublimation
• This technique can be used to two substances, provided that one substance
sublimes and other does not.
• The mixture is placed in an evaporating dish with a glass funnel inverted on
it.
• Evaporating dish is heated.
• The substance which sublimes will stick with the walls of funnel. And other
substance will remain in the dish.

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Simple distillation
• Used to separate a liquid and soluble solid from a solution (e.g. water from
a solution of salt water)
• 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

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Important Note:
1. The thermometer should be placed beside the side arm of the distillation flask.
This ensures that the thermometer measures the boiling point of the substance
that is being distilled.
2. Cold water enters the bottom of the condenser and leaves from the top after
cooling the water vapour.
3. The condenser slopes downwards so that the pure solvent formed is collected
into the receiver (beaker).
4. If the distillate is volatile, the receiver is placed ina container filled with ice. This
keeps the temperature of the distillate low so that it remains in the liquid state.

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Graph showing how temperature changes as a salt solution is distilled

This method can be used to separate mixtures of liquids with different boiling
points.but it is difficult to separate mixtures of liquids whose boiling points differ
by less than 200C. In this case fractional distillation is used.

Fractional distillation
• This method is used to separate liquids with different boiling points.
• It is same like simple distillation whereas in it fractionating column is used
to separate two liquids.
• Fractionating column is packed with glass beads to provide larger surface
area for quick condensation.
• When boiling point of any liquid is reached, it’s vapor rises, passes through
fractionating column, condensed in the condenser and collected in conical
flask.
• If any liquid with high boiling point evaporates it is condensed by
fractionating column.

Important Note:
1. The liquid with the lowest boiling point will distil over the condenser first.
2. The vapours of liquids with higher boiling points condense along the
fractionating column and re-enter the round-bottomed flask.

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Graph showing how temperature changes as an ethanol/water mixture is
fractionally distilled

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