chapter 18: separation and purification

apparatus
● made of glass
● not attacked by chemicals
● easy to clean

a. beakers
b. flasks (conical)
c. test-tubes
d. burette
e. pipette
f. measuring cylinders
g. gas syringe
h. funnel
i. stopwatch
j. thermometer
k. retort stand
l. balance

solutions and solubility

● solvent: substance that dissolves a solute

● solute: substance that is dissolved in a solvent
● solution: a mixture of one or more solutes dissolved in a solvent
● when water is the solvent, the solution is called an aqueous solution
● the solubility of a substance in water is the amount that dissolves in 100g of water at
that temperature
● solubility increases with temperature
● saturated solution: when a solution can dissolve no more solute at that temperature
separating solids from liquids

filtering, to remove a solid

this technique is used to separate an undissolved solid from a mixture of the solid and a
liquid/solution

● 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
● filtrate: the small liquid particles allowed to pass through the filter paper
● residue: the large solid particles allowed to are suspended on the filter paper

crystallisation

● 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

● 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
 ● then washed with distilled water to remove any impurities
● they are allowed to dry
● common places to dry crystals are between sheets of filter paper or in a drying oven

evaporation: to remove all the solvent

● the solubility of some substances changes very little as the temperature increases
● to obtain salt from an aqueous solution, you need to keep heating the solution to
evaporate the water

separating two solids

● find a solvent that dissolves only one of them

● this causes the other solid to act as th residue
● perform filtration

distillation: simple & fractional

simple distillation

● distillation is used to separate a liquid and soluble solid from a solution 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
distilled water which is collected in a beaker
 ● after all the water is evaporated from the solution, only the solid solute will be left
behind

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) with different boiling points
● 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
 ●
●

● used to refine petroleum

● used in producing ethanol
● used to separate nitrogen, oxygen and the noble gases from the air

paper chromatography

● chromatography is used to:

● separate substance from a mixture
● to check if a substance is pure
● identify substances in a mixture

separate substances
● use chromatography paper
● 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

to check if a substance is pure

● we can use a chromatogram to compare the substances present in a mixture to
known 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
● to identify whether a mixture contains a known sample, the dots need to be in line
with one another.

● 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 paper chromatography

identify substances in a mixture

● 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
● used for this as ink would run into the chromatogram along with the sample
● 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
locating agents

● 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
● example: ninhydrin

retention factor (rf) values

● 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

rf =distance ¿ origin ¿ ¿˙ origin ¿ solvent front ¿

distance ¿

● is a ratio
● has no units
● will always be less than 1

assessing purity

● pure substances melt and boil at specific and sharp temperatures

● 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
● 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

melting point test using an oil bath

● this is then int may appear lower than the sample's actual melting point