SEPARATION TECHNIQUES /METHODS

1. Filtration

2. Crystallisation can mean a liquid substance changing to its solid form. However, the term
usually means what happens when the liquid from a solution has evaporated to a point
beyond the solubility limit. Then solid crystals will 'grow' out of the solution because the
solution is too concentrated for all the solid to remain dissolved at that temperature.
Crystallisation is often done from a hot concentrated solution, because most substance are
more soluble in the hot liquid. Consequently on cooling a hot concentrated solution, crystals
form as the solubility gets less and less.
The processes of crystallisation are demonstrated in
the diagrams below.
3. Magnetism
Magnetism is a technique used to separate a mixture of magnetic substance and non-
magnetic substances (e.g. iron filings and saw dust). Magnetic substances (e.g., iron fillings)
will be attracted to the magnet while non-magnetic substances (e.g. saw dust) will not be
attracted to the magnet.

4. Separating funnel
If two liquids do not mix completely, they form two separate layers and are known as
immiscible liquids (e.g. oil or paraffin and water). This is
illustrated in the diagram below, where the lower liquid will be more
dense than the upper layer of the liquid and shows how you can
separate these two liquids using a separating funnel.

5. Decantation
Decanting is the simplest possible way of separating a liquid
(pure or a solution) from an insoluble solid which has a density
greater than water (i.e. > 1.0 g/cm3). The solid-liquid mixture is
allowed to stand e.g. in a beaker, until all the solid settles out to the bottom of the container.
Then the liquid is carefully poured off to leave the insoluble solid behind. However it is
inefficient e.g. a small amount of liquid is always left in the solid residue and very fine solid
particles take some time to settle out and any disturbance of the liquid can mix them in with
the liquid being poured off. Wine may be served in a decanter to leave the undesirable solids
behind - no good for bits of cork though, they float!
6. Centrifuging
Centrifuges are devices or apparatus that can be used to separate insoluble materials
(usually a solid) from a liquid, where normal filtration does not work well e.g. a
suspension of very fine (tiny) solid particles. The centrifuge consists of carriage or glass
tube holder, mounted on an electrically motor driven vertical axle. The carriage holds the
balanced glass tubes of equal amounts of the solid-liquid mixture in each tube, all tubes
initially in a horizontal position before the motor is switched on. The tube carriage is rotated
at high speed safely in a fully enclosed container. Unbalanced tubes can break with the extra
vibration and this situation has a 'knock on' effect, quite literally, as other tubes are likely to
shatter with the erratic high speed unbalanced motion. High velocity glass fragments are not
good for you! On rapid rotation of the carriage the tubes whirl round horizontally and the
centrifugal force causes the more dense insoluble material particles to move outwards,
separating from the liquid. When rotation ceases the solid particles end up at the 'bottom' of
the glass tubes with the liquid above. After the centrifuging operation the liquid can be
decanted off and the solid is left at the bottom of the glass tube. You might be interested in
the solid, liquid or both products depending on the context. Centrifuges come in all sizes and
centrifuge technology has many applications in the separation of mixtures and the
purification of materials.
Uses-applications of centrifuging: In biology cells can be separated from fluids. A waste
'sludge' can be treated e.g. removing toxic solids from contaminated water from an industrial
process. Milk can be separated from whey. Edible oils, wines and spirits can be cleaned or
'clarified' of solid impurities. Expensive oils and other fluids used as lubricants in machining
metal parts in industry become contaminated with tiny metal fragments. The larger pieces of
metal are easily removed by filtration or sedimentation (allowing to settle out) but the very
fine metal particles can only be removed by using a centrifuge. This is likely to be a cheaper
option than buying more machine fluid AND reducing pollution since the fluid is recycled
leaving less waste to dispose off.
7. Paper Chromatography

This method of separation is used to

see what coloured materials make up
e.g. a food dye analysis.
The material to be separated e.g. a
food dye (6) is dissolved in a solvent
and carefully spotted onto
chromatography paper or a thin layer
of a white mineral material on a glass
sheet. Alongside it are spotted known colours on a 'start line' (1-5).
The paper is carefully dipped into a solvent, which is absorbed into the
paper and rises up it. The solvent may be water or an organic liquid like an alcohol (e.g.
ethanol) or a hydrocarbon, so-called non-aqueous solvents. For accurate work the distance
moved by the solvent is marked on carefully with a pencil and the distances moved by each
'centre' of the coloured spots is also measured. These can be compared with known
substances BUT if so, the identical paper and solvent must be used (See Rf values below).
Due to different solubilities and different molecular 'adhesion' some colours move more than
others up the paper, so effecting the separation of the different coloured molecules.
Any colour which horizontally matches another is likely to be the same molecule i.e. red (1
and 6), brown (3 and 6) and blue (4 and 6) match, showing these three are all in the food dye
(6).
Note that at the start of the experiment, the start line:
(i) Should not be in the solvent; because if the start line is in the solvent, the mixture
substances and the colours on it would dissolve in the solvent and will not move up in the
separating medium (filter paper). To prevent this, the start line should not be in the solvent at
the star of the experiment.
(ii) Should be draw in pencil and not in ink, because if the start line is drawn in ink,
colours in ink (ink has many colours) would also separate on the separating medium
thereby interfering with the results. Hence drawn in pencil so as to prevent this from
happening.
The distance a component (colour or dye) moves, compared to the distance the solvent front
moves (top of grey area on 2nd diagram) is called the reference value or Rf value and has a
value of 0.0 (not moved - no good), to 1.0 (too soluble - no good either), but Rf ratio values
between 0.1 and 0.9 can be useful for analysis and identification.
distance moved by disolved substance ( solute )
The formula is: Rf =
distance moved by solvent
Some technical terms: The substances (solutes) to be analysed must dissolve in the solvent,
which is called the mobile phase because it moves. The paper or thin layer of material on
which the separation takes place is called the stationary or immobile phase because it
doesn't move.
Factors that Affect Chromatography
- the separating medium ( stationary phase). How thick and porous the stationary phase is.
- the surface tension of the solvent, ie how fast or slow the solvent spreads on the medium
 - the viscosity of the solvent, ie how thick or thin the solvent is.

Applications of Chromatography
 Separating proteins from amino acids
 Separating pigments from chlorophyll
 Obtaining anti-biotics from their growing media
 Identifying flavouring components in food stuffs
8. Simple distillation
Simple distillation
is used to obtain pure
liquid from a
solution. e.g.
obtaining pure water
from salt or sea
water.

Distillation
involves 2 stages and
both are physical state changes.
(i) The liquid or solution mixture is boiled to vaporise the volatile component in the mixture
(liquid ==> gas). The ant-bumping granules give a smoother boiling action.
(ii) The vapour is cooled by cold water in the condenser to condense (gas ==> liquid) it back
to a liquid (the distillate) which is collected.
This can be used to purify water because the dissolved solids have a much higher boiling
point and will not evaporate with the steam.
9. Fractional distillation
Fractional distillation is used to separate miscible liquids (liquids that mix completely) and
have different boiling points.
Fractional distillation involves 2 main stages
and both are physical state changes. It can
only work with liquids with different
boiling points. However, this method only
works if all the liquids in the mixture are
miscible [e.g. alcohol(ethanol) and water,
crude oil etc].
(i) The liquid or solution mixture is boiled to
vaporise the most volatile component in the
mixture (liquid ==> gas). The ant-bumping
granules give a smoother boiling action.
(ii) The vapour passes up through a
fractionating column, where the separation
takes place (theory at the end). This column is
not used in the simple distillation described
above.
(iii) The vapour is cooled by cold water in the condenser to condense (gas ==> liquid) it
back to a liquid (the distillate) which is collected.
This can be used to separate alcohol from a fermented sugar solution.
It is used on a large scale to separate the components of crude oil, because the different
hydrocarbons have different boiling and condensation points.
Fractional Distillation Theory:
Imagine green liquid is a mixture of a blue liquid (boiling point 80oC) and a yellow liquid
(boiling point 100oC), so we have a coloured diagram simulation of a colourless alcohol and
water mixture! As the vapour from the boiling mixture enters the fractionating column it
begins to cool and condense. The highest boiling or least volatile liquid tends to condense
more i.e. the yellow liquid (water). The lower boiling more volatile blue liquid gets further up
the column. Gradually up the column the blue and yellow separate from each other so that
yellow condenses back into the flask and pure blue distils over to be collected. The 1st liquid,
the lowest boiling point, is called the 1st fraction and each liquid distils over when the top of
the column reaches its particular boiling point to give the 2nd, 3rd fraction etc.