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Methods of separating mixtures and purifying them

A mixture is a material made up of at least two


substances which may be elements or compounds,
physically mixed together but are NOT chemically
combined together, so the elements and compounds
retain their original chemical properties i.e. components
of a mixture retain their individual chemical
properties. Components of a mixture can be separated by
physical means

A.Distillation (Also known as simple distillation)


i.

ii.

The liquid or solution mixture is heated to boil and


vaporize the most volatile component in the mixture (liquid
==> gas). The ant-bumping granules give a smoother boiling
action.
The vapour passes up from the flask and down into
the condenser, where it is cooled by cold water
and condenses (gas ==> liquid) back to a liquid (the
distillate) which is collected in the flask.

Simple distillation can be used to separate a liquid from a


solution (separating the solvent that dissolves substances,
from a solute - the substance that had dissolved).
Simple distillation works fine if the substances to be
separated have very different boiling points like salt and
water, BUT it is too simple a method to separate a mixture
of liquids especially if the boiling points of the components
are relatively close e.g. separating the fractions in crude oil
and separating water and ethanol obtained from fermenting
sugar to alcohol with yeast.

For these sort of mixtures, you need fractional distillation

B. Fractional distillation
How can you separate a complex mixture of liquids by a
method of distillation? Simple distillation isn't good enough
to do an efficient job of separating liquids with boiling
points that may be relatively close together. The liquids
must all dissolve in each other i.e. they are all fully miscible.
Fractional distillation involves 2 main stages and both are
physical state changes. It can only work with liquids with
different boiling points but the boiling points can be quite
close together. However, this method only works if all the
liquids in the mixture are miscible (e.g. alcohol & water,
hydrocarbons in crude oil etc.) and do NOT separate out
into layers like oil & water (immiscible).
i.

ii.

The liquid or solution mixture is poured into the roundbottomed flask, heated and boiled to vaporize the most
volatile component in the mixture (liquid ==> gas). The antbumping granules give a smoother boiling action.
The vapour passes up through a fractionating column, where
the separation takes place. The fractionating column is
packed with glass beads or short rods/tubes to give a large
surface area for both evaporation and condensation. This
column is not used in the simple distillation described above.
When the temperature at the top of the column reaches
the boiling point of the lowest boiling component, that
component will then distil over into the condenser. The
higher boiling liquids, the most easily condensed liquids,
condense and separate out, running back into the flask
mixture, whereas the lower boiling liquid's vapour passes
through into the Liebig condenser. This is because the

iii.

temperature falls as you rise up the special fractionating


column.
The vapour is cooled by cold water in the condenser
to condense (gas ==> liquid) it back to a liquid (the distillate)
which is collected in the flask. The 1st liquid, with the
lowest boiling point, evaporates first, and is called the 1st
fraction. Then, each liquid distils, with increasing boiling
point, over the top of the column, when it reaches its
particular boiling point to give the 2nd, 3rd fraction etc.
The boiling point of each fraction can be read off the
thermometer.

Fractional distillation is use separate oxygen and nitrogen


from liquefied air, though the distillation takes place at
very low temperatures, below -160oC
It is used on a large scale to separate the components of
crude oil, because the different hydrocarbons have
different boiling and condensation points (see oil). Very tall
fractionating columns are used to ensure the separation of
an extremely complex mixture of hydrocarbons.

C. Paper chromatography
This method of separation is used to see what colored
materials make up
Chromatography can be used to identify substances and
check on the purity of a substance.
i.

The colored material mixture to be separated e.g. a food


dye (6 on the diagrams below) is dissolved in a solvent like
ethanol ('alcohol') and carefully spotted onto
chromatography paper or a thin layer of a white mineral
material on a glass sheet (immobile or stationary phase).
Alongside it are spotted known colors of pure dyes on the
reference 'start line' (1-5), which is drawn in pencil so it
doesn't 'run or smudge'

ii.

The paper is carefully dipped into the solvent (mobile


phase) and suspended so the start line (baseline) is above
the liquid solvent, otherwise all the spots would dissolve in
the solvent! The solvent is absorbed into the paper and
rises up it as it soaks into the paper. The solvent may be
water (aqueous solvent) or an organic liquid non-aqueous
solvent like an alcohol (e.g. ethanol, butanol) or a
hydrocarbon (e.g. hexane).

For better results:


Try different solvents e.g. water or ethanol ('alcohol'),
propanone ('acetone') or butanol.
If you can enclose the whole system in a larger glass
container with a lid on, it reduces evaporation of the
solvent.

The fastest moving spots should be able to move at least 5


cm to get a reasonably accurate Rf value.

At the start
mark a baseline in
pencil - mark
won't dissolve or
run. Make sure it
is above the
surface of the
solvent, so as not
to dissolve the
spots directly.

The prepared
chromatogram

When the
solvent is near

paper is carefully
placed in the

the top of the


paper, the paper

solvent so the
baseline and

is removed and
allowed to dry

spots are above


the solvent. The

before
examination and

solvent is allowed
to move up the

measurement of
the RF values of

You then carefully paper. The colors


begin to separate
put spots of the
out. Its best
mixtures and
done in a larger
standards (known
materials) onto
the baseline. so
we start with an
even line of
solute chemical
spots e.g. dyes
or any colored
compound.

covered beaker
so the solvent
doesn't
evaporate into
the laboratory!

all the dyes.


The final result
is called the
chromatogram.

How do we
measure an Rf
value? Its
quite simple to
measure a
reference value
(Rf) value for a
dye colour. e.g.
for the green
dye spot, S
might be 7.2
cm, D might be
5.3 cm, so
Rf = D/S =
5.3/7.2 = 0.74

Reference value (Rf)= distance moved by substance spot(D)


distance moved by solvent front (S)
THEORY OF CHROMATOGRAPHY
Due to different solubilitys of the coloured chemicals in
the solvent AND different strengths of molecular
'adhesion' attraction to the paper, some colors the
components travel different lengths.
The final result is the vertical separation of the spots up
the paper which is now referred to as the chromatogram.
Any colour which horizontally matches another is likely to
be the same molecule
The distance a substance moves, compared to the distance
the solvent front moves is called the reference value. It can
be useful for identification of materials.
I.

It is possible to analyse colourless mixture of chemicals if


the 'spots' can be made coloured by add LOCATING
AGENTS
If a substance is pure, only one spot will appear on the
chromatogram, impurities may show up as other faint spots.

D. Four techniques used in a particular separation and


purification procedure
Filtration, evaporation, crystallization and drying are four
techniques used in the isolation and purification of a solid
product from a chemical reaction

I.

Filtration
Filtration uses a filter paper or fine porous ceramic to
separate a solid from a liquid. It works because the tiny
dissolved particles are too small to be filtered BUT
any insoluble non-dissolved' solid particles are too big to go
through!
Filtration removes solid impurities from a solution

II.
II.
II.
II.
II.
II.
II.
II.
II.
Evaporation
Evaporation means a liquid changing to a vapour. In a
mixture separation procedure, it is the removal of most of
the liquid from a solution, usually to cause crystallization to
leave solid crystals in the evaporating dish - but you should
not heat some salts to complete dryness.
It is advisable to do filtration before evaporation to
remove insoluble impurities.

III.

Crystallization
Crystallization 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 of the dissolved solid. 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.
Crystallization is often done from a hot concentrated
solution, because most substance are more soluble the
hotter the liquid.
Consequently, on cooling a hot concentrated solution,
crystals form as the solubility gets less and less and the
solubility limit is exceeded, so crystals must form.
You get the best and bigger crystals by not over
evaporating the hot solution and allowing the crystals to
form as slowly as possible. You can leave a fairly
concentrated hot solution to slowly cool and further
evaporation takes place to give a good yield of crystals.

Crystallization is an important purification method because

impurities tend to stay in the solution and dont come in the


crystals. This may due to their solubility limit not being
exceeded or the impurity particles will not fit into the
regular crystal lattice of the desired crystallizing product .

IV.

DECANTATION
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.

A stirrer rod can be kept over the top to control the


pouring of the liquid

E. Miscellaneous Separation Methods and


other apparatus uses
I.

Separating funnel
Used for 2 or more immiscible liquids
i. The mixture is put in the separating
funnel with the stopper on and the tap
closed and the layers left to settle out.
The denser liquid will always from the
lower layer
ii. The stopper is removed so no vacuum
forms as the liquid flows down, and the
tap is opened.
iii. As the less dense liquid goes out, close the tap.

II.

Magnet

Can be used to separate iron, nickel, cobalt, or steel


from a mixture.
III.

IV.

Solvent Extraction
Solvent extraction involves sing a liquid to dissolve a
solid / another liquid to separate it from a mixture.
Centrifugation
Used to separate insoluble materials from a liquid, where
normal filtration does not work well e.g. a suspension of
very fine solid particles.
Involves rotating a test tube at high speed so particles
form layers according to their difference in density
Used to separate/purify: Blood, milk, edible oils, lubricants