Exercise No.

1: Demonstration sessions for various purification techniques such as

filtration, decantation, crystallization, distillation and chromatography.

Few important terms

A solvent is a liquid that dissolves the substance, in doing so it must completely break
the bonds between the particles in the substance being dissolved (the solute). This
enables the solute particles to fully mix with the solvent.
The solute is the substance that is being dissolved in a solvent. A solid may dissolve in
one liquid (soluble) but not in another (insoluble).
A solution is a mixture of a liquid with something dissolved in it. If you evaporate the
solvent away, you should be left with the 'dry' solid solute you dissolve in the first
place.

Soluble means the substance (gas, liquid or solid) dissolves in a liquid to form a

solution.

Insoluble means a substance won't dissolve in a particular liquid.

Solubility is how much of a substance (the solute) will dissolve in a liquid solvent to
give a saturated solution. A saturated solution is one in which no more substance will
dissolve in the liquid at a particular temperature.

Evaporation means a liquid changing to a gas or vapour. In separation, its removing

the liquid from a solution, usually to leave solid crystals.

It can be done quickly with gentle heating or left out to 'dry up' slowly in 'open air'.
The solid will almost certainly be less volatile than the solvent and will remain as a
crystalline residue.
Evaporation is often followed by crystallization.
1. FILTERATION

This operation is performed for the separation of the precipitate from the mother
liquor. The media employed for filtration are:

1. Filter paper (Ordinary filter paper/quantitative filter paper)

2. Sintered glass filtering crucibles/vitreosil filtering crucibles/porcelain filtering
crucibles

The choice of the filtering medium will be controlled by the nature of the precipitate.
Filtration can be used to isolate the product of a reaction, the product maybe
insoluble or a crystallized product, remove solid impurities from a solution. It is also
used to remove some solids in water for our domestic supply.
 2. Decantation

Decanting is a chemical laboratory process used to separate mixtures. Decanting is

just allowing a mixture of solid and liquid or two immiscible liquids to settle and
separate by gravity. This process can be slow and tedious without the aid of a
centrifuge. In this process once the mixture components have separated, the lighter
liquid is poured off leaving the heavier liquid or solid behind. Typically, a small
amount of the lighter liquid is left behind.

In laboratory conditions, small volumes of mixtures are decanted in test tubes. If time
is not a concern, the test tube is kept at a 45° angle in a test tube rack. This allows
the heavier particles to slide down the side of the test tube while allowing the lighter
liquid a path to rise to the top. If the test tube were held vertically, the heavier
mixture component could block the test tube and not allow the lighter liquid to pass
as it rises. ………………………………………………………………………………………………………………………

A centrifuge can greatly increase the rate of separation by simulating a great increase
in the force of gravity.

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/cm 3).
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.
Some mixtures that can be decanted:
● Oil and water - oil floats on top of water. Decanting the mixture allows the oil to be
poured off the water.
● Gasoline or kerosene and water - this mixture is an example often cited as a safety
hazard. Decanting a mixture containing flammable solvents can be dangerous as the
flammable material evaporates and forms dangerous fumes.
● Dirt and water - muddy water can be cleared up by decanting. The soil will sink to
the bottom of the tube allowing the clear water to be poured off.
● Wine - Sediment from the fermentation process can produce an undesirable taste.
Wine is decanted to separate the wine from these sediments.
● Cream and milk - Cream is separated from milk by decantation. Cream rises to the
top of the milk mixture and is easily skimmed off.
● Blood and plasma: A centrifuge is necessary for this decantation. Plasma can be
removed from blood by decantation.

3. Crystallisation 
It can mean a liquid (dissolved) substance changing to its solid form 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 the
entire solid to remain dissolved at that temperature.
Crystallisation is often done from a hot concentrated solution, because most
substances 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.
Crystallisation is also an important purification method because trace impurities tend
to stay in solution as solubility differs from substance to substance.
Drying may be the final stage in the chemical preparation of a product. There may be
traces of solvent in the solid product e.g. water or an organic solvent.
A solid product can be left in a fume cupboard to allow any excess solvent to
evaporate.
A solid product can be gently heated in an oven.

A solid product can be dried in desiccators, which contains a drying agent like silica
gel, which absorbs moisture (water vapor) from the air, which had evaporated from
the solid product. It is also a way of keeping a dried product dry! Many chemicals will
absorb moisture from the air, which is obviously prevented if they are stored in a dry
air environment

4. Chromatography
A technique known as chromatography, which is a term taken from the Greek
language & means “written in color”, will be used to separate the substances into
their various colors.

Chromatography is a separation process that is achieved by distributing the

components of a mixture between two phases, a stationary phase and a mobile phase.
Those components held preferentially in the stationary phase are retained longer in
the system than those that are distributed selectively in the mobile phase. As a
consequence, solutes are eluted from the system as local concentrations in the
mobile phase in the order of their increasing distribution coefficients with respect to
the stationary phase; ipso facto a separation is achieved
VARIOUS TYPES OF CHROMATOGRAPHY
I. On the basis of interaction of solute to the stationary phase
a. ADSORPTION CHROMATOGRAPHY

b. PARTITION CHROMATOGRAPHY

c. ION EXCHANGE CHROMATOGRAPHY

 d. MOLECULAR EXCLUSION CHROMATOGRAPHY

II. On the basis of chromatographic bed shape

a. COLUMN CHROMATOGRAPHY
b. PLANAR CHROMATOGRAPHY
c. PAPER CHROMATOGRAPHY
d. THIN LAYER CHROMATOGRAPHY
e. DISPLACEMENT CHROMATOGRAPHY
III. Techniques by physical state of mobile phase
a. GAS CHROMATOGRAPHY
b. LIQUID CHROMATOGRAPHY
c. AFFINITY CHROMATOGRAPHY
d. SUPERCRITICAL FLUID CHROMATOGRAPHY
 Exercise No.1.1
1) How to separate soil particles from water?

Ans) We can separate soil particle from water by the process of sedimentation and
filtration.Segmentation is a process based on gravity,thereby allowing the heavier
particle (soil) to settle down and the clear liquid(water) is collected at the top
phase.The heavier particle that settled down are called as sediment

2) Explain separation of ethanol from water.

Ans) Fractional distillation is a method for separating the liquid from a mixture of
two or more liquids. For example, liquid ethanol can be separated from a mixture
of ethanol and water by fractional distillation.This method works because the
liquid in the mixture has different boiling points.

3) How can once separate NaCl from CaCO3 in a given powdered mixture form?

Ans)Ans)To separate NaCl from CaCo3 in a mixture form we need to: Firstly,water
should be added to the mixture of NaCI and CaCo3 water.Stir water into the
mixture and dissolveNaCI.
The Pour off the solution and evaporate it to recover the separated NACL.
Name & Signature of Teacher In charge-