Separation and Purification

Filtration
Principle: Separation of an insoluble water from a solution or solvent

Apparatus

Note:
Limitation: The process of Filtration cannot separate a soluble solid from a solution.
Importance: Purification of river water to make it drinkable.
Crystallization
Principle: Separation of a soluble solid from a solution.
Crystal: The definite geometrical shape is called it's crystal. The process of obtaining a
pure solid sample from it's solution.

Methods to Crystallize a substance

Cold Method

e.g. prepare cold crystals of copper sulphate (CuSO4)

1. Prepare a saturated solution of CuSO4.

2. Filter the solution.
3. Place the filtrate in a cold atmosphere, after many hours few large size crystal will
form.
4. Filter to separate crystal, wash it with distill water and then dry it between the folds
of filter paper.

Note:

It is a slow process but very suitable method for making large size crystals.
It is a very suitable method for making heat unstable crystals.

Hot Method

e.g. prepare cold crystals of copper sulphate (CuSO4)

1. Prepare a saturated solution of CuSO4.

2. Filter the solution.
3. Place the filtrate on flame in evaporating dish until crystallizations, cool it, filter it
and wash it with distill water and then dry it between folds of filter paper.

Note:

Don't heat the filtrate till dryness because:

1. The crystals may decompose, if it is heat unstable.
2. water of crystallization may loss if present.
3. A powdered compound is obtained instead of crystals.
Effects of Excess heat on Crystals

Example

Importance
Desalination of Sea Water (Removal of salt from Sea Water)

Simple Distillation

Principle: Separation of pure solvent from from soluble solid solute.

Apparatus

1. Order of working: First boiling and then condensing.

2. Anti bumping stones are added to avoid splashing or bumping of Solution at

boiling point to prevent large bubbles to form and to allow small bubbles to form at
boiling point.

3. The bulb of the thermometer should be parallel to the mouth of delivery tube to
measure an accurate boiling point.
4. In water condenser, the water should enter from the lower bottom side to ensure
good condensation because when water move from bottom to top then it
completely fill the condenser, stay longer and the vapors which are just going to
escape from the condenser will also occur.

5. Top of the receiver flask should be open to allow trap air and uncondense vapor
to escape.

Importance:

1. To make distill water.

2. Desalination

Note: Uses of Distill water

1. As electrolyte in car battery.

2. It is used in pharmacy to make medecines.
3. For making solutions of exact concentration in laboratory for experiments.

Fractional Distillation

Principle: Separation of miscible (dissolved) liquids from each other according to

the difference in their boiling points.

Apparatus

Function of Fractionating column

It is packed with glass beads which increases its surface area, it's function is to
condense back the vapors of unboiled liquid and allow the vapors of the liquid
whose boiling points has been reached to pass through.

Note:

1) The liquid with the lowest boiling point separate first and so on and so forth.
2) When b.p point one particular liquid is reached then reading on thermometer
becomes constant until it is distilled over. When one liquid is distilled over then
reading on thermometer starts to rise and also droplets in the receiver flask stops
for a while, in this way the student comes to know that one liquid is completely
collected in the receiver flask.
Importance

1. Fractional Distillation of petroleum.

2. Fractional Distillation of liquid Air.

What happens when a solution of water and ethanol undergoes Fractional

distillation?

A column called fractionating column, is attached to the round-bottomed flask and

the condenser.
Many glass beads in the fractionating column provide a large surface area for vapor
to condense on.
During Fractional distillation,
1. The liquid with the lowest boiling point will distill over first.
2. The vapors of liquid with higher boiling points condense along the
fractionating column and fall back into the round-bottomed flask.
Fractional Distillation of water and acetone

1. Acetone vapour and water vapour rises up the column as solution is heated.

2. The water vapour condenses in the fractionating column and falls back into
the flask.

3. Acetone, which has a lower boiling point than water, reaches the upper part
of the column and is distilled over.

4. At this stage, the temperature shows a constant temperature, which is the

boiling point of Acetone.

5. In the condenser,
1) Hot Acetone vapour condenses as running water cools it.
2) Liquid Acetone flows down the inner tube of the condenser and into the
receiver (a conical flask).

6. Acetone is collected as the distillate in the receiver.

Sublimation

Principle: The direct conversion of a solid into a gas upon heating and a gas into a
solid upon cooling without converting into a liquid form is known as sublimation.
Such a substance is known as sublime.

Purification of Impure Iodine

Chromatography
From a greek word
1. Chroma means color
2. Graphy means picture
Principle: Separation of Dyes/Colors from each other according to their solubility
in the given solvent.
e.g. Paper Chromatography

Paper Chromatography

This technique is used to separate substances that 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. 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 travels up the paper by capillary action, taking some of the coloured
substances with it.

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.

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

Interpret Simple Chromatograms

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.

An impure substance will show up with more than one spot, a pure substance
should only show up with one spot.
 Analysis of the composition of ink using paper chromatography

Importance of Purity

A pure substance consists of only one substance and contains nothing else.

To have a pure substance for food and drugs is very important as impurities could be
dangerous even in small amounts.

Melting and boiling point analysis is routinely used to assess the purity of food and
drugs.

For example, if a sample of water melts at exactly 0°C and boils at exactly 100°C then
the water is pure.

If the melting and boiling points of the water aren’t these exact values then the water
must be impure and contain other substances i.e. it must be a mixture.
Retention Factor (Rf) Values

These values are used to identify the components of mixtures.

The Rf value 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

Retention factor = distance moved by compound ÷ distance moved by solvent.

The Rf value is a ratio and therefore has no units.

Using Rf values to identify components of a mixture

Locating Agents

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 invisible samples such as proteins.

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.
Applications of Chromatography

1. It is used to check the purity of a substance; always a pure substance gives one
spot on separation.

2. It is used to identify and separate poisonous food addictive or food colors which are
not recommended by WHO.

3. It is used to separate and identify even colorless compounds e.g. amino acid.
Protein is made up of colorless amino acids on separation they are not visible then
a locating agent (e.g. Ninhydrin solution) is sprayed on chromatogram due to which
different amino acids becomes visible with different colors which are then
compared with the standard chart of amino acids hence identified.

4. This technique is used by forensic scientists to investigate crimes, from the incident
place sample are collected which are then compared with the samples collected
from suspects if matching occurs then they reach to conclusion.

5. It is also used to identify poisonous insecticides which are not recommended by

WHO.

6. Various plants pigments (e.g. chlorophyll) can also be separated by this technique.