Introduction to Experimental Techniques

1. Analytical Chemistry:
The science of chemical characterization.

2. Analysis:
Complete chemical characterization include:
i. Qualitative Analysis:
The analysis in which
10/29/17 elements
Prof.Rana Hassan Tariqin a compounds are identified.
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ii. Quantitative Analysis:
The analysis in which relative amount of elements in compound
are estimated.
iii. Main Steps in Quantitative Analysis:
Obtaining sample for analysis.
Separation of desired component.
Measurement and calculation of result.
Drawing conclusion from analysis.

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3. Method of Purification:
Method of Purification Application
1. Filtration Separation of soluble and insoluble solids.

2. Evaporation Separation of a soluble solid from solution.

3. Crystallization Separation of solid by cooling either form solution of molten liquid.

4. Decanting and Separation by suspension.

Centrifuging
5. Simple distillation Separation of liquid from a solution.

6. Fractional distillation Separation of a fraction from mixture of miscible liquids.

7. Solvent Extraction Solvent extraction from solution.

8. Sublimation Separation of sublimant from solid mixture.

9. Chromatography
10/29/17 Separating colours,
Prof.Rana Hassandyes,
Tariq amino acids etc. 3
 Filtration

1. Definition:
Separation of insoluble particles from liquids.
2. Filter Media:
Method
Method ofof
filtration
filtration

Filtration
Filtration
Filtration
Filtration through
through
through
through filter
filter
filter
filter paper
paper crucibles
crucibles

Sintered
Sintered
Ordinary
Ordinary Fluted
Fluted filter
filter Gooch
Gooch glass
glass
10/29/17 filter
filter paper
paper paper crucible
Prof.Rana Hassancrucible
paper Tariq 4
crucible
crucible
i. Filtration through Filter Paper:
a. Through ordinary Filter Paper:
Solvent pass through leaving insoluble particles on filter paper.
Filter paper are classified on the basis of pores.
Filter paper should be filled with precipate upto 1 / 4 1 / 2.
Tip of stem should be in touch of beaker to avoid any splashing.

b. Through Fluted Filter Paper:

Fluted filter paper is obtained by folding ordinary filter paper in fan
like arrangement.
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ii. Filtration through Filter Crucibles:
i. Gooch Crucible:
It is made up of porcelain.
It has a porous base.
Its base covered with filter paper or asbestos mat.
Contamination of filter paper with crystals.
Reactive solution HCl, KMnO4 can be filtered by using asbestos mat.
ii. Sintered Glass Crucible:
It is made up of glass.
In its base sintered glass disc is sealed.
No need to cover base.
Reactive substance safely filtered.
No need of any alteration.
There is no contamination.
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 Crystallization

1. Definition:
Separation of solid as crystals when hot saturated solution is
cooled.

2. Principle of Crystallization:
At high temperature solute is soluble in solvent and excess
solute is crystallize out when
10/29/17 it isTariq
Prof.Rana Hassan cooled. 7
3. Steps of Crystallization:
i. Choice of Solvent:
Solvent is selected by hit and trial basis.
It should dissolve a large amount of the substance at its boiling
point and only a small amount at the room temperature.
It does not react with the solute.
It should either not dissolve the impurities or the impurities
should not crystallize from it along the solute.
On cooling it should deposit well formed crystal of the pure
compound.
It should be inexpensive.
It should be safe to use and should be easily removable.

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ii. Example of Solvent:

Water
Water Rectified
Rectified spirit
spirit Ethanol
Ethanol Diethyl
Diethyl ether
ether Acetone
Acetone

If one solvent is not suitable than combination of solvents are

used.
Water bath is used when solvent is inflammable.
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ii. Preparation of Saturated Solution:
The solute is dissolved in a minimum amount of solvent at its
boiling point to form saturated solution.

iii. Filtration:
Fluted filter paper or normal filter paper is for filtration.
Hot filtration avoid premature crystals.

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 iv. Cooling:
Medium size crystals = Moderate rate.
Large size crystals = Slow cooling.
Premature crystals = Rapid cooling.
v. Collection of Crystals:
Gooch crucible is used for the separation of crystals.
vi. Drying of Crystallize Substance:
Placing crystals between the folds of filter paper.
Heating crystals in oven.
Vacuum desiccator are used to dry crystals.
CaCl2, P2O5 and silica gel is used n desiccator to absorbed moisture.
CaCl2 is a hygroscopic
it adsorbs water, it changes color, going from blue to purple to pink as the moisture is adsorbed
1. Montmorillonite Clay. Montmorillonite clay is a naturally occurring adsorbent created by the controlled drying of magnesium aluminum silicate of the sub-bentonite type. ...

2. Silica Gel. Silica gel is silicon dioxide (SiO2). ...

3. Indicating Silica Gel. ...

4. Molecular Sieve. ...

5. Calcium Oxide. ...

6. Calcium Sulfate. ...

7. Other Adsorbents . 10/29/17 Prof.Rana Hassan Tariq 11

vii. Decolourization of undesirable Colours:
Colouring crystals are dissolve in solvent and
boiled.
Solvent contain animal charcoal absorbed colour.
The solution is filter in hot state.
Moderate cooling is carried out.
Crystals of pure substance will be separate out.

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 Sublimation

1. Definition:
The process in which a solid, when heated, vapourizes
directly without passing through the liquid phase.

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2. Examples:

Naphthalene Iodine Ammonium chloride Benzoic acid

Camphor Anthracene Anthraquinone Hexachloroethane

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 Solvent Extraction

1. Definition:
A solute can be separated from a solution by shaking the
solution with a solvent in which the solute is more soluble
and the added solvent does not mix with the solution.

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2. Distribution Law:
A solute distributes itself between two immiscible liquids in a
constant ratio of concentrations irrespective of the amount of
solute added.
3. Steps for Solvent Extraction:
Take a solution containing solute in a separating funnel.
Add small amount of an immiscible solvent.
Shake them well.
Separate the organic layer.
Evaporate the organic layer to get dried crystals.

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4. Key Points:
1.
Solvent extraction used to separate organic compound from
water.
Solvent extraction is a equilibrium process.
Ratio of final concentration at equilibrium is constant known
as distribution coefficient.
K

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 Introduction to Chromatography

1. Definition:
Technique used for the separation of components of mixture
which involves the distribution of a solute between stationary
phase and a mobile phase.

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2. Stationary Phase:
It may be solid or liquid.
It may be packed in a column.
It may be spreaded as a layer or distribution as a film.
Examples:
Silica gel.
Alumina.
3. Mobile Phase:
It is called eluent.
It flowing over the stationary phase.
It may be gas or liquid.
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1. Examples:
Water.
Ethanol.
Acetic acid.
Acetone
Gases.
4. Principle of Chromatography:
In chromatography substances are separated due to their
relative affinities for the two phases.
This distribution of components of a mixture between two
phase is distribution coefficient K.
K

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5. Types of Chromatography:
i. Adsorption Chromatography:
The chromatography in which stationary phase is solid.
The substance leave the mobile phase to become adsorbed on
the surface of solid phase.
Examples:
Column chromatography.
Thin layer chromatography (TLC).
ii. Partition Chromatography:
The chromatography in which stationary phase is liquid.
The substance being separated are distributed throughout both
the stationary and mobile phase.
Examples:
Paper chromatography.
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 Paper Chromatography

1. Introduction:
In 1944 Gordon and Martin introduce paper chromatography.
2. Ways of Paper Chromatography:
Ascending = solvent rises up.
Descending = solvent flows down.
Radial / Circular = solvent flows in circular fashion.

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1. i. Ascending Paper Chromatography:
The solvent travels upwards by capillary action.
Apparatus:
Chromatographic tank.
Sample (to be separated).
Whatmanns paper no 1.
Chromatogram:
Dried filter paper which contain coloured component of the mixture.
Solvent Front:
Distance travelled by solvent from original spot.
Rf Value:
It is retardation factor of each component of the mixture.
Rf
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3. Uses of Chromatography:
Separation and identification of coloured pigments.
Identification of medicines and proteins.
Analysis of urine.
Determination of purity of compound.
Used in organic synthesis for
Separation
Isolation
Purification
Equally important for quantitative and qualitative analysis.

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