CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY

LECTURE NO. 1
PREVIEW OF TODAY’S TOPICS
 Analytical Chemistry  Filtration  Crystallization
 Sublimation
LONG QUESTION
Why there is a need to crystallize crude product? Explain crystallization process. (K.B)
SHORT QUESTIONS
• How chemical characterization of a compound is done (LHR 2019-K.B)
• Draw the beautiful diagram of sublimation process (LHR 2021-K.B)
ANALYTICAL CHEMISTRY
Definition:
Deals with chemical characterization of a substance.
Qualitative Analysis
Identification of elements present in a compound e.g. elemental analysis.
Quantitative Analysis
Determination of relative amount of each element present in a compound e.g combustion analysis.
Main steps in Quantitative Analysis:
1. Obtaining a sample for analysis:
A minute amount of substance is taken as a sample.
2. Separation of desired component:
The component whose analysis is to be carried out is separated from the sample.
3. Measurement and calculation of the result:
Then the amount of the main component is estimated by particular quantitative technique.
4. Drawing conclusion from analysis:
The experimental values are interpreted in the form of observations, calculations and results.
FILTRATION
Definition:
The separation of insoluble particles (precipitates) from the liquid by passing mixture through a
filter medium.
• Filter Medium: Porous medium such as filter paper/crucibles.
• Selection of Filter Medium: Depends upon precipitate size.
• Filteration through Filter Paper
1. Process of filtration
2. Variety of filter Papers (Porosity of filter paper)
3. Size of filter paper
4. Size of funnel
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 CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY
5. Smooth filtration
6. Folding of filter paper
7. Gentle suction for filtration
8. Fluted filter paper (Increase in rate of filtration)
• Filteration through Filter Crucibles
(a) Gooch Crucible:
1. Composition:
Made up of porcelain, perforated bottom covered with paper pulp, filter paper or asbestos
mat cut to its size.
2. Advantage: Quick Filtration
(b) Sintered Glass Crucible:
(i) Composition: Made up of glass, porous glass disc sealed into its bottom.
(ii) Advantage:
• No preparation is needed as with the Gooch crucible.
• The process is very smooth and time saving.
CRYSTALLIZATION
Definition:
The formation of crystals of a substance when it’s hot saturated solution is cooled moderately.
• Objective of Crystallization: To purify a crude product.
• Principle
The solute should be soluble in a suitable solvent at high temperature and the excess amount of
the solute is thrown out as crystals when it is cooled.
• Steps of Crystallization
1. Choice of solvent
2. Preparation of saturated solution
3. Filtration (if impurities are insoluble)
4. Cooling
5. Collecting the crystals
6. Drying of the crystallized substance
7. Decolourization of undesirable colours
SUBLIMATION
Definition:
The direct conversion of solid into gas on heating without passing through liquid phase.
e.g. Sublimeable (sublimands) solids are iodine, ammonium chloride, naphthalene an benzoic
acid

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 CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY
MULTIPLE CHOICE QUESTIONS
1. During the process of crystallization the hot saturated solution is (GRW 2021 K.B)
a) Cooled at moderate rate to get medium sized crystals
b) Cooled very slowly to get large sized crystals
c) Evaporated to get the crystals of the product
d) Mixed with an immiscible liquid to get the pure crystals of the product
2. Which one of the following compound is purified by sublimation (LHR 2019, 22-K.B)
a) Benzoic acid b) SiO2
c) CS2 d) NaI
3. Which of the following compounds do not show process of sublimation (LHR 2021-K.B)
a) Ammonium chloride b) Iodine
c) Naphthalene d) Carbon tetra chloride
4. One of the following substances does not undergo sublimation (LHR 2022-U.B)
a) Ammonium chloride b) Naphthalene
c) Iodine d) Mercury Repeated extractions using
5. small portion of solvent are more (U.B)
a) Accurate b) Efficient
c) Slow d) Rapid
SHORT QUESTIONS
1. Why is there need to crystallize a crude product? (MTN 2019-U.B)
Ans: Crystallization is performed to purify the crude product that has many soluble and
insoluble impurities in it. The insoluble impurities of the product are removed by filtration
process. But the soluble impurities of the product can be removed by crystallization.
Crystallization is a purification technique. Crude product is crystallized to remove the soluble
impurities. These impurities will remain in the mother liquor. The liquid which remains after
crystallization is called mother liquor.
2. Explain safe and reliable method for drying of crystals. (MTN 2022-K.B)
Ans: When crystals are dried with filter paper, they may be crushed and contaminated. In
oven, we cannot avoid decomposition or melting of crystal. A safe and reliable method of drying
crystals is through a vacuum desiccator. In this process, the crystals are spread over a watch glass
and kept in a vacuum desiccator for several hours with a drying agent. The drying agents used in
a desiccator are CaCl2, silica gel and P2O5.

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 CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY
LECTURE NO. 2
PREVIEW OF TODAY’S TOPICS
 Solvent Extraction  Chromatography
LONG QUESTION
Define and explain paper chromatography in a brief way? (K.B)
SHORT QUESTIONS
• Differentiate between stationary and mobile phase (GRW 2021, DGK 2022-U.B)
• Differentiate between adsorption and partition chromatography?
(GRW 2018,19, FSD 2022-U.B)
SOLVENT EXTRACTION
Definition:
Separation of a solute from a solution by shaking it with an immiscible solvent in which the
solute is more soluble.
• Solvent Extraction is done for:
Separation of organic compounds from water.
Separation of compound from aqueous solution which is volatile or thermally unstable.
• Process:
1. Ether Extraction:
The process which is used to separate the product of organic synthesis from water.
2. Efficiency of the Process:
Repeated extractions using small portions of solvent are more efficient.
3. Distribution Law: (Partition Law)
“A solute distributes itself between two immiscible liquids in a constant ratio of concentration
irrespective of the amount of solute added.”
• Distribution of iodine between two immiscible solvents
The distribution of iodine between two immiscible solvents i.e.
Water in the presence of KI (Potassium iodide) and carbon tetrachloride (CCl4.)
1. Dynamic Equilibrium:
K + (aq) + I− (aq) I 2(s) + I − (aq) I3−(aq)
H2O
KI(s)
Soluble in CCl4 Soluble in water
2. Transfer of Iodine: From water (polar) to CCl4 (non polar) solvent
3. Change in Colour: Brown to Purple
4. Efficiency of the Process: Repeated extractions are more efficient
5. Distribution Constant (K): Shows ratio of solute in both phases
[I 2 (CCl4 )]
K=
[I3−(aq ) ]
CHROMATOGRAPHY
Definition:
Process used to separate the components of a mixture on the basis of their difference in relative
affinity with two phases i.e stationary and mobile phases.
1. Stationary Phase:
A solid or a liquid supported as a thin film on the surface of an inert solid.
2. Mobile Phase:
A liquid or gas that flows over the surface of the stationary phase.

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CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY
• Principle:
In chromatography, substances are separated due to their relative affinities for the stationary
phase and mobile phase. The distribution of the components of a mixture between the two phases
is governed by the distribution co-efficient (K)
• Distribution Co-efficient (K):
1. Smaller Value of K: More solute affinity with stationary phase
2. Greater Value of K: More solute affinity with mobile phase.
• Types of Chromatography (on the basis of stationary phase):
1. Adsorption Chromatography: Stationary phase is solid
2. Partition Chromatography: Stationary phase is liquid
• Paper Chromatography:
Technique in which the stationary phase is water adsorbed as thin film on paper and the mobile
phase is usually an organic liquid. Paper chromatography is a type of partition chromatography
• Types of Paper Chromatography (on the basis of direction of movement of mobile phase):
1. Ascending paper chromatography (mobile phase moves up)
2. Descending paper chromatography (mobile phase moves down)
3. Radial paper chromatography (mobile phase moves in circular fashion)
• Ascending Paper Chromatography
In this technique, the solvent is in a pool at the bottom of a vessel in which the paper is supported
and the solvent travels upwards by the capillary action.
• Apparatus and process
1. Chromatographic Tan
2. Wattmann’s Chromatographic Paper
3. Suspending the Paper
4. Upward Movement of Solute
5. Removing the Strip
6. Chromatogram
7. Retardation Factor
Distance travelled by a component from original spot
Rf =
Distacne travelled by solvent from original spot
x
R f (B) =
y
z
R f (C) =
y
8. Identification of Components
• Units of Rf (Retardation factor) = No unit
• Uses of Chromatography:
1. Qualitative as well as quantitative analytical technique.
2. Isolation of products
3. Determination of the purity of a substance.
4. Identification of components of mixture like mixture of inks, mixture of amino acids etc.
5. Separation of components

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 CHAPTER 2 ANALYTICAL TECHNIQUES IN CHEMISTRY
MULTIPLE CHOICE QUESTIONS
1. Solvent extraction is an equilibrium process and is controlled by
(GRW 2019, 21 LHR 2018, 21, MTN 2022 RWP 2022-K.B)
a) Law of mass action b) The amount of solvent used
c) Distribution law d) The amount of solute
2. Solvent extraction method is particularly useful technique for separation, when the
product to be separated is (LHR 2022, SGD 2019, RWP 2019-U.B)
a) Non-volatile or thermally unstable b) Volatile or thermally stable
c) Non-volatile or thermally stable d) Volatile or thermally unstable
3. The comparative rates at which the solutes move in paper chromatography, depend on
(GRW 2018, 21, FSD, 2019, SGD 2019, DGK 2022, MTN 2022, SWL 2022, -K.B)
a) The size of paper b) Rf values of solutes
c) Temperature of the experiment d) Size of the chromatographic tank used
4. Solvent extraction is an equilibrium process an it is controlled by (FSD 2021-U.B)
a) Thin layer chromatography b) Partition chromatography
c) Absorption chromatography d) Gel chromatography
5. The chromatography in which stationary phase is liquid is called (LHR 2018-U.B)
a) Thin layer chromatography b) Partition chromatography
c) Absorption chromatography d) Gel chromatography
SHORT QUESTIONS
1. What is Rf value? Why it has no units? (BWP 2022, DGK 2022-K.B)
Ans: Each component has specific retardation factor which depends upon its distribution
coefficient and is called Rf value. It is given by.
Distance travelled by a component from the orignal spot
Rf =
Distance travelled by solvent from the orignal spot
It has no unit because it is ratio of two distances.
2. What is ether extraction? (LHR 2019, 21 MTN 2022-K.B)
Ans: Ether extraction:
The most common laboratory example of solvent extraction is ether extraction.
Process:
• In a typical organic synthesis, the aqueous solution containing the organic product is taken up
with ether in a separating funnel and allowed to separate.
• The inorganic impurities remain in aqueous phase while the organic compound goes to the
ether layer. The ether layer is separated out and the organic product is obtained by
evaporating the ether.
Efficiency of the process:
Repeated extractions using small portions of solvent are more efficient than using a single but
larger volume of solvent.

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