Chapter # 02 (Experimental Techniques in Chemistry) Prof.

Azam Rasool
Head of Chemistry Department

IMPORTANT TERMS

QUANTITATIVE ANALYSIS:
The type of analysis which determines the amount of various components in sample is
called quantitative analysis.

CRYSTALLIZATION:
It is the separation of a solid from solution by increasing its concentration above saturation
point in such a manner that excess of solid separates out in form of crystals on cooling.

GOOCH CRUCIBLE:
Filter crucible which is made up of porcelain having a perforated bottom which is covered
with a paper pulp or a filter paper cut to its size is called Gooch crucible.

PARTITION CHROMATOGRAPHY:
The type of chromatography in which stationary phase is a liquid is called partition
chromatography.

STATIONARY PHASE:
The part of chromatography over which mobile phase flows is called stationary phase.

MOBILE PHASE:
The part of chromatography that flows over stationary phase is called mobile phase.

CHROMATOGRAPHY:
It is an analytical separation method used for the separation of mixture due to their relative
affinities for the stationary and mobile phase.

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Chapter # 02 (Experimental Techniques in Chemistry) Prof.Azam Rasool
Head of Chemistry Department

Q: How many steps are involved in complete quantitative analysis? Write them.
Ans: A complete quantitative analysis involves the following steps
i. Obtaining a sample
ii. Separation of desired constituent
iii. Measurement and calculations of results
iv. Drawing the conclusion

Q. Concentrated HCl and KMnO4 solutions cannot be filtered by Gooch crucible. Give reason.
Ans: REASON:
Concentrated HCl and KMnO4 solutions are highly reactive and cannot be filtered by
using Gooch crucible because they react with filter paper. For this purpose, perforations are
covered with asbestos mate.

Q. What is Filtration?
Ans: “The process of separation of insoluble solid particles from liquids by passing
them through a filter medium is called as filtration.”

Q. What is fluted filter paper?

Ans: Ordinary filter paper is folded in such a way that a fan like arrangement is obtained.
PURPOSE:
It is used to increase the rate of filtration.

Q. How does a Gooch crucible increase the rate of filtration?

Ans: GOOCH CRUCIBLE:
Gooch crucible is made of porcelain. It has perforated base covered with a piece of
filter paper or asbestos mate. The rate of filtration can be increased if Gooch crucible is placed
in a suction of filtering apparatus. In this way, Gooch crucible increases rate of filtration.

Q. Differentiate between Gooch crucible and sintered glass crucible.

Ans: DIFFERENCE BETWEEN GOOCH CRUCIBLE AND SINTERED GLASS CRUCIBLE:
GOOCH CRUCIBLE SINTERED GLASS CRUCIBLE
It is made of porcelain. It is made of glass.
It has porous base covered with filter It has sintered glass disc sealed into its
paper or asbestos mat. bottom.
Reactive materials can’t be filtered easily. Reactive materials can be filtered easily.

Q. Why is there a need to crystallize the crude product?

Ans: REASON:

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Chapter # 02 (Experimental Techniques in Chemistry) Prof.Azam Rasool
Head of Chemistry Department

When a solid substance is produced during a chemical reaction, it always contains

impurities. To obtain pure solid compound, crude product is crystallized from a suitable
solvent.

Q. Which solvents are mostly used for crystallization?

Ans: SOLVENTS USED FOR CRYTALLIZATION:
The following solvents are mostly commonly used
i. Rectified spirit
ii. Ether
iii. CCl4
iv. Acetone
v. Water

Q. Write down the main characteristics of a solvent selected for crystallization of a

compound. OR
What do you mean choice of solvent?
Ans: CHARACTERISTICS:
The main properties of solvent are as follows
i. It should be inexpensive.
ii. It should be safe to use.
iii. It should not react chemically with solute.
iv. It should be easily removable.

Q. Mention the major steps in crystallization.

Ans: STEPS OF CRYSTALLIZATION:
The steps of crystallization are as follows
 Choice of solvent
 Preparation of saturated solution
 Filtration
 Cooling
 Collecting and washing of crystals
 Drying crystalline substance
 Decolourization

Q. How the decolourization of undesirable colours is carried out for freshly prepared
crystalline substances?
Ans: DECOLOURIZATION OF CRYTALS:
The decolourization of undesirable colours is carried out by boiling the substances with
sufficient amount of animal charcoal. The animal charcoal adsorbs all desirable colours and
pure crystalline substance is obtained.
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Chapter # 02 (Experimental Techniques in Chemistry) Prof.Azam Rasool
Head of Chemistry Department

Q. In solvent extraction technique, why repeated extraction using small portions of solvent
are more efficient than using a single extraction but lager volume of solvent?
Ans: REASON:
It is due to constant value of distribution coefficient which is equilibrium concentration
of solute in two solvent independent of amount of solvent.
Thus, if repeated extraction are used, then, equilibrium is established many times, so, more
amount of substance will be obtained. While in single extraction, equilibrium is established
only once. So, repeated extraction with small solvent is useful than single with large solvent.

Q. How desiccator is useful for drying crystals?

OR
Explain safe and reliable method of drying the crystals?
Ans: DESICCAOR:
The prepared crystals are wet and they need drying, In a desiccator, the crystals are
spread on watch glass and placed in a desiccator for several hours.
DRYING AGENTS:
The drying agents like CaCl2, silica gel or P2O5 are used. They don`t damage crystals.
That is why they are useful.

Q. Define sublimation with examples.

Ans: SUBLIMATION:
“The vaporization of a solid on heating directly into vapours without passing through
liquid phase is called sublimation.”
EXAMPLES:
For example, naphthalene, iodine and benzoic acid show sublimation.

Q: What do you mean by solvent extraction?

Ans: According to this technique 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.
Example: Ether extraction is the most common example.

Q. What is distribution coefficient? To which technique it is applicable?

Ans: DISTRIBUTION COEFFICIENT (kD):
“Distribution coefficient is defined as the ratio of concentration of a solute in the
organic phase to concentration of that solute in aqueous phase.”

Concentration of a solute in the organic phase

KD =
Concentration of that solute in aqueous phase

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Chapter # 02 (Experimental Techniques in Chemistry) Prof.Azam Rasool
Head of Chemistry Department

It is applicable to solvent extraction.

Q. Define Distribution law?

Ans: A solute distributes itself between two immiscible liquids in a constant ratio of
concentration independent of the amount of solute added.

Q. Differentiate between stationary phase and mobile phase.

Ans: DIFFERENCE BETWEEN STATIONARY & MOBILE PHASE:

STATIONARY PHASE MOBILE PHASE

The phase over which mobile phase
flows. It may be a liquid or a solid
supported on the surface of an inert
solvent.
Example: Silica gel, water adsorbed
in paper etc.
Mobile phase flowing over the
surface of stationary phase may be a
liquid or a gas.
Example: Acetone, Hexane etc.

Q. What is Rf value? Give its units.

Ans: Rf VALUE:
“It is defined as the ratio of distance travelled by components from original spot to
distance travelled by solvent from original spot.”

Rf = 𝑫𝒊𝒔𝒕𝒂𝒏𝒄𝒆 𝒕𝒓𝒂𝒗𝒆𝒍𝒍𝒆𝒅 𝒃𝒚 𝒂 𝒄𝒐𝒎𝒑𝒐𝒏𝒆𝒏𝒕 𝒇𝒓𝒐𝒎 𝒐𝒓𝒊𝒈𝒊𝒏𝒂𝒍 𝒔𝒑𝒐𝒕

𝑫𝒊𝒔𝒕𝒂𝒏𝒄𝒆 𝒕𝒓𝒂𝒗𝒆𝒍𝒍𝒆𝒅 𝒃𝒚 𝒕𝒉𝒆 𝒔𝒐𝒍𝒗𝒆𝒏𝒕 𝒇𝒓𝒐𝒎 𝒐𝒓𝒊𝒈𝒊𝒏𝒂𝒍 𝒔𝒐𝒑𝒕
UNIT:
It has no unit because it is ratio between two same quantities.

Q. Differentiate between Adsorption and Partition chromatography.

OR
What are classes of chromatography?
Ans: DIFFERENCE BETWEEN ADSORPTION AND PARTITION CHROMATOGRPHY:

ADSORPTION CHROMATOGRPHY PARTITION CHROMATOGRPHY

In adsorption chromatography stationary In partition chromatography, stationary
phase is solid. phase is liquid.
Example: Thin layer chromatography Example: Paper chromatography.
(T.L.C).

Q. Give the main uses of paper chromatography.

Ans: APPLICATIONS OF PAPER CHROMATOGRAPHY:
Following are uses of paper chromatography
i. It is used to identify the different amino acids.
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Chapter # 02 (Experimental Techniques in Chemistry) Prof.Azam Rasool
Head of Chemistry Department

ii. It is used for separation and identification of coloured pigments.

iii. It separates mixture of very small quantities ay very low concentration.
iv. It is equally important in quantitative and qualitative analysis.

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