QUALITATIVE AND

QUANTITATIVE ANALYSIS OF
ORGANIC COMPOUND
 QUALITATIVE ANALYSIS OF ORGANIC COMPOUND

Qualitative analysis : Detection of element present in compound

(a)
(b) Detection of Nitrogen, Sulphur and Halogen :- [Lassaigne's Test]
Preparation of lassaigne's solution or sodium fusion extract:
Nitrogen, sulphur and halogens present in an organic compound are detected by “Lassaigne’s
test”. The elements present in the compound are converted from covalent form into the ionic
form by fusing the compound with sodium metal. Following reactions take place:

C, N, S and X come from organic compound.

NaSCN
But if Na taken in excess then NaCN and Na2S is formed
 NaSCN

3 NaSCN Fe(SCN)3

NaSCN
ppt
Quantitative analysis
 QUANTITATIVE ANALYSIS OF ORGANIC COMPOUND

Quantitative analysis : Calculation of precentage of element in compound.

Estimation of carbon and hydrogen: [Liebig’s method]

Calculation of % of C and H :-
Carbon and Hydrogen If mass of organic compound is W gm.
of organic compound mass of H2O or CO2 produced is m gm
are converted into
For H H2O  2H
CO2 and H2O
18 2
 18 gm of H2O contains 2 gm of hydrogen
 1 gm of H2O contains 2 gm of hydrogen
18
 m gm of H2O contains 2 × m gm of hydrogen
18
2 m
Precentage of hydrogen in W gm organic substance = % of H =   100
18 W
 Q.1 0.3960 gm of an organic compound on combustion gives 0.792 gm CO2 and
0.324 gm of H2O. Calculate the % of C and H ?

12 Wt. of CO 2
Sol. % of C = × ×× 100
44 Wt. of compound

12 0 .7 92
= × × 100 = 54.55%
44 0.39 6

2 Wt. of H 2 O
% of H = × × 100
18 Wt. of compound

2 0.324
= × × 100 = 9.09%
18 0.396
Estimation of halogen : Carius Method

Halogen of organic compound

is converted into AgX (ppt.)

Estimation of sulphur : Carius Method

Sulphur is estimated in the

form of BaSO4.

Estimation of phosphorus : Carius Method

Phosphorus is estimated in
the form of magnesium
pyrophosphate (Mg2P2O7)
Q.
Q.
Estimation of Nitrogen : There are two methods for estimation of nitrogen:
(i) Dumas method [in form of N2]
(ii) Kjeldahl’s method [in form of NH3]

(i) Duma's method :

V1 = Volume of N2 gas.
P1 V1 P2 V2 Mentioned in question
= P1 = Pressure of N2 – Aqueous tension
T1 T2
T1 = Temperature
P1 V1  273
V2 =
T1  760 V2 - Volume of N2 at STP
P2 - 760mm of Hg
T2 - 273K
Calculation of % of Nitrogen

 22400 ml of N2 at STP weight = 28 gm

 V ml of N2 at STP weight = 28
 V gm
22400

28 V
% of Nitrogen in W gm organic substance = % of N =   100
22400 W

Applicable for all nitrogenous compounds

Q. 0.25 gm of an organic compound at NTP gives 31 ml of N2 gas by Duma's method. Find
out of % of N
 Q. 31.7 ml of moist N2 was obtained from 0.2033 gm of an organic compound in
Duma's method at 14°C and 758 mm pressure. If aq. tension at 14°C = 14 mm than
calculate % of N

Sol. P1 = Pressure of N2 – Aq. tension = 758 – 14 = 744 mm

P2 = 760 mm T2 = 273
V1 = 31.7
T1 = 273 + 14
T1 = 287K
P1 V1 273 744  31.7  273
V2 =  = = 29.51 = V ml
T1 760 287  760
 TRY YOURSELF (HOME WORK)
Q.

(NCERT)

Ans : 17.46 %
Kjeldahl method is not applicable to (ii) Kjeldahl's method : [in form of NH3]
• Compound containing nitrogen is heated with H2SO4 so compound
compounds containing nitrogen in
gets converted in to ammonium sulphate.
nitro, azo and azoxy groups and • Now above mixture is heated with excess of NaOH which liberates
nitrogen present in the ring (e.g. Ammonia gas.
• Ammonia gas is absorbed in excess of standard solution of H2SO4.
pyridine) as nitrogen of these
• The amount of ammonia produced is determined by estimating the
compounds does not change to amount of H2SO4 consumed.
ammonium sulphate under these • Estimation of H2SO4 is done by titrating the H2SO4 left after

conditions. absorption of ammonia with standard alkali solution.

• The difference between the initial amount of acid taken and that left
after absorption of ammonia is the amount of H 2SO4 used.

N1= N of H2SO4 , V1= Volume of H2SO4 (ml)

N2= N of NaOH, V2= Volume of NaOH (ml)
Q. 30 ml 0.25 N H2SO4 are used in neutralizing NH3 obtained from 0.75 gm of an organic
compound in Kjeldhal's method find out % of N in the compound
Q. In Kjeldhal's method, NH3 evolved from 0.25 gm of an organic compound was passed
into 30 ml N/2 H2SO4. 50 ml N/10 NaOH were required to neutralize the unreact acid,
calculate % of N.
Q.

(NCERT)
PURIFICATION OF
ORGANIC
COMPOUNDS
 SUBLIMATION

This method is used to separate sublimable

compounds from nonsublimable impurities.

Sublimation: On heating, some solid substances

change from solid to vapour state without passing
through liquid state.
Camphor, naphthalene, anthracene, benzoic acid,
phthalic anhydride are purified by sublimation.
 CRYSTALLISATION
It is based on the difference in the solubilities of the compound and the
impurities in a suitable solvent
The impure compound is dissolved in a solvent in which the compound that needs to be
purified is sparingly soluble at room temperature but appreciably soluble at higher
temperature and impurities highly soluble at all temperatures,
On cooling the solution, pure compound crystallises out and is removed by filtration
The filtrate (mother liquor) contains impurities and small quantity of the compound
 DISTILLATION

The vaporisation of a liquid by heating and subsequent condensation of

vapours by cooling is known as distillation.

1.Simple distillation
2.Fractional distillation
3.Distillation under reduced pressure (vacuum distillation)
4.Steam distillation
 SIMPLE DISTILLATION
This important method is used to separate
(i) volatile liquids from nonvolatile impurities and
(ii) the liquids having sufficient difference in their
boiling points

(C2H5OC2H5)
 FRACTIONAL DISTILLATION
If the difference in boiling points of two liquids is not much, simple distillation cannot be used to
separate them
FRACTIONAL DISTILATION is employed for separating two or more volatile liquids having boiling points close
to each other
 A- more volatile
B- less volatile
In vapour phase
A>50% B<50%
Suppose A=60%
B=40%
This vapour condensed into liquid
New liquid : A=60%
B=40%

In vapour phase
A>60% B<40%

Repeated again and again

DISTILLATION UNDER REDUCED PRESSURE
(VACUUM DISTILLATION)
This method is used to purify liquids having very high boiling points
and those, which decompose at or below their boiling points.

In this process a liquid is made to boil at a temperature lower than its

normal boiling point by reducing pressure.

Glycerol can be separated from spent-lye in

soap industry by using this technique
STEAM DISTILLATION
This technique is applied to separate
substances which are steam volatile and are
immiscible with water

1. Aniline is purified by steam distillation.

2. o-nitro phenol is purified by steam distillation.
The organic solvent is later removed by
distillation or by evaporation to get
back the compound.
 CHROMATOGRAPHY
❖ Chromatography is an important technique extensively used to separate mixtures into their
components, purify compounds and also to test the purity of compounds.

❖ In this technique, the mixture of

substances is applied onto a stationary
phase, which may be a solid or a liquid.
❖ A pure solvent, a mixture of solvents, or
a gas is allowed to move slowly over the
stationary phase. The components of
the mixture get gradually separated from
one another.
❖ The moving phase is called the mobile
phase.

Based on the principle involved, chromatography is classified into different categories. Two of these are:
(a) Adsorption chromatography, and
(b) Partition chromatography.
 Adsorption Chromatography

Adsorption chromatography is based on the fact that different compounds are adsorbed on an adsorbent to
different degrees.
Commonly used adsorbents are silica gel and alumina.
When a mobile phase is allowed to move over a stationary phase (adsorbent), the components of the
mixture move by varying distances over the stationary phase.

Following are two main types of chromatographic techniques based on the principle of differential
adsorption.
(i) Column chromatography, and
(ii) Thin layer chromatography.
(i) Column Chromatography:
➢ Column chromatography involves separation
of a mixture over a column of adsorbent
(stationary phase) packed in a glass tube.
The column is fitted with a stopcock at its
lower end .
➢ The mixture adsorbed on adsorbent is
placed on the top of the adsorbent column stronger interactions
packed in a glass tube.
➢ An appropriate eluant (Mobile phase) which
is a liquid or a mixture of liquids is allowed to weaker interactions
flow down the column slowly.
➢ Depending upon the degree to which the
compounds are adsorbed, complete
separation takes place.
➢ The most readily adsorbed substances are
retained near the top and others come down
to various distances in the column.
(ii) Thin Layer Chromatography
Thin layer chromatography (TLC) is another type of adsorption chromatography, which involves
separation of substances of a mixture over a thin layer of an adsorbent(silica gel or alumina) coated on
glass plate.

As the eluant(mobile phase) rises up the

plate, the components of the mixture move
up along with the eluant to different
distances depending on their degree of
adsorption and separation takes place

As solvent moves up

The relative adsorption of each component of the mixture is expressed in terms of its
retardation factor / retention factori.e. Rf value
Distance moved by the substance from base line (x)
Rf = Distance moved by the solvent from base line (y)
 PARTITION CHROMATOGRAPHY
Paper chromatography is a type of partition chromatography.
In paper chromatography, a special quality paper known as chromatography paper is used.
Chromatography paper contains water trapped in it, which acts as the stationary phase
SUMMARY ON CHROMATOGRAPHY