ANALYSIS OF COMPOUNDS
 Leibigs method
 Carbon and hydrogen are
detected by heating the
compound with copper(II) oxide.
 Carbon present in the compound
is oxidised to carbon dioxide
(tested with lime-water which
develops turbidity)
 hydrogen to water (tested with
anhydrous copper sulphate, which
turns blue)
C+ 2CuO ∆ 2 Cu+CO 2

→
 2 H +CuO ∆ Cu+ H 2 O
→ iron(II) sulphate and forms
 sodium hexacyanoferrate(II
C O2 +Ca(OH )2 →Ca CO3 ↓+ H 2 O
 thiocyanate decomposes to yield
5 H 2 O+Cu SO 4 (White ) →CuSO 4.5 H 2O ( Blue )
 Lassaignes test
 Nitrogen, sulphur, halogens and
phosphorus present in an organic
compound
 The elements present in the
compound are converted from
covalent form into the ionic form
by fusing the compound with
sodium metal.
 Na+C+ N ∆ NaCN
→
 2 Na+ S ∆ Na 2 S
→

Na+ X ∆ Na X (X =Cl , Br∨I )
→ presence of iodine.
 Cyanide, sulphide and halide of
sodium so formed on sodium
fusion are extracted from the
fused mass by boiling it with
distilled water
 This extract is known as sodium
fusion extract.
 Test for Nitrogen
 The sodium fusion extract is
boiled with iron(II) sulphate and
then acidified with concentrated
sulphuric acid
 The formation of Prussian blue
colour confirms the presence of
nitrogen
 Sodium cyanide first reacts with
On heating with concentrated
sulphuric acid some iron(II) ions
are oxidised to iron(III) ions
which react with sodium
hexacyanoferrate(II) to produce
iron(III) hexacyanoferrate(II)
(ferriferrocyanide) which is
Prussian blue in colour
 6 CN – + Fe2+¿ →¿ ¿
 3¿
 x H→2 O Fe 4 ¿
 Test for Sulphur
 The sodium fusion extract is
acidified with acetic acid and lead
acetate is added to it
 A black precipitate of lead
sulphide indicates the presence of
sulphur
 2– 2+¿→ PbS (Black )¿
S + Pb
 On treating sodium fusion extract
with sodium nitroprusside,
appearance of a violet colour
further indicates the presence of
sulphur
2–
 S +¿
 nitrogen and sulphur both are
present in an organic compound,
sodium thiocyanate is formed. It
gives blood red colour and no
Prussian blue since there are no
free cyanide ions
 Na+C+ N + S → NaSCN
–
 Fe3 +¿+S CN → ¿¿
 If sodium fusion is carried out
with excess of sodium, the
cyanide and sulphide.

NaSCN + 2 Na → NaCN + Na2 S
 Test for Halogens
 The sodium fusion extract is
acidified with nitric acid and then
treated with silver nitrate
 A white precipitate, soluble in
ammonium hydroxide shows the
presence of chlorine
 yellowish precipitate, sparingly
soluble in ammonium hydroxide
shows the presence of bromine
 yellow precipitate, insoluble in
ammonium hydroxide shows the
– +¿→ AgX ¿
 X + Ag
 X represents a halogen – Cl, Br or
I
 If nitrogen or sulphur is also
present in the compound, the
 ANALYSIS OF COMPOUNDS

sodium fusion extract is first
boiled with concentrated nitric
acid to decompose cyanide or
sulphide of sodium formed during
Lassaigne’s test.
 These ions would otherwise
interfere with silver nitrate test
for halogens
 Test for Phosphorus
 The compound is heated with an
oxidising agent (sodium
peroxide)
 The phosphorus present in the
compound is oxidised to
phosphate
 The solution is boiled with nitric  percentage of carbon =
acid and then treated with
ammonium molybdate.
 A yellow colouration or
precipitate indicates the presence
of phosphorus
  Nitrogen
Na3 P O4 +3 HN O3 → H 3 P O4 +3 NaN

H 3 P O 4+ 12 ( NH 4 ) 2 Mo O4 + 21 HN O3 → ( N H 4 ) 3 PO 4 .12 Mo O3 +21 N H 4 N O3 +12 H 2 O
 The mass of water produced is
determined by passing the
mixture through a weighed U-
tube containing anhydrous
calcium chloride
 Carbon dioxide is absorbed in
another U-tube containing
concentrated solution of
potassium hydroxide
 These tubes are connected in
series
increase in masses of calcium
chloride and potassium hydroxide
gives the amounts of water and
carbon dioxide
12 x m2 x 100
44 x m
 percentage of hydrogen =
2 x m2 x 100
18 x m
O3 methods
 Two
 Dumas maethod
 Kjeldahls method
 Dumas method
solution of potassium hydroxide
which absorbs carbon dioxide.
 Traces of nitrogen oxides formed,
if any, are reduced to nitrogen by
passing the gaseous mixture over
a heated copper gauze
( P−P1 ) P2 V 2
 =
T1 T2
 P = pressure of moist gas
 P1 = pressure due to water vapour
 P – P1 = pressure of dry gas
 V1 = vol of gas in ml
 T1 = Temperature of gas in K
 P2 = pressure of gas at STP
 T2 = 273 K
 V2 = vol of nitrogen at STP
 Percentage of nitrogen =
28 x V 2 (STP) x 100
22400 x m
 Kjeldahs method
 The compound containing
nitrogen is heated with
concentrated sulphuric acid.
 Nitrogen in the compound gets
converted to ammonium sulphate

 Quantitative analysis  The nitrogen containing organic  acid mixture is then heated with
compound, when heated with excess of sodium hydroxide
 A known mass of an organic
compound is burnt in the
copper oxide in an atmosphere of  The liberated ammonia gas is
carbon dioxide, yields free absorbed in an excess of standard
presence of excess of oxygen and
nitrogen in addition to carbon solution of sulphuric acid.
copper(II) oxide
dioxide and water 
The amount of ammonia
 Carbon and hydrogen in the
 produced is determined by
compound are oxidised to carbon
dioxide and water ( y
2 ) (
y estimatingZ the amount of y
C X H Y N Z + 2 X + CuO → XC O2+ H 2 O+ N 2 + 2 X + Cu
2 sulphuric2acid consumed 2in the )

 The mixture of gases so produced reaction.
C X H Y +(x + y /4)O2 → x C O2+( y /2)H 2 O
is collected over an aqueous
 ANALYSIS OF COMPOUNDS

 It is done by estimating unreacted  adding magnesia mixture which

sulphuric acid left after the org comp AgN O3 AgCl aq N H 3 solubleon ignition yields Mg2P2O7
→ →
absorption of ammonia by 

titrating it with standard alkali org comp MgS O 4 , N H 3 Mg ¿
org comp AgN O3 AgBr aq N H 3 sparingly soluble →
solution → →

org comp H 2 S O4 , CuS O4 ¿ 

  Percentage of P =
→ org comp AgN O3 AgI aq N H 3 insoluble
 N H 3 + H 2 S O4 → ¿
 Kjeldahl method is not applicable
to compounds containing
nitrogen in nitro and azo groups
and nitrogen present in the ring
(E.g. pyridine) as nitrogen of
these compounds does not change
to ammonium sulphate
 Percentage of nitrogen =
1.4 x V (¿ ml)x N
m
N -normality
 Carius method
 Halogens
 A known mass of an organic
compound is heated with fuming
nitric acid in the presence of
silver nitrate contained in a hard
glass tube known as Carius tube
in a furnace
 Carbon and hydrogen present in
the compound are oxidised to
carbon dioxide and water
 The halogen present forms the
corresponding silver halide
(AgX). It is filtered, washed,
dried and weighed
 Percentage of halogen =
at mass of X x m1 x 100
mass of AgX x m
→ →
 Atomic weight
 Iodine = 127 
 Bromine = 80 H 3 P O 4+ 12 ( NH 4 ) 2 Mo O4 + 21 HN O3 → ( N H 4
 Ba = 137
 Ag = 108
 Sulphur
 A known mass of an organic
compound is heated in a Carius
tube with sodium peroxide or
fuming nitric acid.
 Sulphur present in the compound
is oxidised to sulphuric acid
 It is precipitated as barium
sulphate by adding excess of
barium chloride solution in water
 Percentage of sulphur =
32 x m2 x 100
233 x m
 Phosphoprus
 A known mass of an organic
compound is heated with fuming
nitric acid whereupon phosphorus
present in the compound is
oxidised to phosphoric acid
 It is precipitated as ammonium
phosphomolybdate, (NH4)3
PO4.12MoO3, by adding ammonia
and ammonium molybdate.
 phosphoric acid may be
precipitated as MgNH4PO4 by
62 x m2 x 100
222 x m
 Percentage of P =
31 x m2 x 100
1877 x m
 Oxygen
 The percentage of oxygen in an
organic compound is usually
found by difference between the
total percentage composition
(100) and the sum of the
percentages of all other elements
 A definite mass of an organic
compound is decomposed by
heating in a stream of nitrogen
gas.
 The mixture of gaseous products
containing oxygen is passed over
red-hot coke when all the oxygen
is converted to carbon monoxide.
 This mixture is passed through
warm iodine pentoxide (I2O5)
when carbon monoxide is
oxidised to carbon dioxide
producing iodine
 2 C+O2 1373 2CO
→
I 2 O5 +5 CO → I 2 +5 C O2

 ANALYSIS OF COMPOUNDS

 Percentage of oxygen
32 x m2 x 100
¿
88 x m
 The percentage of oxygen can be
derived from the amount of
iodine produced also
 The elements, carbon, hydrogen
and nitrogen present in a
compound are determined by an
apparatus known as CHN
elemental analyse
 The analyser requires only a very
small amount of the substance (1-
3 mg) and displays the values on
a screen within a short time.
 Layers Test – bromine
 Beilsteins Test – halogen