Organic Qualitative Analysis

Experim
Observation Inference
ent
Sugars, amine salts, amides,
1state Liquid imides, aniiides and amino
acids absent
2. Colour i. Yellow May be nitro compound
ii. Dark brown May be amino compound
iii. Red May be phenol
i. Pleasant May be alcohol, ester, ether,
3. Odour
smelling ketone or aldehyde
ii. Ammonical
May be aliphatic amine
or fishy
iii. Aniline like May be aromatic amine
iv. Phenolic May be phenol
v. Nitrobenzene
Nitro compound
like
 DETECTION OF ELEMENTS
A small place of freshly cut sodium was taken in
a dry sodium fusion tube and heated it gently
over the flame till it metals. Dropped a little of
the unknown into the tube, heated it strongly to
red-hot and plunged it while hot into 5 ml of
distilled water contained in a China-dish. Boiled
the contents for a minute or two and filter. With
the clear filtrate the following testes were done:
(a) To
0.5 ml of the extract 3-4
drops of a dil. Freshly Deep violet Sulphur present
prepared solutions of
sodium prusside was added

(b) To 0.5 ml of the

extract, few crystals of
ferrous sulphate was added Blue or green colour or Nitrogen present
and was heated to boil dil. precipitate
H2SO4 was added
(i) A crudy white
Chlorine present
(c) To 0.5 ml of the extract, precipitate
equal (3 drops) volume of (ii) A pale yellow
dil. HNO3 was added. precipitate of AgBr
sparingly soluble in Bromine present
Boiled for a minute and NH4OH
then it was cooled. Silver
nitrate solution was added (iii) A lemon yellow
to it. precipitate of Agl Iodine present
insoluble in NH4OH
SOLUBILITY TEST
 Soluble in Sugar, amino
(i) Solubility in water and salt an amide
H2O insoluble in like urea,
ether thiourea
Soluble in HCl
Basic substance
(ii) Solubility in and
like amino
5% dilute HCl regenerated in
compound
dil NaOH
Soluble in
Acidic
(iii) Solubility in NaOH and
substance like
5% NaOH regenerated in
carboxic acid
dil HCl
To 1 ml of 5%
solution of NaHCO3, Substance reacts Strongly acidic
0.2 g of the giving effervescence substance
unknown was added
TEST FOR AROMATIC NATURE

Burns with
a non sooty Aliphatic
flame
The unknown of 0.01 g was

taken in a Nickel spoon and

Burns with
a sooty Aromatic
burned
flame
TEST FOR SUGERS
a. Molish Test
To 1 ml of an aq. solution of the
unknown, few drops of an alc.
solution of a-napthol was added. The
test tube was immersed in a beaker of Violet ring Sugar
water. 1 ml of conc. H2SO4 was
slowly poured down the sides of the
test tube.
b. Barfoed’s Test
To 0.5 ml of the Barfoed reagent, the
solution of the unknown in water A red ppt.
Monosaccharide
was added and warmed on a water within 5 min
bath
Tollen’s Test
To 0.5 ml of AgNO3 solution, 2-
3 drops of dilute NaOH was
added. The brown ppt was
dissolved in a minimum amount
of dilute NH4OH. To the Tollen’s Appearance of Reducing sugar present
silver mirror
reagent so prepared a small
amount of unknown dissolved in
H2O or EtOH and was added
and warmed on a water bath
 TEST FOR PHENOLS
a. FaCl3 Test
(i) Purple, blue or
0.02/drop of unknown was dissolved in 5 ml green color other Phenol groups
than yellow
of H2O. A drop of neutral FeCl3 solution was
(ii) White ppt. Napthol
added

Dissolved 0.02 g in 3cc of dil. NaOH, a few Blue liquid Napthol alpha or
drops of CHCl3 and warmed gently changing to green
beta-napthol
or brown
b. Phthalein fusion test
To 0.02 g of the unknown mixed with 0.02 g
of phthalic anhydride, a drop of conc. H2SO4 A blue purple,
green or red
was added and warmed for a minute. To this colour intense Some phenols
mixture, a large volume of water alkalified green fluorescence
with dil. NaOH was added.
 16. Test of esters

Test for Dicarboxylic acids

Phthalein test
To 0.02 g of the unknown, 0.02 g
of resorcinol was mixed, a drop of
conc. H2SO4 was added to it
warmed for a minute. Few drops of
this was added to a large volume of Intense green Ortho or dicarboxylic
water, alkalified with dil. NaOH fluorescence acids

Warmed for a minute. Few drops

of this was added to a large volume
of water alkalified with dil. NaOH
TEST FOR ALDEHYDES AND KETONES
a. Borsche’s Test
To 2 ml of the Borsche’s reagent, few
drops of the unknown was added, then Orange or yellow Aldehyde or
dissolved in EtOH or H2O. Heated to coloured ketones
precipitate groups
boil and cooled finally
b. Tollen’s Test
To 0.5 ml of AgNO3 solution, 2-3 drops
of dilute NaOH was added. The brown
ppt was dissolved in a minimum
amount of dilute NH4OH. To the Appearance of Addehyde
Tollen’s reagent so prepared a small silver mirror group present
amount of unknown dissolved in H2O
or EtOH and was added and warmed
on a water bath
c. Schiff’s test
Instantaneous
To the unknown dissolved in EtOH or pink coloration Aldehyde
H2O, Schiff’s reagent was added i.e., within 20 group present
seconds
 Test of esters
a) To 2 drops of the unknown dissolved
EtOH was added along with hydroxyl
amine hydrochloride in methanol
Ester groups
Then equal volume of NaOH was added. Violet colour present
Boiled for a minute and cooled. Acidified
with excess of conc. HCl and 2 drops of
FeCl3 was added

Smell of the
b) 0.1 g of the unknown was refluxed with substance
disappears on Ester group
3 CC of 20% NaOH for 3 mins after acidification with confirmed
adding 2-3 drops of EtOH. conc. HCl a solid
acid separates
TEST FOR AMINES
(a) Carbylamine reaction:
Aliphatic or aromatic
A trace of the unknown was heated with a drop
Offensive odour primary amino group
present
of dil. HCl and few drops of dil. NaOH

Dye Test for amines

b) Reaction with HNO2

(1) Few drops of
solution when
Aromatic primary
added to beta-
amino group present
naphthol in NaOH
0.2 g of the unknown was dissolved in dil. HCl, gives a red ppt. (dye)
(2) A yellowish
cooled in ice water and was slowly added a few sweet smelling oil Secondary amine
or solid is formed
drops of saturated NaNO2 solution and a few (nitrosoamine)
(3) Yellow or
orange colour
drops of NaNO2 solution was added slowly
produced on adding
Tertiary aromtic amine
excess NaOH gives
a deep green colour
or precipitate
. Test for anilides (For neutral solids)

0.1 g of the unknown was refluxed with

A red dye
was Anilide
3 ml of 1:1 HCl for 3 min and cooled in
obtained
ice water and dye test was performed

Test for nitro compounds

a) Barker-Mulliken test
0.5 ml of an alc. solution of unknown
was boiled with a pinch of Zn dust and 1 Immediate
ml of aq. NH4Cl filtered the mixture Nitro group
black
present
Few drops of the filtrate was added in to precipitate
Tollen’s reagent (1) ml
Test for alcohols

a) Action with sodium

To a few drops of the dry unknown 1

Brisk and
continuous Alcohols
ml of dry a benzene a piece of Na was
efferverscene
added

b) Reaction with CH3COCl

Reaction take
To 0.1 g of the unknown, few drops of place with
production of
CH3 COCl was added. heat

The above mixture was warmed gently

for a minute, and poured into dil. Fragrant smell Alcohols

Na2CO3
. Test for Ethers and Hydrocarbons

a) Solubility in cold conc. H2SO4

Ether or unsaturated
(i) Soluble in cold
A little of the substance was shaken with cold compound
(ii) Insoluble in
conc. H2SO4 in a dry test tube Hydrocarbon
cold

b) Iodine test for a ethers

A little of the unknown was added to 1 ml of a Violet of the soln

change to tan Ether
colour
little purple solution of iodine in CS2

c) Test for polynuclear hydrocarbons

0.02 of the unknown was strongly heated with

a little anhydrous AlCl3 in a dry test tube, till a Blue or bluish Ploynuclear
colour hydrocarbon
sublimate was formed. Conc. H2SO4 was added

when cold the sides of the test tube