Systematic Analysis of Anions (Acid Radicals)

Action of dil HCl: Brisk effervescence with the Gas evolved is CO2
1 About 1ml of dil. HCl is taken in the test tube and liberation of a colourless,
a small quantity of the salt is added. odourless gas.

The above gas is passed through lime water. Lime water turns milky. Presence of Carbonate confirmed.

Action of dil. H2SO4: Presence of acetate.

2 A little of the substance is rubbed with dil. Smell of Vinegar Vinegar smell is due to the formation of
H2SO4 and the smell is noted. acetic acid.

a) Colourless pungent gas fuming Gas evolved is HCl. Dense white fumes
in moist air, dense white fumes are due to the formation of NH4Cl.
Action of Conc. H2SO4: when glass rod dipped in NH4OH
About 10mg of the salt is warmed with 0.5ml of is introduced in the test tube. Presence of Chloride.
3 Conc H2SO4 in a dry boiling tube.

b) Reddish brown vapours on Gas evolved is NO2

heating Presence of Nitrate (NO2).

Action of Conc. H2SO4 and Copper turnings:

4 The salt is heated with Conc.H2SO4 and copper Dense reddish-brown fumes with Gas evolved is NO2. Presence
turnings. irritating smell. of Nitrate.

1
 Confirmatory Tests for Anions:
Confirmatory tests for anions are carried out by Sodium carbonate extract.
Preparation of Sodium Carbonate extract: (For insoluble salts) Sodium carbonate extract is prepared by boiling 1gm of the substance with
thrice its weight of anhydrous sodium carbonate and 20ml of water in a China dish for 10 minutes. It is then cooled and filtered. The filtrate
is called the Sodium Carbonate Extract.

The following tests are done with the sodium carbonate extract or by water extract.

1 For Chloride:
Silver Nitrate Test: White curdy ppt soluble in
Presence of chloride confirmed
A little of the extract is acidified with dil. HNO3. NH4OH
It is boiled to expel CO2 and cooled. A few drops
of silver nitrate added to the solution.

For Sulphate:
2 White precipitate insoluble in all
Presence of Sulphate confirmed
A little of the extract is acidified with dil. HCl. It mineral acids
is boiled and cooled and BaCl2 is added.
For Nitrate:
3
Brown Ring Test-
Extract is acidified with dil. H2SO4 and freshly A brown ring is formed in the
Presence of Nitrate confirmed
prepared FeSO4 sol. is added. Conc H2SO4 is junction of the two layers
added carefully by the side of the test tube
without shaking

4 For Acetate:
Ferric Chloride test- Red colour turning brown on
The extract is acidified with dil HNO3 boiled Presence of Acetate confirmed
heating
and cooled. It is then neutralized with NH4OH.
Excess of Ammonia is boiled off. To the neutral
solution, neutral FeCl3 is added.

5
For oxalate:
Calcium chloride test: A white precipitate. The pink
The extract is acidified with dil. Acetic acid and colour discharged with Presence of Oxalate confirmed.
then CaCl2 solution is added. The above ppt is effervescence.
dissolved in dil.H2SO4 and then add KMnO4
solution drop wise.

Preparation of Original Salt solution:

The salt is dissolved in water/ dil. HCl/ dil. HNO3 to prepare the original salt solution.

Systematic Analysis of Cations

2
 Smell of Ammonia, dense white
1 NaOH solution is added to the salt and warmed. Presence of Zero Group (NH4+)
fumes with HCl
Presence of Group I cations
2 Dil. HCl is added to the original salt solution. White precipitate (Pb2+)

Presence of Group II cations

3 H2S is passed through the above solution Black precipitate (Cu2+)
Presence of Group III cations
White precipitate (Al3+)
Boil off H2S, add 2 drops of conc. HNO3.
4
Boil and add solid NH4Cl and excess of NH4OH. Presence of Group III cations
Black precipitate (Fe2+)

Presence of Group IV cations

Dirty White precipitate (Zn2+)
To the above solution- add NH4Cl, Presence of Group IV cations
5 excess of NH4OH and then H2S is Black precipitate (Ni2+)
passed
Presence of Group IV cations
Pale pink precipitate (Mn2+)

Boil off H2S. Add NH4Cl, excess of NH4OH and Presence of Group V cations (Ba2+,
6 White precipitate
saturated (NH4)2CO3 solution. Sr2+, Ca2+)

To the above solution, add NH4OH and

disodium hydrogen phosphate solution. Presence of Group VI cations
7 White crystalline precipitate
Rub the inner sides of the test tube with a glass (Mg2+)
rod.

CONFIRMATORY TEST FOR CATIONS

Analysis of Group Zero (NH4+):
0
Nessler's reagent test:
Brown precipitate. Presence of ammonium confirmed
To the salt solution, add Nessler's reagent.

Analysis of Group 1 cation (Pb2+):

The group I precipitate is dissolved in hot water. It is split into two parts.

Potassium Chromate test:

1 Yellow precipitate. Presence of lead is confirmed.
To one part, add potassium chromate solution.

Yellow precipitate which is soluble in hot

Potassium Iodide test:
water and reappears as golden spangles Presence of lead is confirmed.
Add KI solution to the other part.
on cooling.

2
Analysis of Group 2 cation (Cu2+):
Presence of copper is confirmed.

3
 The black group II precipitate is boiled with dil. Pale blue precipitate which dissolves in
HNO3. Add dil. H2SO4. Then, NH4OH is added excess of NH4OH to give a deep blue
in excess. solution.

To the salt solution, add Potassium ferrocyanide

Chocolate brown precipitate. Presence of copper is confirmed.
solution.

Analysis of Group 3 cation (Al3+):

Lake test:
Dissolve the group 3 white precipitate in dil. Blue precipitate floating on colourless Presence of Aluminium is
HCl. Add two drops of blue litmus solution. solution. confirmed.
3 Then add NH4OH drop wise till blue colour
develops.
Ash test:
To the salt solution, add conc. HNO3. Boil it
with 2-3 drops of cobalt nitrate. Blue ash Presence of Aluminium is
A filter paper soaked in this solution is burnt to confirmed.
ashes.

Analysis of Group 4 cation (Zn2+ and Mn2+):

Dissolve the group 4 precipitate in hot dil HCl.

White precipitate dissolves in excess

NaOH Presence of Zinc is confirmed
NaOH test:
Add NaOH solution drop wise in excess to the
above solution. White precipitate turns brown on
Presence of Manganese confirmed
standing

4 Ash test:
To the salt solution, add conc. HNO3. Boil it
with 2-3 drops of cobalt nitrate. Green Ash Presence of Zinc is confirmed
A filter paper soaked in this solution is burnt to
ashes.

Permanganic acid test:

The above solution is boiled with Conc. HNO3
Pink colour Presence of Manganese confirmed
and PbO2.
It is then diluted with water.

Analysis of Group 5 cation (Ba2+, Sr2+ and Ca2+):

5 Dissolve the group 5 precipitate in hot dil Acetic acid. Divide it into 3 parts.

4
 Potassium Chromate test:
To the first part, add potassium chromate White precipitate Presence of Barium is confirmed.
solution.

Flame test:
A small quantity of the salt is made into a paste
with conc. HCl in a watch glass.
A little of the paste is shown in non-luminous Green Flame Presence of Barium is confirmed.
flame with a platinum wire and the colour is
noted.

Ammonium Sulphate test:

To the second portion, add Ammonium White precipitate Presence of Strontium confirmed.
sulphate solution.

Flame test:
A small quantity of the salt is made into a paste
with conc. HCl in a watch glass.
A little of the paste is shown in non-luminous Crimson red flame Presence of Strontium confirmed.
flame with a platinum wire and the colour is
noted.

Ammonium Oxalate test:

To the third portion, add Ammonium oxalate White precipitate Presence of Calcium is confirmed.
solution.

Flame test:
A small quantity of the salt is made into a paste
with conc. HCl in a watch glass.
A little of the paste is shown in non-luminous Brick Red Flame Presence of Calcium is confirmed.
flame with a platinum wire and the colour is
noted.

Analysis of Group 6 cation (Mg2+):

Ash test:
6 To the salt solution, add conc. HNO3. Boil it with
2-3 drops of cobalt nitrate. Pink ash Presence of Magnesium confirmed.
A filter paper soaked in this solution is burnt to
ashes.