tQUALITATIVE ANALYSIS

ANION ANALYSIS

1. Dil H2SO4 group

Preliminary test : Heat a pinch of salt with dil. Sulphuric acid

i. Carbonate ion(CO32-) (Brisk effervescence of CO2)

ii. Nitrite ion(NO21-) (Brown fumes of NO2)
iii. Sulphide ion(S2-) (Rotten egg smell of H2S)
iv. Sulphite ion(SO32-) (SO2 Gas with a burning sulphur smell)

Confirmatory Tests of dil. H2SO4 group

1. Carbonate ion:
i. Lime water test: pass the gas evolved in the preliminary test through lime
water using a W-tube. The lime water turns milky and the milkiness
disappears on passing the gas for long time.
ii. MgSO4 test : add a few drops of MgSO4 to the OS of the given salt.
Formation of a white ppt of MgCO3 confirms the presence of CO32- ion.

2. Nitrite ion:
i. Dipheylamine test: Add a few drops of diphenylamine solution to the OS of
the given salt. A blue colouration indicates the presence of nitrite ion.
ii. FeSO4 test: to the OS of the given salt add a few drops of dil H2SO4 followed
by the addition of freshly prepared FeSO4 solution. The development of
black or brown colour in the solution confirms NO2-1.

3. Sulphide ion:
i. Sodium nitroprusside test {Na2[Fe(CN)5NO]}: Add a few drops of sodium
nitroprusside solution to the OS of the given salt. A purple or violet
colouration confirms the presence of S2- ions.
ii. Lead acetate test {Pb(CH3COO)2}: add a few drops of Lead acetate solution
to the OS of the given salt. The formation of a black ppt of lead sulphide
confirms the presence of sulphide ion in the given salt.
 4. Sulphite ion:
i. Potassium Dichromate test:{K2Cr2O7} pass the SO2 gas generated on
treatment with dil H2SO4 solution through potassium dichromate solution.
The solution turns green to confirm the presence of SO32-.
ii. BaCl2 test{BaCl2}: the addition of a few drops of BaCl2 solution to theOS
of the salt results in the formation of a white ppt which dissolves on the
addition of dil. HCl.

2. Conc. sulphuric acid group

Preliminary test: Heat a pinch of salt with a few drops of conc. sulphuric acid

i. Chloride ion(Cl-1) (colourless gas with a pungent smell that turns into white
fumes when a rod dipped in NH4OH is brought near the mouth of the test tube)
ii. Bromide ion(Br-1) (orange brown fumes of Br2)
iii. Iodide ion(I-1) (violet vapours of I2)
iv. Nitrate ion (NO3-1) (brown fumes of NO2)
v. Acetate ion(CH3COO-) (vinegar like smelling vapours of CH3COOH)
vi. Oxalate ion (C2O42-) (a colourless mixture of CO2 and CO gas evolved)

Confirmatory tests of Conc. sulphuric acid group:

1. Chloride ion:
i. Silver nitrate test: to the OS of the salt add a few drops of dil HNO 3 followed
by the addition of AgNO3 solution. The formation of a curdy white ppt
soluble in NH4OH confirms the presence of Cl-1.
ii. Chromyl chloride test{CrO2Cl2}: In one arm of a W-tube, a pinch of salt is
mixed with a pinch of solid potassium dichromate and NaOH is added to
the other arm of the tube. A few drops of conc. H2SO4 are added to the arm
containing the salt and K2Cr2O7 and the gas evolved is allowed to pass
through NaOH solution in the other arm. The solution turns yellow. Further,
the addition of a few drops of acetic acid and lead acetate solution to the
 NaOH containing arm, the formation of yellow ppt confirms the presence
of Cl-1.

2. Bromide ion:
i. Silver nitrate test: to the OS of the salt add a few drops of dil. HNO 3,
followed by the addition of a few drops of AgNO3 solution. The formation
of a pale yellow ppt that dissolves in NH4OH with difficulty confirms the
presence of Br-1.
ii. Layer test: to the OS of the give salt add CS2 followed by the addition of
conc. HNO3. The development of orange-brown colouration in the organic
layer on shaking the test tube vigorously confirms the presence of Br-1.

3. Iodide ion:
i. Silver nitrate test: to the OS of the given salt add a few drops of dil. HNO3,
followed by the addition of AgNO3 solution. The formation of yellow
precipitate that is insoluble in NH4OH confirms the presence of I-.
ii. Layer test: to the OS of the given salt add CS 2 followed by the addition of
conc. H2SO4. The development of violet colour in the organic layer on
shaking the test tube vigorously confirms the presence of I-.

4. Nitrate ion:
i. Copper turnings test: add a few copper turnings to the test tube during the
preliminary test. The brown fumes intensify leaving behind a blue coloured
solution of CuSO4.

ii. Brown ring test: to the OS of the given salt add FeSO 4 solution followed by
the addition of conc. H2SO4 slowly along the sides of the test tube. The
formation of a brown ring at the junction of the two layers confirms the
presence of NO3-1 .

5. Acetate ion (CH3COO-1)

i. Oxalic acid test: mix a pinch of salt with oxalic acid and prepare a paste
with a few drops of water. The paste smells of vinegar which confirms the
presence of acetate.
 ii. Ferric chloride test: to the OS of the salt add a few drops of neutral FeCl3
solution to obtain a red-coloured filtrate. Divide the solution into two parts:
a. Add a few drops of dil. HCl to one part → red colour disappears
b. Add some water and boil the contents of the test tube→ reddish brown
ppt obtained.

6. Oxalate ion(C2O42-)
i. Calcium chloride test: to the OS of the given salt add a few drops of dil.
Acetic acid and boil off CO2 gas. Add a few drops of CaCl2 solution to the
test tube. Formation of a white precipitate soluble in dil. HNO3 confirms the
presence of oxalate ions.
ii. Potassium permanganate test: Filter the above precipitate and add a few
drops of dil. H2SO4 followed by a few drops of KMnO4 soltion. The pink
colour of KMnO4 discharges on warming; confirming the presence of
oxalate in the salt.

Independent group (not indicated by dil or conc. H2SO4)

1. Sulphate ion(SO42-)
i. BaCl2 test: to the OS of the given salt add a few drops of BaCl2 solution.
Formation of a white precipitate insoluble in HCl confirms the presence of
sulphate ion.
ii. Lead acetate test: to the OS of the given salt add a few drops of lead acetate
solution. The formation of white precipitate confirms the presence of
sulphate.

2. Phosphate ion (PO43-)

i. Ammonium molybdate test: boil the OS of the salt with a few drops of
conc. HNO3, followed by the addition of ammonium molybdate solution.
Development of yellow colouratio or formation f yellow ppt confirms the
presence of PO43-.
ii. Magnesia mixture test: boil the OS of the salt with a few drops of HCl. Add
a few drops of magnesia mixture to the test tube and allow the mixture to
stand. The formation of white precipitate confirms phosphate ion.
Preparation of Magnesia mixture: In a test tube add a pinch of solid NH 4Cl
to about 1mL of Magnesium Chloride. boil and cool, followed by the
addition of NH4OH (in excess), till the solution smells strongly of ammonia.