Qualitative Inorganic Analysis (Salt Analysis)

I. Preliminary tests Physical examination

EXPERIMENT 1. Colour OBSERVATION Light Green Blue (or) Bluish Green Pale Pink Brown (or) Reddish Brown 2. 3. State Odour Odour of rotten eggs Odour of Ammonia Cold (or) hot distilled water Cold (or) hot dil. HCl. 1. White sublimate formed Sulphides Ammonium Salts may be present Crystalline (or) Amorphous Odour of burning Sulphur INFERENCE Ferrous Salts Copper Salts Manganous Salts Ferric Salts may be present

Sulphites

4.

Solubility

5. Dry Test A small quantity of the substance is taken in dry test tube and is heated first gently and then strongly.

Ammonium slats

2. Black sublimate formed Iodide along with violet vapours 3. Substance looses water of crystallisation. Water droplets appear on walls of container 4. Substance is yellow when hot and white when cold. 5. Substance is Orange when hot and white when cold. 6. Reddish brown gas with pungent smell evolved. 7. The substance is blue and becomes colourless on heating. Hydrated salts

Zinc salts

Lead salts

Nitrate

Hydrated Copper Sulphate (CuSO45H2O)

6. Flame Test Prepare a paste of the salt with a few drops of conc. HCl on a watch glass and place a small amount of this paste on glass rod and introduce it (oxidizing flame) into the flame

Apple green Bluish green Brick Red Green flashes Crimson Red

Barium Salts Copper Salts Calcium Salts Zinc or Manganese salts Strontium

IDENTIFICATION OF ANIONS
1. Action with dil. HCL: To the little of the substance dil. HCI is added. a) A colourless, odourless gas evolves with quick effervesces. They turn lime water milky. b) A colourless gas with smell of rotten eggs is evolved. It turns lead acetate (or) lead nitrate paper black. c) A colourless gas with smell of burning sulphur is evolved. The gas turns Potassium dichromate paper green. 2. Action with Con. H2SO4: To a little of the substance Con. H2SO4 is added and the test tube is heated. a) colourless gas with pungent colour is evolved. White dense fumes are evolved when a glass rod dipped in NH4OH exposed to the gas. Carbonate is present.

Sulphide is present.

Sulphide is present.

Chloride may be present

b) A colourless gas along with reddish brown vapours are evolved. The gas turns a drop of AgNO3 taken on glass rod pale yellow. c) Reddish brown vapours are evolved. A drop of AgNO3 is exposed to the gas. No. Pt is formed. 3. Action with BaCl2: To the salt solution BaCl2 is added. White ppt. is formed.

May be Bromide

Nitrate may be present

May be Sulphate

CONFIRMATORY TESTS FOR ANIONS

1. CARBONATE: To the given salt solution BaCl2 solution is added. 2. SULPHATE: To the given salt solution BaCl2 solution is added. 3. Chloride and Bromide: Salt is mixed with a pinch of MnO2 and a few drops of Conc. H2SO4 are added. The test tube may be warmed. A White ppt. of Barium Corbonate which is soluble in dilute HCl is formed. A White ppt. of Barium Sulphate which is insoluble in dilute HCl is formed. a) Greenish yellow vapours are evolved with pungent smell. b) Dark brown vapours which condense to red liquid on the sides of test tube. Reddish brown vapours are evolved the liquid in the tube turns blue or green. Carbonate is confirmed (CO3)-2

Sulphate is confirmed (SO4)-2

Chloride is confirmed (Cl)-1

Bromide is confirmed (Br)-1

4. NITRATE: Salt is taken in a test tube. One (or) Two copper tunings and a few drops of Con. H2SO4 are added and heated.

Nitrate is confirmed.

PREPARATION OF SODIUM CARBONATE EXTRACT

The slat is mixed with 3 times anhydrous Na2CO3 and sufficient distilled water is added and boiled for about 5 minutes. It is cooled and filtered. The filtrate is called Sodium Carbonate extract. 1. TEST FOR Chloride and Bromide: A small amount of extract is neutralized with dil HNO3 and AgNO3 solution is added. a) A white ppt. which is completely soluble in NH4OH and is soluble in HNO3. b) A pale yellow precipitate which is soluble in NH4OH in soluble in dil HNO3. Chloride is confirmed.

Bromide is confirmed.

2. BROWN RING TEST: A small amount of extract in neutralized with dil. H2SO4 freshly prepared solution of ferrous sulphate is added the test tube is added the test tube is kept inclined and Con. H2SO4 is added along its walls. 3. TEST FOR SULPHATE: A Small amount of extract neutralized with dil. HCl, BaCl2 solution is added.

Brown ring is formed at the junction of two layers.

Nitrate is confirmed (NO3)-1

A white crystalline ppt. which insoluble in Conc. HCl. Is formed.

Sulphate is confirmed (SO4)-2

IV. IDENTIFICATION OF CATIONS AMMONIUM ION

1) To the given salt NaOH solution is added and heated. Ammonia vapours are evolved with pungent smell. They produce dense white fumes when glass rod dipped in conc. HCI held in the gas. Filter paper changes to reddish brown colour. (NH4)+1 is confirmed.

2) A filter paper dipped in Nessellers reagent is exposed to the above vapours

(NH4)+1 is Confirmed.

Preparation of Original Solution:

The original solution is prepared by dissolving the salt in suitable solvent To the original solution dil. HCl is added.

I Group
AgCl White PbCl2 - White

To the above solution pass H2S gas. II Group Cus Black Pbs Black Hgs Black The original solution is saturated with NH4CI (solid) and NH4OH. III Group To the above solution pass H2S gas. Fe+2 Pale IVGroup The original solution is saturated Green Mn S with NH4CI (S), NH4OH solution and Al+3 White Flesh colour (NH4)2CO3 is added. Zn S White V Group BaCO3 White CaCO3 White VI Group No group reagents Original solution Is tested for (Mg+2),(NH4) +1 ions

CONFIRMATORY TEST FOR CATIONS

I.GROUP CATIONS: 1) To the original solution K2CrO4 is added. 2) To the original solution KI solution is added. a) Yellow ppt. is formed. Pb+2 is confirmed.

b) Yellow ppt. is formed. It dissolves in boiling water. On cooling golden yellow spangles are formed.

Pb+2 is confirmed.

II. GROUP CATTIONS: 1) To the original solution NH4OH solution is added. 2) To the original solution K4 (Fe (CN) 6) solution is added.

Bluish green ppt. which is soluble Cu+2 is confirmed. in excess NH4OH giving a deep blue colour is formed. A chocolate colour of deep brown colour solution is formed. Cu+2 is confirmed.

III. GROUP CATIONS: 1)To the original solution NH4Cl(s) and NH4OH are added.

a) A dull green ppt. Which is soluble in dil. HCl, dil. H2SO4 is formed. b) A white gelatinous ppt. which is soluble in alkalies is formed.

Fe+2 is confirmed.

Al+3 is confirmed.

2) To the original solution K4(Fe(CN)6) is added.

a) A pale blue ppt. is formed. b) No reaction.

Fe+2 is confirmed.

Al+3 is confirmed. Zn+2 is confirmed.

IV GROUP CATIONS: 1) To the original solution NaOH solution is added.

a) A white ppt. which is soluble in excess of NaOH is formed. b) A white ppt. turning brown which is insoluble in excess NaOH is formed.

Mn+2 is confirmed.

2) To the original solutions NH4CI + NH4OH is added and H2S gas is passed.

a) A white ppt. is formed. b) A flesh colour ppt. is formed.

Zn+2 is confirmed. Mn+2 is confirmed.

V.GROUP CATIONS: 1) To the original solution K2CrO4 is added

a) Yellow ppt. which is soluble in dil HCl is formed. b) No reaction.

Ba+2 is confirmed.

Ca+2 is confirmed. Ba+2 is confirmed.

2)To the original solution Ammonium Oxalate is added

a) A white ppt. which is soluble in acetic acid is formed. b) A white ppt. which is insoluble in acetic acid is formed.

Ca+2 is confirmed.

VI.GROUP CATIONS: 1. The original solution NH4OH is solution is added. 2. Add NH4CI, excess of NH4OH and sodium hydrogen phosphate solution to the original solution

White ppt. is formed.

Mg+2 is confirmed.

A white ppt. is formed.

Mg+2 is confirmed.