1.

Preliminary Tests
a) Note the colour of the salt. Observations (i) Blue (ii) Bluish green (iii) Brown or yellowish brown (iv) Brown or deep pink or violet (v) Light green (vi) Light pink or flesh coloured (vii) White Inference Cu2+ Cu2+ or Ni2+ Fe3+ or Mn2+ Co2+ Fe2+ or Ni2+ Mn2+ Absence of Cu 2+, Ni2+ Fe3+, Fe2+, Mn2+ and Co2+ 1. Note the smell of the salt by rubbing the moistened salt between the fingers. (i) Ammoniacal smell (ii) Smell of rotten eggs (iii) Vinegar smell NH4+ S2CH3COO-

2. Take a little of the salt on a piece of paper and place this on the palm of your hand to find whether the salt is heavy or light.

(i) It is quite heavy salt (ii) It is a light salt and a fluffy powder

Ba2+ or Pb2+ Salt ZnCO3 or MgCO3 or CaCO3

2. Dil H2SO4 Test Take a little of the salt (about 0.5g) in a test tube and add dil. H2S04. Warm if no reaction takes place. (a) Gas Evolved (i) A colourless, odourless, gas evolves with effervescence which turns lime water milky (CO2 gas)

CO32-

(ii) A colourless gas having burning sulphur smell evolves which turns acidified potassium dichromate green (SO 2 gas)

SO32-

(iii) A colourless gas having rotten eggs smell evolves which turn lead acetate paper black H 2S gas (iv) A brown gas having pungent smell evolves which turns FeSO 4 solution black (NO2 gas)

S2-

NO2-

(v) No gas evolved

CO32- ,SO32- ,S2- ,NO2Absent Pb2+, Ba2+, Sr2+ or Ca2+ is present

(a) A white ppt is formed in the reaction mixture 2. Conc H2SO4 Test

Take a little of the salt in a test-tube. Add conc H2SO4 just to soak the salt and then heat.

(i) A colourless gas having pung-gentsmell evolves whichgives white dense fumes with a rod dipped in NH 4OH (HCI gas) (ii) A yellowish brown gas having irritating smell evolves which turns starch paper yellow (Br2 gas) (iii) A dark violet gas evolves which turns starch paper blue (l 2 gas) (iv) A reddish brown gas having pungent smell evolves which turns. FeSO 4 solution black. (NO2 gas) (v) A colourless gas having vinegar smell evolves. [Acetic acid (CH3COOH) vapours] (vi) A colourless, odourless gas which burns with a blue flame (CO gas) along with CO2 gas which turns lime water milky.

Cl-

BrINO3-

CH3COO-

Oxalate (C2O42-)

3.Confirmatory (or wet) Tests for Acid radicals

1. Confirmation of carbonate (a) Take a little of the salt in a test-tube and add distilled water. Shake (i) Soluble carbonate of NH4+ Insoluble CO 32-

(i) Clear solution (ii) Salt is insoluble in water

(b) Magnesium sulphate test : To the aqueous solution of soluble carbonate add MgSO4 solution (c) Phenolphthalein test: To another part of aqueous solution of soluble salt add phenolphthalein 2. Confirmation of sulphite

White precipitate

Soluble CO32-confirmed

Pink colour

Soluble CO32- confirmed

(a) Barium chloride test: To a portion of aqueous solution or soda extract add acetic acid till effervescence ceases. Then add BaCI2 solution.

A white ppt which dissolves in dil HCI with the evolution of SO 2 gas

SO32- confirmed

(b) Ferric chloride test: To a portion of aqueous extract add FeCI 3solution. 3. Confirmation of Chloride (a) Silver nitrate test:To aqueous solution or soda extract, add dil HNO3 till acidic. Then add AgNO 3 solution.

Dark red colour which changes into reddish brown ppt on boiling

SO32- confirmed

Curdy white ppt soluble in NH4OH

Cl- confirmed

(b) MnO2 test: Mix salt with MnO2 in a test tube. Then add conc. H 2SO4 and heat.

Yellowish green gas evolves which bleaches moist blue litmus paper

Cl- confirmed

(c)Chromyl Chloride test: Mix salt with solid K2Cr2O7 in a test tube. Then add conc H 2SO4 and heat. 4. Confirmation of bromide (a )Silver nitrate test:To aqueous solution or soda extract add HN0 3till acidic.Then add AgN03 solution. 5. Confirmation of iodide (a) Silver nitrate test:To aqueous solution or soda extract add HN0 3 till acidic. Then add AgN03 solution. 6. Confirmation of nitrate

Red vapours of chromyl chloride evolve which on passing through water gives yellow solution which on adding lead acetate solution gives yellow ppt

Cl- confirmed

Pale yellow ppt sparingly soluble in NH4OH

Br- confirmed

Yellow ppt insoluble in NH4OH

I- confirmed

(a) Ring test: To the aqueous solution of the salt, add freshly prepared FeS0 4 solution. Shake and then add conc. H 2S04 along the sides of test-tube.

Dark brown or black ring is formed at the junction of the layers of the acid and the solution

NO3- confirmed

(b) Copper chips test: To a little of the salt in a test tube add copper chips (or paper pellet) and then add conc.H 2S04. Heat.

Dark brown fumes evolves

NO3- confirmed

7. Confirmation of acetate (a) Oxalic acid test: Mix a little of the salt with solid oxalic acid. Moisten it with a drop of water. Rub this paste between the fingers.

Vinegar smell

Acetate confirmed

(b) Ester test: To a little of the salt taken in a test tube add conc. H2SO4 & few drops of ethyl alcohol. Heat

Pleasant fruity smell of ester

Acetate confirmed

(c) FeCI3 test: To the aqueous solution of the salt add neutral FeCI 3 solution

Blood red colour

Acetate confirmed

8. Confirmation of sulphate

(a) BaCI2 test: To a little of the solution add HCI. Heat to expel if any gas is formed. Then add BaCI2 solution.

White ppt insoluble in HCI

S042- confirmed

4.Wet Tests for Basic radicals

1. Preparation of original solution (O.S.)

Take a little of the salt and try to dissolve in the following solvents one by one (i) (ii) (iii) (iv) Distilled water - cold or hot Dil. HCI - cold or hot Conc. HCI - cold or hot HNO3 - cold or hot

Once the solvent is found out then prepare O.S. with 0.5 to 1g. of the salt Note : (i) If solvent is conc. HCI please dilute the solution with distilled water. (ii) If solvent is HNO3, evaporate the solution to dryness and dissolve in water 2. Analysis of Group Zero (NH4+ ) Sodium hydroxide test :To a little of salt add conc, solution of NaOH and Heat. 3. Analysis of Group 1 (Pb2+) (i) To the original salt solution in water add HCl (a) White ppt (b) No ppt (ii) Hot water test: Filter the white ppt, wash with water and add 10 ml of water. Heat ppt dissolves Pb2+ is present 1st group is present 1st group is absent A colourless gas having ammonical smell is evolved which turns Nesselers solution reddish brown

NH4+ is present

(iii) Potassium chromate test : To one part of hot aqueous solution of the salt add potassium chromate solution. Note: If on adding HCI to aqueous solution no ppt is formed or original solution is prepared in HCI, then Pb 2+ is absent.

yellow ppt

Pb2+ is confirmed

4. Analysis of Group II [Pb2+, Cu2+ and As34] This group salts are not in labs To the original solution add dil HCL and then pass H2S gas through a portion of this solution. If a coloured ppt is formed then pass H2S gas through the whole of the solution. 5. Analysis of Group III (Fe3+ & Al3+) (i) To the original solution, add conc. HNO 3 heat cool. Then add NH4CI solid. Again heat and cool. Then add NaOH till it gives smell of NH3.

a) No ppt

Group II is absent

(a) Reddish Brown ppt

Fe3+ is present

(b) Gelatinous White ppt (c) No ppt (a) Potassium sulphocyanide test : To one part add potassium sulphocyanide solution Blood red colour

Al3+ is present Fe3+ and Al3+ absent Fe3+ confirmed

(b) Potassium ferrocyanide test: To the second part add potassium ferrocyanide solution Lake test: To one part add HCI till the solution turns acidic. Then add 2 drops of blue litmus followed by NH4OH till it gives smell of ammonia 6. Analysis of Group IV (Ni2+, Co2+, Mn2+, Zn2+) This group salts are not in labs (i) To the solution of 5(ii), which gives smell of ammonia, pass H2S gas through a test portion 7. Analysis of Group V( Ba2+,Sr2+ & Ca2+) (i) To the rest of solution from 6(i) through which H2S gas has not been passed, add saturated ammonium carbonate solution and warm.

Deep blue solution

Fe3+ confirmed

Blue ppt floating in colourless solution

Al3+ confirmed

No ppt

IV group is absent

(a) A white ppt (b) No ppt

Ba2+, Sr2+ or Ca2+ is present V group is absent

Potassium chromate test : To the white ppt of 7(i) add acetic acid and heat. To the warm solution add potassium chromate solution. Wash the yellow ppt with hot water & perform flame test with it.

A yellow ppt

Ba2+ present

Grassy green flame through naked eye and bluish green through blue glass Ammonium oxalate test: To the filtrate of 7(iii) add ammonium oxalate solution Flame test: Perform flame test with the white ppt of 7(v) 8. Analysis of GroupVI (Mg2+) (i) Ammonium phosphate test: To the Oriqinal solution add NH 4Cl,NH4OH inslight excess and then ammonium phosphate. (ii) Cobalt nitrate test: Perform cobalt nitrate test with the salt A white ppt appears on scratching the sides of the test tube A white ppt Brick red through naked eye

Ba2+ confirmed

Ca2+ present Ca2+ confirmed

Mg2+ present

Pink mass

Mg2+ confirmed