QUALITATIVE ANALYSIS

Scheme for Systematic Analysis of a Mixture containing two Salts

Qualitative Analysis
Tests For Anions

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Preparation of Sodium Carbonate Extract:

One gram of the mixture is treated with thrice its weight of anhydrous Na 2 CO3 and about 20 to 25 ml of water and boil it for about 15 minutes. The mixture is then cooled and filtered . the filterate is known as Sodium Carbonate Extract. It is used to perform wet tests. EXPERIMENT Action of dil HCl . OBSERVATION INFERENCE

.
DryTest 1

a. Brisk efferverscence

To a little of the mixture dil HCl is added and warmed.

b.

c. d.

with the evolution of colourless odourless gas turning lime water milky Colourless gas with the smell of rotten eggs, turning lead acetate paper black. Colourless gas with smell of burning matches. Reddish brown vapours with pungent smell

a. Presence of CO 3 2b. Presence of S 2 c. Presence of SO 3 2d. Presence of NO 2

Action of Conc. H2 SO 4 .

a. Colourless gas forming

thick white fumes with Conc. NH4 OH at the mouth of the test tube. b)Fuming gas with reddish brown vapours, with the solution turning brown. Fuming gas with violet vapours, solution turning black. Smell of vinegar Reddish brown vapours on strong heating or on heating with Cu turnings.

a. Presence of Cl b. Presence of Br c. Presence of I- d. Presence of

CH 3 COO - .

A little of the mixture is treated with conc H2 SO 4 and warmed. If there is no reaction to the above solution Copper turnings are added and warmed

b.

c. d. e.

a. Presence of NO 3 -

Ammonium Molybdate test A little of the mixture is warmed with Conc. HNO 3 and Ammonium Molybdate.

Bright Yellow precipitate of Ammonium Phospho molybdate is formed.

Presence of PO 4 3-

Wet test 4

To a little of the salt solution or Sodium Carbonate extract after acidification with dil

White precipitate which is insoluble in dil HCl is formed

Presence of SO 4 2-

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QUALITATIVE ANALYSIS

HCl BaCl 2 solution is added.

Confirmation test for Halides: MnO2 Test To a little of the mixture MnO2 and Conc. H2 SO 4 is added and warmed

a. Greenish Yellow gas

b. c.

with pungent smell turning KI paper brown. Reddish brown vapours condensing to form red droplets. Violet vapours condensing to form violet solid.

a. Presence of Cl b. Presence of Br c. Presence of I-

Wet Test

AgNO3 Test. The Sodium Carbonate extract is acidified with dil. HNO 3 boiled and treated with AgNO3

a. Curdy white

b.

precipitate soluble in excess of NH4 OH solution. Pale Yellow ppt. sparingly soluble in NH4 OH. insoluble in NH4 OH.

a. Presence of Cl b. Presence of Br c. Presence of I-

c. Yellow precipitate

Confirmation of Chloride Chromyl Chloride Test. The Mixture is mixed with solid K2 Cr 2 O 7 and warmed with Conc. H2 SO 4 . The issuing vapours are passed into H2 O in a test tube, followed by NH4 OH and Lead Acetate solution

a. Reddish brown gas

b.

dissolving in H2 O forming yellow solution. Yellow ppt. is formed on adding lead acetate solution.

Presence of Cl - confirmed.

Confirmation of NO 3 Brown Ring Test. The extract is mixed with dilute H2 SO 4 and freshly prepared FeSO 4 solution. Conc. H2 SO 4 is added along the sides of the test tube without shaking.

Brown ring is formed at the junction of the two liquids. This is due to the formation of the following comples [Fe(H2 O)5 NO] Penta aquo nitroso ferrus(II) Complex ion (Nitroso ferrous sulphate)

Presence of NO 3 Confirmed

Conf. of CH 3 COO - .

a. Red colour turning

brown on boiling.

a) Presence of CH 3 COO -

a. The extract is

acidified with dil HNO 3 boiled and neutralised with NH4 OH followed by FeCl3

b. Pleasant fruity smell.

b) Presence of CH 3 COO Confirmed.

b. Ester test. The

extract is treated with ethyl alcohol and a drop of Conc. H2 SO 4 and warmed. The solution is now added to a large quantity of water.

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QUALITATIVE ANALYSIS

Confirmation of PO 4 3- . The extract is treated with dil. HNO 3 and excess of AgNO3 . NH4 OH is now added through the sides of the test tube.

Yellow ring is formed at the neutral junction.

Presence of PO 4 3- .

Confirmation of S 2- . The extract is treated with dilute acetic acid and Lead Acetate

Black precipitate

Presence of S 2-

Tests For Cations

Zero I Group II Group NH4 + Pb2+ Pb2+ Cu2+ Cd2+ III Group Al3+ Fe3+ Mn 2+ IV Group Mn 2+ Zn 2+ Ni2+ V Group Ba 2+ Sr 2+ Ca 2+ VI Group Mg2+ Salt solutions is treated with NH4 Cl followed byNH4 OH and (NH4 )2 HPO 4 Salt solutions is treated with NH4 Cl followed byNH4 OH and (NH4 )2 CO 3 Salt solution is treated with NH4 Cl solid followed NH4 OH and H2 S. Salt solution is treated with NH4 Cl solid followed by NH4 OH NaOH and Nesslers Reagent Salt Solution and dil. HCl Salt Solution , dil HCl and H2 S Brown Precipitate White Precpitate Black Precipitate Black Precipitate Yellow Precipitate Gelatinous White ppt. Gelatinous Brown ppt. White turning Brown on standing. Buff or Pale pink ppt Dull white ppt Black ppt White ppt White ppt White ppt White ppt

Preparation of Original Solution .

The mixture should be dissolved in an suitable solvent. The choice of solvents can have the following sequence.1.Cold Water, 2. Warm water, 3. Dilute HCl, 4. Concentrated HCl, 5. Dilute HNO3 , 6. Concentrated HNO3 , and 6. Aquaregia. The solution prepared by dissolving the mixture in the solvent is referred to a the original solution or O.S.

0 Group

EXPERIMENT

OBSERVATION

INFERENCE

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QUALITATIVE ANALYSIS

Shake the aqueous mixture solution well with NaOH and note the odour. To one ml of Nesslers (K 2 [HgI4 ]) reagent add aqueous mixture solution

Smell of Ammonia NH3

Presence of NH4 + indicated

Brown precipitate of Mercuric Amido Iodide (NH2 .HgO.HgI) is obtained.

NH4 + Confirmed

I Group

A) White Precipitate. Dissolve the above precipitate in hot water and perform the following tests

The white ppt. of PbCl 2 is soluble in hot water Pb2+ + 2Cl - PbCl 2 Yellow precipitate due to the formation of PbCrO4 . Pb2+ + CrO4 PbCrO4 .

Pb2+ may be present

(i) Treat a part of the above solution with K2 CrO4 solution

Pb2+ Present

(ii) To another part of group one solution add KI solution

Yellow precipitate due to the formation of PbI 2 which is soluble in hot water reappears as golden spangles on cooling Pb2+ + I - PbI 2

Pb2+ Confirmed

II Group

Black Precipitate.(NiS). Dissolve the group II black residue in dil HNO 3 and perform the following tests. a) If the solution is blue perform the following tests. (i) Add NH4 OH drop wise until it is in excess.

a. Solution is blue b. Solution is Colourless

a. Cu2+ b. Pb2+

Blue precipitate is formed which dissolves in excess of the reagent. Cu2+ + 2OH - Cu(OH) 2 Cu(OH) 2 + 4NH4 OH [Cu(NH3 )4 ](OH) 2 + 4H2 O.

Cu2+

(ii) Acidify the second portion with acetic acid and add potassium Ferrocyanide.

Reddish brown precipitate is obtained. 2Cu2+ + [Fe(CN) 6 ] 4- Cu2 [Fe(CN) 6 ]

Cu2+

b) If the solution is colour less perform the following tests. (i) Add KI to one part of the above solution.

Yellow precipitate due to the formation of PbI 2 which is soluble in hot water reappears as golden spangles on cooling. Pb2+ + 2I- PbI 2 Yellow precipitate due to the formation of PbCrO4 Pb2+ + CrO4 2- PbCrO4

Pb2+ Confirmed

(ii)Add K2 CrO4 to another part of the solution

Pb2+ Confirmed

B. Yellow precipitate
(CdS)

Presence of Cd2+

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QUALITATIVE ANALYSIS

Boil the yellow precipitate with yellow ammonium sulphide and divide into two parts .

(i) One part of the residue is dissolved in dil HNO 3 and ammonium hydroxide is added drop wise. (ii) To the Second part of the above solution pass H2 S.

White Precipitate soluble in excess.

Presence ofCd 2+

III Group

Yellow precipitate.

Presence ofCd 2+ Confirmed.

A. Gelatinous white ppt.

of Al(OH) 3 . Dissolve the white gelatinous precipitate by boiling with NaOH solution and divide it into two parts.

(i) To the first part add NH4 Cl and boil (ii) To the second part add dil. HCl ,litmus solution and excess of NH4 OH Ash test: Group III residue + 3 drops of conc. HNO 3 + 3 drops of Cobalt nitrate. Dip a rolled filter paper in this solution and burn in the flame B) Gelatinous brown ppt. Fe(OH) 3 . Dissolve the ppt. in dil HCl and divide it into two parts. (i) To one part of the above precipitate add Potassium Ferrocyanide solution.

White precipitate

Al3+ present Presence of Al3+ confirmed.

A blue lake

A Blue tinted ash is obtained. 2Al(OH) 3 Al2 O 3 + 3H2 O. 2 Al2 O 3 + 2Co(NO)3 2CoO.Al2 O 3 + 4NO 2 + O 2

Presence of Al3+ confirmed.

A blue (Prussian blue) coloured solution or precipitate is formed. Fe3+ + 3 [Fe(CN) 6 ] 4- Fe4 [Fe(CN) 6 ] 3

Presence of Fe3+ indicated.

(ii) To the second part add Potassium thiocyanide.

Blood red coloration Fe3+ + 3CNS - Fe(CNS)3

Presence of Fe3+ confirmed.

IV Group

A) Black precipitate. (NiS) Conformation for Ni2+ Dissolve the black precipitate in dil. HCl add NH4 Cl and NH4 OH and divide into two parts:

Presence of Ni2+

(i) To the first part add Dimethyl Glyoxime (ii) Through the second part pass H S gas.

Rose Red Precipitate.

Presence of Ni2+ Confirmed. Presence of Ni2+

A black precipitate is formed

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QUALITATIVE ANALYSIS
2

Confirmed.

B)DullWhite precipitate. Conformation for Zn 2 + Dissolve the white ppt. in dilute HCl, to this solution NaOH is first added in drops then in excess until the ppt. dissolves.

(i) To one part add Acetic acid and potassium Ferrocyanide.

White precipitate is formed. Zn 2+ + [Fe(CN) 6 ] 4- Zn 2 [Fe(CN) 6 ] White precipitate is formed

Presence of Zn 2+ confirmed.

(ii) Pass H2 S and filter

Presence of Zn 2+ confirmed. Presence of Zn 2+ confirmed

Ash test: Group IV residue + 3 drops of conc. HNO 3 + 3 drops of Cobalt nitrate. Dip a rolled filter paper in this solution and burn it in the non luminous part of the flame. C) Conformation of Mn 2+ . Buff precipitate is heated with PbO 2 and conc. HNO 3 and dilute with water.

Green tinted ash is formed.

The supernatent liquid turns pink due to the formation of permanganic acid. 2Mn(NO 3 )2 + 5PbO + 6HNO 3 5Pb(NO 3 )2 + 2HMnO 4 + 2H2 O

Presence of Mn 2+ is confirmed.

V Group

White precipitate: Dissolve the group V precipitate in minimum quantity of Acetic acid and divide into three parts. Keep aside a part of the group precipitate for Flame test.

i. To one part of the

above soln. Add K2 CrO4 .

A Yellow precipitate is formed. Ba 2+ + CrO4 2- BaCrO 4 A White precipitate is formed. Sr 2+ + SO 4 2- SrSO4 A White precipitate is formed. Ca 2+ + C 2 O 4 2- Ca C 2 O 4 a) Apple Green flame b) Crimson Flame c) Brick Red Flame

Presence of Ba 2+ Ba 2+ confirmed.

To the second part add CaSO4 and boil.

Presence of Sr 2+ confirmed

To the third part add Ammonium Oxalate

Presence of Ca 2+ confirmed

Flame test: The group V residue is treated with conc. HCl and a Nichrome / Platinum wire dipped in the above solution is shown into the non luminous part of the flame.

a) Ba 2+ Confirmed b) Sr 2+ confirmed c) Ca 2+ confirmed

VI Group

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QUALITATIVE ANALYSIS

White Crystalline ppt. Group VI ppt. is dissolved in minimum quantity of dil HNO 3 and few drops of conc. HNO 3 and Cobalt Nitrate are added. A rolled filter paper is dipped in the above solution and burned in the non luminous part of the flame.

A pink tinted ash is obtained.

Presence of Mg2+ is confirmed.

Magneson reagent test: The group VI residue is dissolved in dil. HCl to this a few drops of Magneson reagent is added followed by NaOH.

A blue precipitate is formed.

Presence of Mg2+ is confirmed.

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