Scheme for Systematic Analysis of a Mixture containing two Salts

Qualitative Analysis
Tests For Anions

Preparation of Sodium Carbonate Extract:

One gram of the mixture is treated with thrice its weight of anhydrous Na2CO3 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.

.
DryTest 1

EXPERIMENT Action of dil HCl.

OBSERVATION

INFERENCE

a. Brisk
efferverscence 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.

a. Presence of
CO32-

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

b. Presence of S2-

c. Presence of
SO32-

c.

d. Presence of NO2-

d. Reddish brown
vapours with pungent smell 2 Action of Conc. H2SO4.

a. Colourless gas
forming thick white fumes with Conc. NH4OH at the mouth of the test tube.

a. Presence of Clb. Presence of Br-

A little of the mixture is treated with conc H2SO4 and warmed. If there is no reaction to the above

b. b)Fuming gas solution Copper turnings are added and warmed c.

with reddish brown vapours, with the solution turning brown. Fuming gas with violet vapours, solution turning black. Smell of vinegar

c. Presence of Id. Presence of

CH3COO-.

a. Presence of NO3-

d.

e. Reddish brown
vapours on strong heating or on heating with Cu turnings. 3 Ammonium Molybdate test A little of the mixture is warmed with Conc. HNO3 and Ammonium Molybdate. Wet test 4 To a little of the salt solution or Sodium Carbonate extract after acidification with dil HCl BaCl2 solution is added. Confirmation test for Halides: MnO2 Test To a little of the mixture MnO2and Conc. H2SO4 is added and warmed Bright Yellow precipitate of Ammonium Phospho molybdate is formed. Presence of PO43-

White precipitate which is insoluble in dil HCl is formed

Presence of SO42-

a. Greenish Yellow
gas with pungent smell turning KI paper brown. Reddish brown vapours condensing to form red droplets.

a. Presence of Clb. Presence of Brc. Presence of I-

b.

c. Violet vapours
condensing to form violet solid. Wet Test AgNO3 Test. The Sodium Carbonate extract is acidified with

a. Curdy white
precipitate soluble in excess of NH4OH

a. Presence of Clb. Presence of Br-

solution. dil. HNO3 boiled and treated with AgNO3

b. Pale Yellow ppt.

sparingly soluble in NH4OH.

c. Presence of I-

c. Yellow
precipitate insoluble in NH4OH. Confirmation of Chloride Chromyl Chloride Test. The Mixture is mixed with solid K2Cr2O7 and warmed with Conc. H2SO4. The issuing vapours are passed into H2O in a test tube, followed by NH4OH and Lead Acetate solution Confirmation of NO3Brown Ring Test. The extract is mixed with dilute H2SO4 and freshly prepared FeSO4 solution. Conc. H2SO4 is added along the sides of the test tube without shaking.

a. Reddish brown
gas dissolving in H2O forming yellow solution.

Presence of Clconfirmed.

b. Yellow ppt. is
formed on adding lead acetate solution.

Brown ring is formed at the junction of the two liquids. This is due to the formation of the following comples [Fe(H2O)5NO] Penta aquo nitroso ferrus(II) Complex ion (Nitroso ferrous sulphate)

Presence of NO3 Confirmed

Conf. of CH3COO-.

a. Red colour
turning brown on boiling.

a) Presence of CH3COO-

a. The extract is
acidified with dil HNO3 boiled and neutralised with NH4OH followed by FeCl3

b. Ester test. The

b) Presence of CH3COOConfirmed.

extract is treated with ethyl alcohol and a drop of Conc. H2SO4 and warmed. The solution is now added to a large quantity of water. Confirmation of PO43-. The extract is treated with dil. HNO3 and excess of AgNO3 . NH4OH is now added through the sides of the test tube. Confirmation of S2-. The extract is treated with dilute acetic acid and Lead Acetate

b. Pleasant fruity
smell.

Yellow ring is formed at the neutral junction.

Presence of PO43-.

Black precipitate

Presence of S2-

Tests For Cations

Zero I Group II Group

NH4+ Pb2+ Pb2+ Cu2+ Cd2+

NaOH and Nesslers Reagent Salt Solution and dil. HCl Salt Solution , dil HCl and H2S

Brown Precipitate White Precpitate Black Precipitate Black Precipitate Yellow Precipitate

III Group

Al3+ Fe3+ Mn2+

Salt solution is treated with NH4Cl solid followed by NH4OH

Gelatinous White ppt. Gelatinous Brown ppt. White turning Brown

on standing. IV Group Mn2+ Zn2+ Ni2+ V Group Ba2+ Sr2+ Ca2+ VI Group Mg2+ Salt solutions is treated with NH4Cl followed byNH4OH and (NH4)2HPO4 Salt solutions is treated with NH4Cl followed byNH4OH and (NH4)2CO3 Salt solution is treated with NH4Cl solid followed NH4OH and H2S. 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.

EXPERIMENT
0 Group Shake the aqueous mixture solution well with NaOH and note the odour. To one ml of Nesslers (K2[HgI4]) reagent add aqueous mixture solution I Group A) White Precipitate. Dissolve the above precipitate in hot water and perform the following tests

OBSERVATION

INFERENCE

Smell of Ammonia NH3

Presence of NH4+ indicated

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

NH4+ Confirmed

The white ppt. of PbCl2 is soluble in hot water Pb2+ + 2Cl- PbCl2

Pb2+ may be present

(i) Treat a part of the above solution with K2CrO4 solution

Yellow precipitate due to the formation of PbCrO4. Pb2+ + CrO4 PbCrO4.

Pb2+ Present

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

Yellow precipitate due to the formation of PbI2 which is soluble in hot water reappears as golden spangles on cooling Pb2+ + I- PbI2

Pb2+ Confirmed

II Group Black Precipitate.(NiS). Dissolve the group II black residue in dil HNO3 and perform the following tests. a) If the solution is blue perform the following tests. (i) Add NH4OH drop wise until it is in excess.

a. Solution is blue b. Solution is

Colourless Blue precipitate is formed which dissolves in excess of the reagent. Cu2+ + 2OH- Cu(OH)2 Cu(OH)2 + 4NH4OH [Cu(NH3)4](OH)2 + 4H2O. Reddish brown precipitate is obtained. 2Cu2+ + [Fe(CN)6]4- Cu2[Fe(CN)6] Yellow precipitate due to the formation of PbI2 which is soluble in hot water reappears as golden spangles on cooling. Pb2+ + 2I- PbI2

a. Cu2+ b. Pb2+
Cu2+

(ii) Acidify the second portion with acetic acid and add potassium Ferrocyanide. b) If the solution is colour less perform the following tests. (i) Add KI to one part of the above solution.

Cu2+

Pb2+ Confirmed

(ii)Add K2CrO4 to another part of the solution

Yellow precipitate due to the formation of PbCrO4 Pb2+ + CrO42- PbCrO4

Pb2+ Confirmed

B. Yellow
precipitate (CdS) Boil the yellow precipitate with yellow ammonium sulphide and divide into two parts . (i) One part of the residue is dissolved in dil HNO3 and ammonium hydroxide is added drop wise. (ii) To the Second part of the above solution pass H2S. III Group White Precipitate soluble in excess.

Presence of Cd2+

Presence ofCd2+

Yellow precipitate.

Presence ofCd2+ 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 NH4Cl and boil (ii) To the second part add dil. HCl ,litmus solution and excess of NH4OH Ash test: Group III residue + 3 drops of conc. HNO3 + 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 White precipitate A blue lake Al3+ present Presence of Al3+ confirmed.

A Blue tinted ash is obtained. 2Al(OH)3 Al2O3 + 3H2O. 2 Al2O3 + 2Co(NO)3 2CoO.Al2O3 + 4NO2 + O2

Presence of Al3+ confirmed.

divide it into two parts. (i) To one part of the above precipitate add Potassium Ferrocyanide solution. A blue (Prussian blue) coloured solution or precipitate is formed. Fe3++ 3 [Fe(CN)6]4- Fe4[Fe(CN)6]3 (ii) To the second part add Potassium thiocyanide. IV Group A) Black precipitate. (NiS) Conformation for Ni2+ Dissolve the black precipitate in dil. HCl add NH4Cl and NH4OH and divide into two parts: (i) To the first part add Dimethyl Glyoxime (ii) Through the second part pass H2S gas. B)DullWhite precipitate. Conformation for Zn2+ 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. Zn2+ + [Fe(CN)6]4- Zn2[Fe(CN)6] White precipitate is formed Presence of Zn2+ confirmed. Presence of Zn2+ confirmed. Rose Red Precipitate. A black precipitate is formed Presence of Ni2+ Confirmed. Presence of Ni2+ Confirmed. Presence of Ni2+ Blood red coloration Fe3+ + 3CNS- Fe(CNS)3 Presence of Fe3+ confirmed. Presence of Fe3+ indicated.

(ii) Pass H2S and filter

Ash test: Group IV residue + 3 drops of conc. HNO3 + 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 Mn2+. Buff precipitate is heated with PbO2 and conc. HNO3 and dilute with water.

Green tinted ash is formed.

Presence of Zn2+ confirmed

The supernatent liquid turns pink due to the formation of permanganic acid. 2Mn(NO3)2 + 5PbO + 6HNO3 5Pb(NO3)2 + 2HMnO4 + 2H2O

Presence of Mn2+ 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 K2CrO4 .

A Yellow precipitate is formed. Ba2+ + CrO42- BaCrO4

Presence of Ba2+ Ba2+ confirmed.

To the second part

add CaSO4 and boil.

A White precipitate is formed. Sr2+ + SO42- SrSO4

Presence of Sr2+ confirmed

To the third part

add Ammonium Oxalate

A White precipitate is formed. Ca2+ + C2O42- Ca C2O4

Presence of Ca2+ confirmed

Flame test: The group V residue is treated with conc. HCl and a Nichrome /

a) Apple Green flame b) Crimson Flame c) Brick Red Flame

a) Ba2+ Confirmed b) Sr c) Ca
2+

confirmed confirmed

2+

Platinum wire dipped in the above solution is shown into the non luminous part of the flame. VI Group White Crystalline ppt. Group VI ppt. is dissolved in minimum quantity of dil HNO3 and few drops of conc. HNO3 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. 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. A pink tinted ash is obtained. Presence of Mg2+ is confirmed.