SALT ANALYSIS SCHEME OF ANALYSIS EXPERIMENT PRELIMINARY EXAMINATIONS : 1) Noted the colour OBSERVATION INFERENCE Colourless Absence of Cu2+,Fe2+,Fe3+,Mn2+,Co2+,Ni2+ Pre. of Cu2+ Pre. of Fe3+ Pre. of Ni2+ Pre. of Mn2+ Pre. of Co2+ Blue Brown Green Pale pink Pink 2) Noted the solubility a) In water b) In dil.HCl 3) Flame Test : A little of the salt is made into paste with conc.HCl. A glass rod is dipped in it and introduced into the flame. 4) Ash Test : A little of the salt is heated with con.HNO3 and cobalt nitrate solution. A filter paper is dipped in it and burnt. a) Soluble and no ppt with Na2CO3 b) Insoluble a) Blue surrounded by green b) Brick red c) Crimson red d) Bluish white e) Grassy green on prolonged heating a) Green ash b) Blue tinted ash c) Pale pink ash a) Pre. of NH4+ a) Evolution of Colourless, odourless gas with brisk effervescence, turns limewater milky. b) Smell of vinegar a) Pre. of carbonates b) Pre. of Pb2+ a) Pre. of Cu2+ b) c) d) e) Pre. of Ca2+ Pre. of Sr2+ Pre. of Pb2+ Pre. of Ba2+ a) Pre. of Zn2+ b) Pre. of Al3+ c) Pre. of Mg2+ SYSTEMATIC ANALYSIS OF ANIONS : 1) Dil.H2SO4 test : To the salt add dil.H2SO4, warm if required. b) Pre. of acetate 2) Conc.H2SO4 test : Treat a small quantity of the salt with Conc.H2SO4, warm if necessary. a) Colourless gas with pungent smell, give dense white fumes when a glass rod dipped in NH4OH is shown. b) Brown gas with pungent smell c) Violet vapours with pungent smell d) Light brown gas with pungent smell on strong heating. e) Smell of vinegar Brown fumes 3) Paper ball test : Heat a little of the salt with Conc.H2SO4 and introduce a paper ball to it. 4) Test for sulphates : White ppt insoluble in Heat a little of the salt solution Conc.HCl with dil.HCl and add BaCl2 solution. 5) Test for phosphates : Yellow ppt Add Conc.HNO 3 to the salt solution and boil. Add exess of ammonium molybdate solution and boil again. a) Pre. of Cl-1 b) Pre. of Br-1 c) Pre. of I -1 d) Pre. of NO 3-1 e) Pre. of CH3COO-1 Pre. of NO 3-1 Pre. of sulphate Pre. of phosphate CONFIRMATORY TEST FOR ANIONS : 1) Carbonates : Magnesium sulphate test : To the salt solution add MgSO 4 solution. 2) Chlorides : a) MnO2 test : Heat a small quantity of salt with Conc.H2SO4 and MnO2 . White ppt a) Greenish yellow gas with pungent smell Pre. of carbonates confirmed Pre. of chloride confirmed b) Chromyl chloride test : Salt is heated with conc.sulphuric acid and pot.dichromate. The vapours are collected and passed through NaOH solution. Add lead acetate solution to this. c) Silver nitrate test : Acidify the salt solution with dil.nitric acid and add silver nitrate solution. 3) Acetates : a) Oxalic acid test : Make a paste of the salt with oxalic acid. Rub the paste and smell. b) Ester test : To the salt add conc.H2SO4 and heat. Add alcohol. Shake. Pour the contents into a beaker containing water. c) Ferric chloride test : To the salt solution add neutral ferric chloride solution. Filter. Divide the filtrate into two portions : I. To one add dil.HCl. II. To the second, add water and boil 4) Sulphate : a) To the salt solution add dil.HCl and barium chloride solution. b) To the salt solution add acetic acid and lead acetate solution. 5) Phosphate : a) Ammonium molybdate test : To salt solution add conc.HNO3 and boil. Add ammonium molybdate and b) Reddish brown vapours Yellow solution Pre. of chloride confirmed Yellow ppt c) White curdy ppt soluble in excess of NH4OH Pre. of chloride confirmed a) Smell of vinegar Pre. of acetate b) Pleasant fruity smell Pre. of acetate confirmed c) Reddish coloured ppt Pre. of acetate confirmed I. II. Reddish colour disappears Reddish ppt White ppt insoluble in HCl Pre. of sulphate confirmed White ppt soluble in hot Pre. of sulphate confirmed ammonium acetate a) Yellow ppt Pre. of phosphate heat again. b) Magnesia mixture test : To the salt solution add magnesia mixture and allow to stand. 6) Bromide : a) To salt add conc.H2SO4 and MnO2 b) To salt add dil.HCl and AgCl 7) Nitrate : a) To a little salt add conc.H2SO4 and add cu turnings and heat. b) To salt solution add fresh FeSO4 and cool. Add conc.H2SO4 b) White ppt Pre. of phosphate confirmed. a) Dense brown fumes b) Pale yellow ppt partially soluble inNH4OH Pre. of bromide confirmed a) Brown vapours and green solution b) Brown ring at the junction between two layer. Pre. of nitrate confirmed Pre. of bromide confirmed Pre. of nitrate confirmed ANALYSIS OF CATIONS: 1) To the salt solution add sodium No ppt carbonate solution 2) To the solution add dil. HCl White ppt 3) To the solution add dil. HCl and pass H2S 4) To the solution add solid ammonium chloride and excess of ammonium hydroxide 5) To the solution add solid ammonium chloride and excess of ammonium hydroxide. Pass H2S 6) To the solution add solid ammonium chloride and excess of ammonium hydroxide. Add ammonium carbonate solution 7) To the solution add solid ammonium chloride and excess of ammonium hydroxide. Add sodium hydrogen phosphate Black ppt White gelatinous ppt Pre. of zero group (Ammonium) Pre. of group 1 (Pb2+) Pre. of group 2 (Cu2+) Pre. of group 3 (Al3+) White ppt Pre. of group 4 (Zn2+) White ppt Pre. of group 5 (Ba2+,Sr2+,Ca2+) White ppt Pre. of group 6 (Mg2+) ANALYSIS OF GROUP 0(AMMONIUM) 1) To the salt solution add NaOH solution. Warm Smell of ammonia. Gives white dense fumes when a glass rod dipped in HCl is introduced. Brown ppt Pre. of ammonium confirmed 1) Potassium iodide test : To the salt solution add KI solution Yellow ppt Pre. of lead confirmed 2) Potassium chromate test : To the salt solution add k2CrO4 solution Yellow ppt Pre. of lead confirmed Chocolate coloured precipitate Pre. of Cu2+ confirmed White ppt Pre. of Cu2+ confirmed Deep blue colour Pre. of Cu2+ confirmed Blue ppt floating in colourless solution Pre. of aluminium confirmed White ppt soluble in excess of NaOH Pre. of aluminium confirmed 2) To the salt solution add NaOH solution. Warm. Add Nesslers reagent Pre. of ammonium confirmed ANALYSIS OF GROUP 1(LEAD) ANALYSIS OF GROUP 2(Copper) 1) To the salt solution add few drops of potassium ferrocyanide solution and acetic acid. 2) To the salt solution add acetic acid and potassium iodide solution. 3) To the salt solution add NH4OH solution. ANALYSIS OF GROUP 3(Aluminium) 1) The white ppt obtained is dissolved in dil.HCl Add 2 drops of blue litmus solution. Then add ammonium hydroxide dropwise till blue colour develops. 2) Add excess of NaOH to the salt solution 3) Ash test is conducted with the group ppt Blue ash Pre. of aluminium confirmed ANALYSIS OF GROUP 4(Zn2+) 1) The white ppt obtained in gp.4 is dissolved in dil.HCl And divided into two a) To one part add NaOH in drops b) To the second part add pot.ferrocyanide solution 2) Ash test is conducted with the group ppt a) White ppt soluble Pre. of Zn2+ confirmed in excess of NaOH b) White/bluish Pre. of Zn2+ confirmed white ppt Green ash Pre. of Zn2+ confirmed ANALYSIS OF GROUP 5(Ba2+,Sr2+,Ca2+) Test for Ba : Potassium chromate test : 1) To the salt solution add K2CrO4 solution. 2) Flame test is conducted with the group ppt. Test for Sr : 1) Add ammonium sulphate to the salt solution. 2) Flame test is conducted with the group ppt. Test for Ca : 1) To the salt solution add ammonium oxalate solution. 2) Flame test is conducted with the group ppt. 1) Yellow ppt Pre. of Ba confirmed 2) Grassy green flame Pre. of Ba confirmed 1) White ppt Pre. of Sr confirmed 2) Crimson red flame Pre. of Sr confirmed 1) White ppt Pre. of Ca confirmed 2) Brick red flame Pre. of Ca confirmed 1) White ppt Pre. of magnesium confirmed 2) Pale pink ash Pre. of magnesium confirmed ANALYSIS OF GROUP 6(Mg2+) Test for Mg2+ : 1) To the salt solution add ammonium phosphate solution. 2) Ash test is conducted with group ppt