SALT ANALYSIS SCHEME OF ANALYSIS EXPERIMENT PRELIMINARY EXAMINATIONS : OBSERVATION INFERENCE 1) Noted the colour Colourless Green Pale pink Pink Absence of Min™*,Co™*,Ni2* Pre. of Ni?” Pre. of Co’ 2) Noted the solubility a) Inwater a) Soluble and no a) Pre. of NH.” b) Indil.HCl ppt with Na2CO; b) Insoluble b) Pre. of Pb™ 3) Flame Test: a) Blue surrounded a) Pre. of Cu?” Alittle of the salt is made into by green paste with conc.HCl. A glass rod b) Brick red b) Pre. of Ca” is dipped in it and introduced c) Crimsonred ) Pre. of Sr* into the flame. d) Bluish white d) Pre. of Pb?* e) Grassy greenon e) Pre.of Ba’ prolonged heating 4) Ash Test: a) Green ash a) Pre.of Zn Alittle of the salt is heated with con.HNO:; and cobalt nitrate solution. A filter paper is dipped in it and burnt. b) Blue tinted ash c) Pale pink ash b) Pre. of Al* c) Pre. of Mg” SYSTEMATIC ANALYSIS OF ANIONS : 1) Dil.H,SOxtest : To the salt add dil.H,SO., warm if required. a) Evolution of Colourless, odourless gas with brisk effervescence, turns limewater milky. b) Smell of vinegar a) Pre. of carbonates b) Pre. of acetate2) Conc.H2SO, test : Treat a small quantity of the salt with Conc.H2S0., warm if necessary. 3) Paper ball test : Heat a little of the salt with Conc.H2SO, and introduce a paper ball to it. 4) Test for sulphates : Heat a little of the salt solution with dil. HCl and add BaCl» solution. a) Colourless gas with pungent smell, give dense white fumes, when a glass rod dipped in NH«QH is shown. b) Brown gas with pungent smell ¢) Violet vapours with pungent smell d) Light brown gas with pungent smell on strong heating. e) Smell of vinegar Brown fumes White ppt insoluble in Conc.HC! a) Pre of i? im b) Pre. of Br* c) Pre. of 1 d) Pre. of NOs? e) Pre. of CHsCOO* Pre. of NO;* Pre. of sulphate 5) Test for phosphates : Add Conc.HNOsto the salt solution and boil. Add exess of ammonium molybdate solution and boil again Yellow ppt CONFIRMATORY TEST FOR ANIONS : Pre. of phosphate 1) Carbonates : Magnesium sulphate test : To the salt solution add MgSOx solution. White ppt Pre. of carbonates confirmed 2) Chlorides : a) MnOstest: Heat a small quantity of salt with Conc.H:S0, and MnO; a) Greenish yellow gas with pungent smell Pre, of chloride confirmedb) Chromylchloride test : Salt is heated with ‘conc.sulphuric acid and pot.dichromate. The vapours arecollected and passed through NaOH solution. Add lead acetate solution to this. Silver nitrate test : Acidify the salt solution with dil. nitric acid and add silver nitrate solution. ¢ b) Reddish brown vapours. Yellow solution Yellow ppt c) White curdy ppt soluble in excess of NHsOH Hi Pre. of chloride confirmed Pre. of chloride confirmed 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.H 50x and heat. Add alcohol. ‘Shake, Pour the contents into a beaker containing water. Ferricchloride test : To the salt solution add neutral ferric chloride solution. Filter, Divide the filtrate into two portions : |. Toone add dil.HCl. ll, Tothe 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. q a) Smell of vinegar b) Pleasant fruity smell c) Reddish coloured ppt 1. Reddish colour disappears Reddish ppt White ppt insoluble in HCl White ppt soluble in hot ammonium acetate Pre. of acetate Pre. of acetate confirmed Pre. of acetate confirmed Pre. of sulphate confirmed Pre. of sulphate confirmed 5) Phosphat a) Ammonium molybdate test : To salt solution add conc.HNO; and boil. Add ammonium molybdate and a) Yellow ppt Pre. of phosphateheat again. b) Magnesia mixture test; To the salt solution add magnesia mixture and allow b) White ppt + Pre. of phosphate ci NN b) To salt add dil. HCl and AgCl 7) Nitrate: a) Toalittle salt add to stand. 6) Bromide: a) To salt add conc.H,SO.and a) Dense brown Pre. of bromide confirmed MnO2 fumes b) Pale yellow ppt partially soluble inNH,QH a) Brown vapours Pre. of bromide confirmed Pre. of nitrate confirmed of ammonium hydroxide conc. H:SOxand add cu and green ‘turnings and heat. solution b) To salt solution add fresh b) Browning atthe | Pre. of nitrate confirmed FeSO, and cool. Add junction between conc.H2SO4 two layer. ANALYSIS OF CATIONS: 1) To the salt solution add sodium | No ppt Pre. of zero group carbonate solution (Ammonium) 2) To the solution add dil. HCI White ppt Pre. of group 1 (Pb*) 3) To the solution add dil. HCl and | Black ppt Pre. of group2 pass H)S: (cu) 4) To the solution add solid White gelatinous ppt Pre. of group3 ammonium chloride and excess (ary ammonium chloride and excess of ammonium hydroxide. Add sodium hydrogen phosphate 5) To the solution add solid White ppt Pre. of group4 ammonium chloride and excess (Zn) of ammonium hydroxide. Pass HS. 6) To the solution add solid White ppt Pre. of group 5S ammonium chloride and excess (Ba®*,Sr2*,Ca®*) of ammonium hydroxide. Add ammonium carbonate solution 7) To the solution add solid White ppt Pre, of group6 (Mg”)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 HCI is introduced. Li Pre. of ammonium contirmed 2) To the salt solution add NaOH solution. Warm. Add Nesslers. reagent Brown ppt Pre. of ammonium confirmed ANALYSIS OF GROUP 1(LEAD) 1) Potassium iodide test : Yellow ppt To the salt solution add KI solution Pre. of lead confirmed 2) Potassium chromate Yellow ppt test: To the salt solution add k2CrO, solution ANALYSIS OF GROUP 2(Copper) Pre. of lead confirmed 1) To the salt solution add few Chocolate coloured drops of potassium precipitate ferrocyanide solution and acetic acid. 2) To the salt solution add acetic acid and potassium iodide solution. White ppt Pre. of Cu* confirmed Pre. of Cu®* confirmed 3) To the salt solution add NH,OH | Deep blue colour solution. ANALYSIS OF GROUP 3(Aluminium) Pre. of Cu* confirmed 1) The white ppt obtained is Blue ppt floating in dissolved in dil. HCl colourless solution Add 2 drops of blue litmus solution. Then add ammonium hydroxide dropwise till blue colour develops. Pre, of aluminium confirmed 2) Add excess of NaOH to the salt_| White ppt soluble in solution excess of NaQH Pre. of aluminium confirmed3) Ash test is conducted with the group ppt ANALYSIS OF GROUP 4(Zn7*) Blue ash - — Pre. of aluminium cx Cy 1) The white ppt obtained in gp.4 is dissolved in dilHCl And divided into two a) Toone part add NaOH in drops a) White ppt soluble jin excess of N8OH b) White/bluish Pre. of Zn® confirmed Pre, of Zn** confirmed b) To the second part add white ppt pot.ferracyanide solution 2) Ashtest is conducted with the | Green ash Pre. of Zn” confirmed group ppt ANALYSIS OF GROUP 5(Ba*,Sr’*,Ca**) Test for Ba : Potassium chromate test : 1) To the salt solution add K;CrO, 1) Yellow ppt Pre. of Ba confirmed solution. 2) Flame test is conducted with 2) Grassy green Pre, of Ba confirmed the group ppt. flame Test for Sr: 1) Add ammoniumsulphate tothe | 1) White ppt Pre. of Srconfirmed salt solution, 2) Flame test is conducted with 2) Crimson red Pre. of Srconfirmed the group ppt. flame Test for Ca: 1) To the salt solution add 1) White ppt Pre, of Ca confirmed ammonium oxalate solution. 2) Flame test is conducted with the group ppt. 2) Brick red flame Pre. of Ca confirmed ANALYSIS OF GROUP 6(Mg**) Test for Mig” : 1) Tothe salt solutionadd ammonium phosphate solution. 2) Ash test is conducted with group ppt 1) White ppt 2) Pale pink ash Pre. of magnesium confirmed Pre, of magnesium confirmed