11puc 6. SYSTEMATIC QUALITATIVE ANALYSIS OF SIMPLE INORGANIC SALTS Analysis of salts means identification of cations and anions present in the salt, Salt is formed by the neutralization reaction between an acid and a base. The No. of units of charges carried by an ion is equal to its valency, Acid Radicals (Anion) Basic Radicals (Cation) 1) They carry -ve charge 2) They can be detected by using solid (0.12) salt 3) They can be detected in Acidic medium with Pfc? 4) Reaction can be seen in the form of effervescence, colour and odour of gas, 1) They carry +ve charge 2) They can be detected by using original solution (2.or3 drops) 3) They can be detected in Basic medium with PM>7 4) Reaction can't be seen instead the product will be seen as precipitate, Analysis of a salt involves four steps which are as follows: 1. Preliminary test 3. Detection of cation 1.Preliminary Tests: a) State : Crystalline or Amorphous 2. Detectionofanion 4, Reportof salt b) Colour : White / colourless, light green (Fe), green (Ni*), Blue (Cu), Brown (Fe), light pink(Mn”), Violet(Co™). ¢) Solubility test : ‘Water dil. HCL dil. HNO, Hot Hot Cold Hot I. Classification of Anion (Acid Radicals). Group Group Reagent Radicals present I dil, H,SO,/ dil, HCL co,* ul Cone. H,SO, Cl. Br, NO, as n No reagents so,?| m. Detection of 1 group anion Experiment Observation Inference Salt + dil. H,SO, dil. HCL effervescence liberating I group Carbonate anion (CO,") Experiment (heat if necessary) colourless, odourless gas which | may be present tums lime watermilky Confirmatory test for Carbonate ion (CO,") (lime water test). Inference Observation Salt + Water, boil the gas liberated is passed into the test tube containing lime water Lime water does not tums milky Carbonate anion (CO,*) is confirmed ‘Detection of II group anions. a. Salt + conc.H,SO, is taken inadry testtube. a. A colourless pungent smell ‘gas which gives dense white fumes with glass rod dipped in NH,OH is exposed to the mouth of the test tube b) White fumes followed by Reddish brown pungent fumes II group chloride ion (CI) may be present Bromide ion (Br) may be present b. Ifno reaction in cold a piece of Cu/ Paper ball is added to the test tube and heated Reddish brown fumes are evolved Nitrate anion (NO, ) may be Present ‘Confirmatory test for Chloride ion (CI) (Chromyl chloride test). Salt +K,Cr,0, crystals in a dry testtube + cone.H,SO,, The above vapours are passed into a test tube containing NaOH solution To the above yellow solution + acetic acid + lead acetate solutions areadded (Orange red vapours are evolved Yellow solution is obtained Bright yellow precipitate Chloride anion (C1) is confirmedupuc Silver Nitrate test for Chloride ion (C1) Salt solution +AgNO, solution Curdy white ppt. which is | Chloride ion (CI)is confirmed Soluble in excess of NH,OH Confirmatory test for Bromide ion (Br) (Globule test). | Experiment Observation Inference Salt + Water shaken to dissolve | An orange red globule is + Cl, water + 3 drops of CCl, | formed the mixture is shaken well Bromide ion (Br’) is confirmed Silver Nitrate (AgNO, ) test. | Salt solution +4 gNO, solution Pale yellow ppt. which is | Bromide ion(Br’)is confirmed sparingly soluble in NH,OH Confirmatory test for Nitrate ion (NO, ’) (Brown ring test). Salt solution + equal volume of | A brown ring is formed at the | Nitrate ion (NO,) is confirmed freshly prepared FeSO, solution | junction of two liquids + few drops of cone. H, SO,are added slowly along the sides of thetesttube. Detection of III group anion ‘Test for sulphate ion (SO, *). Experiment Observation Inference Salt solution + BaCl, solution | Athickwhiteppt. isobtained | 111 group Sulphate ion (SO,2) is Above ppt. +excessofdil. HCI | Precipitate is insoluble Presentand confirmed Detection of Cations (Basic radicals); The detection of basic radicals of salt is based on the Precipitation reaction in solution. Hence it isnecessary to prepare the solution of salt or original solution (0.8) Preparation of original solution (OS): The salt may be soluble in H,O or dil.HC1 or dil HNO, The choice of the solvent to prepare original solution is known from solubility test under preliminary test. Preparation ; About % test tube of solvent is taken and the salt is added little by little with constant shaking until a saturated clear, homogeneous solution is obtained. | Note: Always use 2 or 3 drops of original solution for the detection of basic radicals. “16CLASSIFICATION OF CATIONS (BASIC RADICALS) Group No. Cations present Group reagent Nature of precipitate oO NH,’ No reagent aiLHCL diLHCL+ HS gas Al % NH,Cl,, + excess NHOH Hydroxide precipitate NH,Cl,, + excess Mn" NH,OH +H, gas Zn", Sulphide precipitate NH,Cl, + excess 2 ge cat Ba", Sr7& Ca NILOM + ONH),CO, Carbonate precipitate Mg” ‘No reagent Detection of ‘zero’ group cation. Ammonium ion (NH,”)- Experiment Observation Inference Pungent smell of NH, gas is evolved which gives dense white fumes with glass rod dipped in Cone. HCI solution Salt+ dil. NaOH solution heat Ammonium. ion (NH,) may be present Confirmatory test for Ammonium ion (NH,). Nessler’s reagent test = Brown precipitate is formed As OS + Nessler’s reagent +NaOH (slightexcess) Ammonium ion (NH,) is confirmed Analysis of I group cations OS+dil, HCI | No precipitate I group cations are absent Analysis of IT group cations Experiment Observation Inference OS + dil. HCI+H,S No precipitate Ugroup cations are absent Analysis of III group cations (AI") Experiment Observation Inference A. gelatinous white precipitate is formed OS + a spatula of solid NH,Cl + excess of NH,OH solution, Ul group Aluminium ion( AI”) may be present ——___ |upuc Confirmatory test for Aluminium ion (AP) a) OS + dil, NaOH, first small || quantity, followed by exc Above clear solution + solid NH,Cl, boil & cool under tap water drops of NH,OH A white gelatinous ppt. soluble in excess of NaOH giving a clear solution White gelatinous ppt. reappears b) OS + blue litmus solution + | 4 blue floating mass is formed Aluminium ion (AI) is confirmed Aluminium ion (AI™) is confirmed Analysis of IV group cations (Zn, Mn’). OS + one spatula of solid NH.Cl + excess of NHOH solution +H,S A white or flesh coloured precipitate is formed, IV group cations ( Zn“or Mn”) may be present Confirmatory test for Zinc ion (Zn"). 1. OS+dil. NaOH 2. OS+K,[Fe(CN), | ‘Awhite ppt, soluble in excess of NaOHis formed A bluish White precipitate is formed Zinc ion (Zn™) is confirmed Zincion(Zn™)is confirmed Confirmatory test for Manganous ion (Mn"). 1, OS+ dil. NaOH 2. Permanganic acid test (HMn0,) Few drops of OS + Pinch of White ppt. is obtained which slowly turns into brown on exposure to air A pink supernatant solution is Manganous ion (Mn‘) is confirmed ion (Mn™) NH,OH solution + (NH),CO, solution in Manganous is PbO, + 1 mL Conc. HNO, | obtained confirmed boil the mixture cool, dilute & decant the solution Analysis of V group cations (Ba”, Sr”, Ca”) OS + solid NH,Cl + excess of | White precipitateis formed | V group cations may be present Confirmatory test for Barium ion (Ba 1, OS + Pot.chromate (K,CrO,) solution 2. Flame test : A paste of the given salt is prepared with a few drops ofconc, HClandit is exposed 0 the colourless flame through Platinum wire A yellow precipitate is formed Apple green colour is imparted totheflame Barium ion(Ba”)is confirmed Barium ion(Ba™)is confirmedConfirmatory test for Strontium ion (Sr). mPpuc 1. OS + (NH),SO, . heat and | A white precipitateisformed — | Strontium) on (sr?) is scratch the sides of test tube confirmed witha glassrod 2.Flame Test; . A paste of the given salt is | Crimson red colour is imparted | Strontium jen (Sr) ts prepared with few drops Of 4o the flame confirmed cone, HCI and it is exposed to the colourless flame through Ptwire Confirmatory test for Caleium ion (Ca). 1. OS + Ammonium oxalate | Awhiteprecipitate isformed | Calcium ton is (NHY).C,O, ) confirmed 2.Flame Test ‘A paste of the given salt is | Brick red colour is imparted to /Caleium ion (Ca) is prepared with few drops of | the flame confirmed cone. HC! and it is exposed to the colourless flame through Ptwire ‘Analysis of VI group basic radical Magnesium ion (Mg” ). (OS + solid NH,CI + excess of ] White crystalline precipitate is | Magnesium ion (Mg™) is NH,OH + Na,HPO, or| formed confirmed. (NH),HPO, , scratch the inner walls of test tube with a glass rod NoTE: FLAME TEST Metal chlorides are volatile and impart characteristic colour to the flame. Hence flame test is always done by using cone, HCI solution A paste of the salt is prepared | Apple Green Ba? in cone. HCl on a watch glass. It isheated on acleaned pt, loop in |__Brick Red Cr non luminous Bunsen flame. | Grimson Red = The colour given out by the salt S Sr inthe flame is observed Green cu Preparation of Nessler’s reagent : Alkaline potassium mercuric iodide solution is called Nessler’s reagent. I epared fi called Nessler’s reagent. It is prepared from HgC,& KI solution pepe When drops of KI are added to H gC, scarlet red ppt. is formed which dissolves in excess of KI giving a clear solution, To the clear solution an equal volume of NaOH is added, The resulting solution is called Nessler’s reagent. HgCl,+ 2KI > Hgl, + 2KCI K, Hgl,+ NaOH — Nessler’s reagent. Hgl,* 2KI— K, Hel, Potassium mercuric iodide 19,