‘Aim: To detect one anion and one cation in the given salt no,_for anion present in it. Theory Qualitative analysis is a method of Analytical chemistry that deals with the determination of elemental composition of inorganic salts. It is mainly concerned with the detection of ions in an aqueous solution of the salt. Two basic principles of great use in the analysis are: (i) Solubility product; and (ii) Common ion effect. Common ion effect: Shift in equilibrium on adding a substance that provides more of an ionic species already present in the dissociation equilibrium. Solubility product: It is product of the ionic concentration in a saturated solution. lonic product: It is the product of ionic concentration at any concentration of the solution. ‘When ionic product of a salt exceeds its solubility product, precipitation takes place. lonic product of salt is controlled by making use of common ion effect. Test of anion involves: Material Required * Boiling tube + Test tubes + Test tube stand + Test tube holder + Filter paper Burner + Reagents Preliminary Test Colour: White Odour: no characteristic odour Deliquescence: no Analysis of Anions: {NOTE*Write in past tense ) Experiment ‘Observation Inference Treated 0.1 g ofsalt with ImL | No effervescence and COs, SOx, S*, NO, dil. H,S0s and warmed. evolution of vapours. CH2COO™ absent. Took 0.1 g of salt ina test Brown fumes evolve which become | Presence of NO: indicated. tube and 3-4 drops of conc. H.S0.. | dense upon heating the reaction mixture after addition of copper turnings and the solution acquires blue colour. Took 1 mL of salt solution in water in| Adark browm ring is formed at the | Presence of NOs-confirmed. atesttube, Add 2 mL conc. of H:S0: | junction of the two solutions, ‘and mix thoroughly. Cooled the mixture under the tap. Added freshly prepared ferrous sulphate along the sides of the test tube without shaking.Test for Nitrate ion [NOs] (To be written on unruled page.) (a) If on heating the salt with cone. H,SOs light brown fumes are evolved then heat a small quantity of the given salt with few copper turnings or chips and conc. HaSOs. Evolution of excess of brown fumes indicates the presence of nitrate ions. The solution turns blue due to the formation of copper sulphate. + NaxSOs+4H20 + 2NO Copper sulphate (Blue) > 2NO2 (Brown fumes) (b) Take 1 mL of an aqueous solution of the salt add freshly prepared ferrous sulphate solution and then add cone. H:S0; along the sides of the test tube dropwise. A dark brown ring is formed at the junction of the two solutions due to the formation of nitroso ferrous sulphate .. NaNO3 + H2SOa -> NaHSOs + HNO3 GFeSO, + 3H)SO, + 2HNOs ->3Fe)(SOx)3. + 4,0 +2NO FeSO, + NO~ -> [Fe(NO)|SOs 2N0. + [oy Nitroso ferrous sulphate (Brown) Analysis of Cation: Experiment Observation Inference Noted the colour of the given salt. White Cu, Fe, NI*,Co*, Mn?* are absent. Prepared a paste of the salt with conc. HCI No distinct colour of the Ca**, Sr°*, Ba®*, Cu* may be and performed the flame test. flame seen absent. Heated 0.1 g of salt with 2 mLNaOH solution. | Ammonia gas is not evolved | NHs° absent. {examined by smell) Took a small amount of original solution(ag. | white precipitate did not | Group-1 cation absent only) and dil, HCl was added, appeare. (Pb absent) ‘Added excess of waterto the same test tube. __| No precipitate appeared. Group-II cations absent Warm the solution and passed HaS gas for 1-2 (Pb, Cur" absent) minutes. Shacked the test tube. Took original solution and added 2-3 drops of |_| No precipitate appeared. Grouprll cations absent conc. HNO3 to oxidise Fe” ions to Fe® ions. Heat (Fe** & AP* absent) the solution for a few minutes. After cooling add a small amount of solid ammonium chloride (NH (CHsCOO)Ba + HO + CO (CHsCOO)Ba + KxCrOs BaCrOs + —-2CHsCOOK Barium chromate (yellow precipitate ) (b) Flame test : Take a platinum wire and dip it in conc. HCI. Heat it strongly until the wire does not impart any colour to the non-luminous flame. Now dip the wire in the paste of the (Group-V) precipitate in conc. Hcl, Heat it in the flame. A grassy green colour of the flame confirms the presence of Ba”* ions. Result The given salt contains: Anion: NOs~ cation : Ba®. Precautions {a) Always use an apron, an eye protector and hand gloves while working in the chemistry laboratory. (b) Before using any reagent or a chemical, read the label on the bottle carefully. Never use unlabelled reagent. (c) Do not mix chemicals and reagents unnecessarily. Never taste any chemical. (4) Be careful in smelling chemicals or vapours. Always fan the vapours gently towards your nose. (e) Always pour acid into water for dilution. Never add water to acid, (f) Be careful while heating the test tube. The test tube should never point towards yourself or towards your neighbours while heating or adding a reagent. {g)Always use the reagents in minimum quantity. Use of reagents in excess, not only leads to wastage of chemicals but also causes damage to the environment.