Experiment QA1 Qualitative Analysis Name: Seat No.: Date: Grade: 1. Describe the sample. 2. Report on the solubility of the sample in water. 3. Estimate, using universal test paper, the pH of an aqueous solution of the sample. 4. Heat a small amount of the solid sample in an ignition tube, at first gently and then strongly. Report the observations. 5. Carry out a flame test and report the observations. 6. Report on the action of 2 M H2SO4 on an aqueous solution of the sample. 7. Report on the action of conc. H2SO4 on the solid sample. 8. Report on the action of conc. HNO3 on the solid sample. 9. Report on the action of 2 M NaOH on an aqueous solution of the sample. 10.Report on the action of dilute aqueous NH3 on an aqueous solution of the sample. 11.Report on the action of a few drops of 0.2 M KMnO4 in 2 M H2SO4 on an aqueous solution of the sample. 12.Report on the action of zinc and 2 M H2SO4 on an aqueous solution of the sample. From the result of the above tests, deduce which cation(s) and anion(s) may be present in the solid sample. P.1 Experiment QA1 Qualitative Analysis 1. Describe the sample. Solid, liquid, gas. e.g. i. Green solid. ii. Brown solution. iii. White crystalline solid. iv. Colourless liquid. v. Blue liquid. vi. Yellow viscous liquid. Colour Inference Red HgO, Ag2CrO4, Cu2O Orange Cr2O72- Yellow AgI, AgBr, Fe3+(dil.) Green CuCO3, Fe2+, Cr3+ Blue Cu2+ Purple MnO4- Brown Fe3+(conc.) Black CuO, MnO2, CuS, PbS Pink Co2+ White Most compounds. Probably does not contain a transition metal 2. Report on the solubility of the sample in water. e.g. i. ii. Very soluble. Soluble. iii. Slightly soluble. iv. Insoluble. 1. All salts of group I cations and NH4+ are soluble. 2. All nitrates are soluble. 3. All ethanoates are soluble. 4. All sulphates are soluble except those of Ba2+, Ca2+, Sr2+ and Pb2+. 5. All chlorides/bromides/iodides are soluble except those of Ag+, Cu+, Pb2+ and Hg22+. 6. All carbonates/phosphates/sulphites are insoluble except those of group I cations and NH4+. 7. All hydroxides are insoluble except those of group I cations, NH4+, Sr2+ and Ba2+. 8. All sulphides are insoluble except those of group I and group II cations and NH4+. P.2 Experiment QA1 Qualitative Analysis 3. Estimate, using universal test paper, the pH of an aqueous solution of the sample e.g. i. pH = 2 ii. pH = 7 iii. pH = 13 iv. pH = 9.5 4. Heat a small amount of the sample in an ignition tube, at first gently and then strongly. Report the observations. e.g. i. ii. Gas evolved. Pungent gas evolved. iii. Brown gas evolved. iv. Sublimation. v. Decrepitation. (spitting and cracking) vi. Charring. (carbon produced) vii. Colourless liquid condenses on cooler parts of tube. Observation Inference Sublimation. NH4+ salts. Decrepitation, Anhydrous salts that decompose with evolution of gas. spitting and cracking. e.g. Pb(NO3)2, KMnO4. Charring. CH3COO-, C2O42-. (carbon produced) Gas evolved which O2 produced by decomposition of oxide or nitrate. relights a glowing splint. Gas evolved which turns CO2 produced by decomposition of carbonate or lime water milky. hydrogencarbonate. Gas evolved which burns CO from decomposition of oxalate. with a blue flame. Brown gas evolved. NO2 from a nitrate or Br2 from a bromide. Colourless liquid Probably water from the decomposition of a hydrate, condenses on cooler parts a hydroxide or a hydrogencarbonate. of tube. Pungent gas evolved NH3 from decomposition of ammonium salt. which is alkaline. P.3 Experiment QA1 Qualitative Analysis 5. Carry out a flame test and report the observation. Flame colour Inference Persistent yellow Na+ Lilac K+ Ca2+, Sr2+, Li+ Red/Orange 6. Pale green Ba2+ Greenish blue Cu2+ Report on the action of 2M HCl/2M H2SO4 on an aqueous solution of the sample. Observation Inference Gas evolved which turns lime water milky. Gas evolved has a pungent smell, is acidic and turns dilute KMnO4 colourless. CO2 from CO32- or from HCO3SO2 from SO32- Gas evolved smells with bad eggs and gives a black precipitate with lead nitrate H2S from S2- solution. Pungent acidic gas is evolved and a pale yellow precipitate forms. SO2 or S from S2O32NO2 from NO2- Dark brown acidic gas evolved. Pale green gas evolved which bleaches Cl2 from ClO- indicator. Acidic gas evolved which smells of CH3COOH from CH3COO- or vinegar. HCOOH from HCOO- P.4 Experiment QA1 Qualitative Analysis 7. Report on the action of conc. H2SO4 on the solid sample. e.g. i. Colourless gas evolved. ii. Brown fumes evolved. Observation Inference Pale yellow vapour. Possibly HNO3 vapour from NO3- Steamy fumes evolved which give dense HCl from Cl- white smoke with NH3(g). Brown-orange fumes. Br2 from Br- Purple fumes. I2 from I- Gases evolved which burn with a blue CO and CO2 from C2O42- flame and turn lime water milky. Gas evolved which burns with a blue CO from HCOO- flame. 8. Report on the action of conc. HNO3 on the solid sample. e.g. i. Brown fumes evolved. (most reducing agents such as C, S, SO32-) ii. Black precipitate. (Inference: I-) (I- + NO3- + 2H+ I2 + NO2 + H2O) 9. Report on the action of 2 M NaOH on an aqueous solution of the sample. e.g. i. A blue gelatinous precipitate forms. ii. A white gelatinous precipitate soluble in excess NaOH. iii No precipitate at any stage. Observation Inference Mg2+, Al3+, Zn2+ White gelatinous precipitate. Dirty green gelatinous precipitate. Fe2+ Reddish brown gelatinous precipitate. Fe3+ Pale blue gelatinous precipitate. Cu2+ Dark brown precipitate. Ag+ White powder gelatinous precipitate Pb2+ Na+, K+, NH4+ No precipitate. Note: Al(OH)3, Zn(OH)2 and Pb(OH)2 are soluble in excess 2M NaOH. P.5 Experiment QA1 Qualitative Analysis 10. Report on the action of dilute aqueous NH3 on an aqueous solution of the sample. e.g. i. White precipitate formed. ii. Initial pale blue precipitate which dissolves to form deep blue solution. Observation White gelatinous Inference Action of excess NH3 on precipitate Mg2+/Al3+ Insoluble precipitate White gelatinous Zn2+ precipitate ppt dissolves to form colourless solution Pb2+ Insoluble Dirty green precipitate Fe2+ Insoluble Reddish brown Fe3+ Insoluble Cu2+ ppt dissolves to form deep blue White powderly precipitate precipitate Pale blue precipitate solution Dark brown precipitate Ag+ ppt dissolve to form colourless solution 11. Report on the action of a few drops of 0.2 M KMnO4 on an aqueous solution of the sample. e.g. i ii. No visible change. The acidified KMnO4 solution is turned from purple to colourless. (This indicates that the sample is a reducing agent) 12. Report on the action of zinc and 2M H2SO4 on an aqueous solution of the sample. e.g. i. ii. No visible change. The aqueous solution of the sample decolourized. iii. Colour of solution changes from orange to green. N.B. Any positive result shows that the sample is an oxidizing agent. P.6 Experiment QA1 Gas Colour Qualitative Analysis smell Test Burns with a ‘pop’ Hydrogen Colourless Odourless Equations 2H2+O2 2H2O sound Oxygen Colourless Odourless Relights glowing splint Carbon dioxide Colourless Odourless Turns lime water milky CO2+Ca(OH)2 CaCO3 +H2O Colourless Odourless Burns with blue flame 2CO+O2 2CO2 Carbon monoxide a. turns red litmus blue Pungent Ammonia Colourless b. forms white fumes NH3+HCl NH4Cl smell with HCl Hydrogen Irritating forms white fumes with smell NH3 Choking Turns blue litmus red yellow smell and then bleaches it Reddish Choking Turns blue litmus red smell and then bleaches it Colourless chloride Greenish Chlorine Bromine brown NH3+HCl NH4Cl Cl2+H2O HCl+HOCl Br2+H2O HBr+HOBr Choking Iodine violet Turns starch blue smell Turns acidified Sulphur Cr2O72-+14H++6e- 2Cr3+ Sulphur Colourless dioxide potassium dichromate smell green Nitrogen +7H2O SO2+2H2O 4H++SO42-+2e- Pungent brown dioxide Turns blue litmus red smell Nitrogen Forms brown fumes in Colourless Odourless monoxide 2NO+O2 2NO2 air Turns anhydrous Water Colourless Odourless copper(II) sulphate vapour blue P.7 CuSO4+5H2O CuSO45H2O