HANDBOOK OF PREPARATIVE INORGANIC CHEMISTRY
1 LABORATORY SAFETY RULES AND FIRST AID 1 Introduction 1 Classification of Hazards in a Chemistry Laboratory 1 General Chemistry Safety and Laboratory Rules 3 Safety Symbols 7 First Aid in Chemistry Laboratory 7 2 CALIBRATION OF APPARATUS 11 Introduction 11 Sample Problem 14 Viva Voce Questions 14 3 VOLUMETRIC ANALYSIS 15 Introduction 15 Standard Solution 16 Indicator 16 Types of Titration 17 Units of Concentration in Volumetric Analysis 17 Calculation in Titration 21 Know Your Volumetric Apparatus 22 Cleaning of Titration Apparatus 26 Acid–Base Titration 26 Detection of End Point: Acid–Base Indicators 27 Titration Curve 30 Experiment 31: Determination of strength of sodium hydroxide (NaOH) solution volumetrically 33 Experiment 32: Determination of strength of sodium carbonate (Na2CO3) solution using standardized HCl (~N/20) 35 Experiment 33: Determination of strength of sodium carbonate and sodium bicarbonate present together in the mixture by titrating against HCl solution (~N/20) 38 Experiment 34: Determination of strength of sodium carbonate and sodium hydroxide present together in the mixture by titrating against HCl solution (~ N/20) 43 Experiment 35: Determination of the amount of free alkali present in different soaps/ detergents 48 Experiment 36: Determination of total alkalinity in water samples from different sources 51 Redox Titration 54 Redox Titration Curve 55 Detection of the End Point in Redox Titration 58 Experiment 37: Determination of strength of oxalic acid solution by titrating against potassium permanganate solution 60 Experiment 38: Determination of strength of Mohr’s salt solution (ferrous ammonium sulphate) by titrating against KMnO4 solution 63 Experiment 39: Determination of number of water molecules of crystallization in Mohr’s salt 66 Experiment 310: Determination of strength of Mohr’s salt solution by titrating against potassium dichromate using diphenylamine 68 Experiment 311: Determination of strength of Mohr’s salt solution by titrating against K2Cr2O7 using N-phenylanthranilic acid 71 Experiment 312: Determination of strength of oxalic acid and sodium oxalate 74 Experiment 313: Determination of content of iron present in the given ore by titrating against K2Cr2O7 77 Iodimetric and Iodometric Titrations 80 Experiment 314: Determination of strength of copper sulphate solution iodometrically 82 Experiment 315: Determination of strength of K2Cr2O7 solution iodometrically 86 Experiment 316: Determination of strength of tartar emetic solution iodimetrically 89 Experiment 317: Determination of chlorine in commercial sample of bleaching powder iodometrically 92 Experiment 318: Determination of dissolved oxygen (DO) in water sample iodometrically 94 Complexometric Titrations 96 Experiment 319: Determination of strength of Mg2+ ions or magnesium sulphate complexometrically by titrating against EDTA solution using Eriochrome black-T 101 Experiment 320: Determination of strength of Zn2+ ions or zinc sulphate complexometrically by titrating it against EDTA using Eriochrome black-T 105 Experiment 321: Determination of total, temporary and permanent hardness of water complexometrically using Eriochrome black-T 108 Experiment 322: Determination of strength of solution of Ca2+ ions as calcium carbonate (CaCO3) complexometrically by titrating against EDTA using Eriochrome black-T 112 Experiment 323: Determination of strength of Ca2+ ions present in the given milk sample by EDTA back titration 115 Experiment 324: Determination of strength of Zn2+ ions complexometrically by titrating against EDTA using xylenol orange 118 Experiment 325: Determination of strength of Al3+ ions by EDTA back titration 120 Experiment 326: Determination of strength of Mg2+ and Zn2+ ions by titrating against EDTA solution using Eriochrome black-T and xylenol orange 123 Experiment 327: Determination of strength of Mg2+ and Al3+ ions in the mixture by titrating against EDTA using masking agent 127 Experiment 328: Determination of strength of Ba2+ ions 131 Precipitation Titrations 134 Solubility Product: Basis for Precipitation Titrations 134 Common Ion Effect 135 Titration Curve for Precipitation Titration 135 Experiment 329: Determination of strength of sodium chloride solution using Mohr’s method 138 Experiment 330: Determination of strength of silver nitrate solution using Volhard’s method 140 Experiment 331: Determination of strength of sodium chloride solution using Fajan’s method 142 Viva Voce Questions 145 4 GRAVIMETRIC ANALYSIS 148 Introduction 148 Steps Involved in Gravimetric Analysis 148 Know Your Gravimetric Analysis Apparatus 148 Precipitation Method in Gravimetric Analysis 150 Colloidal Precipitate 151 Experimental Section 156 Experiment 41: Estimation of Ni(II) ions as dimethylglyoximato nickel(II) complex solution using dimethylglyoxime (DMG) gravimetrically 156 Experiment 42: Estimation of copper as CuSCN gravimetrically 159 Experiment 43: Estimation of iron as iron(III) oxide (Fe2O3) gravimetrically 161 Experiment 44: Estimation of Al(III) gravimetrically 159 Viva Voce Questions 166 5 PREPARATION OF INORGANIC COMPOUNDS 168 Introduction 168 Experiment 51: To prepare cuprous chloride from copper (II) sulphate pentahydrate 169 Viva Voce Questions 171 Experiment 52: To prepare manganese(III) phosphate (MnPO4) from manganese(II) sulphate (MnSO4) 171 Viva Voce Questions 173 Experiment 53: To prepare aluminium potassium sulphate 173 Viva Voce Questions 175 Experiment 54: To prepare chrome alum from potassium dichromate 175 Viva Voce Questions 176 Experiment 55: To prepare tetraamine copper (II) sulphate from copper sulphate pentahydrate 176 Viva Voce Questions 178 Experiment 56: To prepare tetraamine carbonato cobalt (III) nitrate complex 179 Viva Voce Questions 180 Experiment 57: To prepare potassium trioxalato ferrate (III) trihydrate complex 180 Viva Voce Questions 183 Experiment 58: To measure conductivity of (a) Tetraamine carbonato cobalt (III) nitrate (b) Tetraaminecopper (II) sulphate (c) Potassium trioxalatoferrate (III) trihydrate and to compare their conductance with M/1000 solution of NaCl, MgCl2 and LiCl3 183 Experiment 59: To prepare cis- and trans-potassium diaquadioxalatochromate (III) complexes 185 Viva Voce Questions 189 Experiment 510: To prepare acetylacetonate complex of Cu2+ 189 Viva Voce Questions 192 Experiment 511: To prepare acetylacetonate complexes of Fe3+ from ferric chloride 192 Viva Voce Questions 193 Experiment 512: Preparation of silver nanoparticles (AgNPs) using silver nitrate solution and their spectroscopic characterization using UV–visible spectrophotometer 193 Viva Voce Questions 196 Experiment 513: Preparation of gold nanoparticles (AuNPs) using citrate reduction method and their characterization using UV–visible spectroscopy 196 Viva Voce Questions 198 Experiment 514: To prepare gold naoparticles using tea leaves or cinnamon 198 Viva Voce Questions 199 Experiment 515: To synthesize ammine complexes of Ni(II) 199 Viva Voce Questions 202 Experiment 516: Synthesis of copper oxalate hydrate complexes: Kinetic vs thermodynamic factors 202 Viva Voce Questions 205 6 QUALITATIVE ANALYSIS OF IONS 206 Introduction 206 Basic Principles of Qualitative Inorganic Analysis 207 Methods of Qualitative Analysis 209 Viva Voce Questions 261 7 CHROMATOGRAPHIC SEPARATION OF IONS 263 Introduction 263 Types of Chromatography 264 Paper Chromatography 266 Experimental Section 270 Chromatographic separation of metal ions 270 Experiment 71(a): To separate and identify Co2+ and Ni2+ ions using ascending paper chromatography (using alizarin as spraying agent) 270 Experiment 71(b): To separate and identify Co and Ni2+ ions using ascending paper chromatography (using DMG as spraying agent) 272 Experiment 71(c): To separate and identify Co2+ and Ni2+ ions using ascending paper chromatography (using PAN as spraying agent) 274 Experiment 72: To separate and identify Co2+, Ni2+, Mn2+ and Zn2+ ions using ascending paper chromatography 275 Experiment 73: To separate and identify Fe3+ and Al3+ ions using ascending paper chromatography 277 Experiment 74: To separate and identify Fe3+, Al3+ and Cr3+ ions using ascending paper chromatography 279 Experiment 75(a): To separate and identify Cu2+ and Cd2+ ions using ascending paper chromatography (using ammonium sulphide as spraying agent) 280 Experiment 75(b): To separate and identify Cu2+ and Cd2+ ions using ascending paper chromatography (using dithiozone as spraying agent) 282 Viva Voce questions 283 8 SPECTROPHOTOMETRIC ANALYSIS 285 Introduction 285 Basic Principles of Spectrophotometry 285 Experimental Section 289 Experiment 81: (a) To determine the wavelength of maximum absorption (?max) (b) To draw the calibration curve 289 Experiment 82: (a) To determine the wavelength of maximum absorption (?max) of the complex formed between Fe2+ and 1,10-penanthroline (b) To draw the calibration curve 292 Experiment 83: To determine composition of the Fe3+–salicylic acid complex by Job’s method 296 Experiment 84: Preparation of silver nanoparticles 299 Experiment 85: Preparation of acetylacetanato complexes of Cu2+ and Fe3+ 299 Experiment 86: Measurement of 10 Dq for [Ti(H2O)6]3+ by spectrophotometric method 300 Viva Voce Questions 305 9 MISCELLANEOUS EXPERIMENTS 306 Experiment 91: Estimation of Cu and Ni in Alloy 306 Experiment 92: Estimation of Cu and Zn in Alloy 307 Experiment 93: Estimation of Analysis of Cement 308 Experiment 94: Estimation of Zinc Oxide (Pigment) 309 Experiment 95: Estimation of Manganese in Steel by Absorption Spectrophotometry 310 Experiment 96: To Determine pH Value Using pH Meter 313 Experiment 97: To Determine pH of Soil Sample 315 Experiment 98: Separation of Cl–, Br– and I– by Ascending Paper Chromatography 316 Experiment 99: To Estimate Copper (II), Calcium (II) and Chloride Ions 317 Viva Voce Questions 318 10 PREPARATION OF INORGANIC REAGENTS 319 Introduction 319 How to Prepare Reagent Solution? 319 General Formula for Calculation of Molar Concentration 320 General Formula for Calculation of Volume of Solution Required for Dilution 320 Preparation of Inorganic Laboratory Reagents 321 Preparation of Dilute Acids and Bases 322 Preparation of Side-Bench Reagents 324 Preparation of Reagents for Qualitative Analysis 326 Preparation of Reagents for Volumetric Analysis 332 Preparation of Special Solutions and Reagents 334