(For B.Sc. Second Year of All Indian University) (PART - II) Dr. FATEH BAHADUR M.Sc., Ph.D. (B.H.U.)

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PRACTICAL CHEMISTRY (For B.Sc. Second Year of All Indian University) (PART - II) Dr. FATEH BAHADUR M.Sc., Ph.D. (B.H.U.) Ex. Head, Department of Chemistry K.N. Govt. P.G. College Gyanpur, Sant Ravidas Nagar, BHADOHI (U.P.) Principal, Ram Lalit Singh Mahavidyalaya Kailhat, Chunar, MIRZAPUR (U.P.) 2011-12 E D I T I O N Future for WINNERS VISHAL PUBLISHING CO.

Exp. No. CONTENTS SECTION - 1 INORGANIC CHEMISTRY EXPERIMENTS A. VOLUMETRIC ANALYSIS Pages 1. Estimation of calcium content in chalk (CaCO 3 ) as calcium oxalate by permanganometric method.... 3 2. Estimation of ferrous (Fe 2+ ) and ferric ions (Fe +3 ) in the given mixture by dichromate method....6 3. Estimation of copper using thiosulphate soluiton....7 4. Determination of acetic acid in commercial vinegar using NaOH....8 5. Estimation of total, permanent and temporary hardness of water by complexometric method using EDTA (disodium salt of ethylene diamine tetra-acetic acid)....10 6. Determination of the alkali content in antacid tablet using HCl...11 B. GRAVIMETRIC ANALYSIS 1. Estimation of Barium as Barium sulphate....21 2. Estimation of Sulphate as Barium sulphate...23 3. Estimation of Copper as Cupric oxide....26 4. Estimation of Silver as Silver Chloride....28 5. Estimation of Chloride as Silver Chloride....30 6. Estimation of Lead as Lead Chromate....33 7. Estimation of Lead as Lead Sulphate....35 8. Estimation of Iron as Ferric oxide....37 9. Estimation of Aluminium as Aluminium oxide...40 10. Estimation of Zinc as Zinc Oxide....41 11. Analysis of Cu as CuSCN from copper sulphate pentahydrate (CuSO 4. 5H 2 O)...44 12. Estimation of Nickel as nickel-dimethylglyoxime....46

SECTION - 2 ORGANIC CHEMISTRY EXPERIMENTS QUALITATIVE ORGANIC ANALYSIS (Identificaiton of Organic Compounds) 2.1. Preliminary Tests...47 2.2. Detection of Elements...50 2.3. Detection of Functional Groups (Class Determination)...54 2.4. Determinaiton of Melting Point or Boiling Point...62 2.5. Possible Compounds...65 SPECIFIC TESTS OF ORGANIC COMPOUNDS Type-A : Compounds Containing Carbon and Hydrogen (with or without Oxygen) 2.6.1. Carboxylic Acids...69 2.6.2. Alcohols...76 2.6.3. Phenols...81 2.6.4. Aldehydes...87 2.6.5. Ketones...92 2.6.6. Esters...94 2.6.7. Carbohydrates...96 2.6.8. Hydrocarbons...99 Type-B : Compounds Containing Nitrogen (In addition to C, H and O) 2.6.9. Amides...103 2.6.10. Nitro-compounds...107 2.6.11. Amines...112 2.6.12. Anilides...118 Type-C : Compounds Containing Nitrogen and Sulphur (In addition to C, H and O) 2.6.13. Thioamides...120 Type-D : Compounds Containing Halogens (In addition to C, H and O) 2.6.14. Halogen Containing Compounds...121

2.6.15. Specimen of Recording Organic Analysis...124 2.6.16. Viva-Voce (Organic Analysis)...125 SECTION - 3 PHYSICAL CHEMISTRY EXPERIMENTS Transition Temperature 1. To determine the transition-temperature of a hydrated salt (e.g., MnCl 2. 4H 2 O or Na 2 SO 4. 10 H 2 O by thermometric method....135 2. To find out the transition temperature of Glauber s salt (Na 2 SO 4. 10H 2 O) by dilatometric method....137 3. To study the effect of a solute (e.g., NaCl, succinic acid) on the critical solution temperature of two partially miscible liquids (e.g., phenol-water system) and to determine the concentration of that solute in the given phenol-water system....141 4. To construct the phase-diagram of two components (e.g., diphenyl-amine-benzophenone system by cooling curve method....146 Solubility 5. To determine the solubility of benzoic acid at different temperatures and to determine H of the dissolution process....149 Thermochemistry Experiments 6. To determine the heat of neutralization of strong HCl and strong base NaOH....153 7. To determine enthalpy of neutralization of weak acid e.g., acetice acid by strong base sodium hydroxide and also determine the enthalpy of ionisation of weak acid (acetic acid)....155 8. To determine the enthalpy of a solution of solid calcium chloride and calculate the lattice energy of calcium chloride from its enthalpy of solution (enthalpy data) using Born-Haber cycle....158 Surface Tension 9. To determine the surface tension of liquid by drop weight method, at room temperature (by stalogmometer)...165

10. To determine the percentage composition of given mixture of two components A and B by drop weight method (Surface tension method)....168 Viscosity 11. To determine the coefficient of viscosity of the given liquid at room temperature by Ostwald's viscometer....173 12. To determine the percentage composion of the given mixture consisting of two liquids A and B, (non-reacting system) by viscosity method....176 13. To determine viscosity of amylalcohol in water at different concentration....178 Chemical Kinetics 14. To study kinetically the reaction rate of decomposition of iodide by H 2 O 2....181 15. To determine rate constant and order of reaction between acetone and iodine catalysed by mineral acid....184 SECTION - 4 CHROMATOGRAPHY 1. Separation and identification of a mixture of amino acids by paper chromatography....193 2. Separation and identification of the constituents present in the mixture of sugars by paper chromatography....199 3. Separation of Lead and Silver ions by paper chromatography....201 4. Separation and identification of a mixture of amino acids by thin layer chromatography (T.L.C.)...203 5. Separation of mixture of dyes by thin layer chromatography using cyclohexane and ethyl acetate as solvent....205 6. Separation of green leaves pigments from spinach leaves using thin layer chromatography....207 7. Prepare and separate 2, 4-dinitropenyl hydrazones of acetone, 2-butanone hexan-2 and 3-0ne using fouline and light petroleum (40 : 60)...210 Viva-Voce...212 Appendices...214