Experimental Methods in Inorganic Chemistry

JOHN TANAKA University of Connecticut

STEVEN L. SUIB University of Connecticut

P r e n t i c e H a l l , U p p e r S a d d l e R i v e r , New J e r s e y 0 7 4 5 8

TABLE OF CONTENTS

Part I Background Material 1

2 Safety in the Chemical Laboratory 6 Laboratory Notebooks 8 Laboratory Glass and Laboratory Glassblowing 21 Heating and Cooling 31 Handling Air and Moisture Sensitive Compounds 34 Chromatography 38 Thermal Analysis 41 Infrared Spectroscopy 47 Magnetic Susceptibility 58 Mass Spectrometry 65 Nuclear Magnetic Resonance 73 X-Ray Diffraction 89 Electron Paramagnetic Resonance 93 Computational Chemistry 105 Structural Inorganie Chemistry

Part II Laboratory Exercises 121

122 Crystal Growth in Gels 128 Structural Inorganie Chemistry via Models - Session One 140 Structural Inorganie Chemistry via Models - Session Two 156 Sodium Peroxoborate 161 Measurement of High Temperatures 165 Preparation of Phosphors 169 Copper(II) Oxide 175 Structural Inorganie Chemistry via Models - Session Three 192 Brücke and Magnesia 198 Strontium Zincate(II) 201 Cadmium(II) Iodide 205 Manganese(IV) Oxide 208 Pillared Clays

TABLE OF CONTENTS

215 Potassium Nitrilosulfonate 220 Tin(IV) Chloride 227 Surface Conductive Glass 231 Copper(I) Chloride 235 Mercury(II) Tetrathiocyanatocobaltate 238 Synthesis of a Superconductor 243 12-Tungstophosphoric Acid 246 Copper Compounds 249 Potassium Trifluoronickelate(II) 254 Potassium Trifluoromagnesate 259 Potassium Iodate and Clock Reaction 263 Ethylenediamine Complexes of Cobalt and Nickel 268 Ethylenediamine Complexes of Chromium 272 Hexaammine Cobalt(III) Chloride 275 Chloropentaamminecobalt(III) Chloride/

Nitropentaamminecobalt(111) Chloride 279 Ferrocene 285 Phase Diagram of an Alloy 294 Metal Complex Used for DNA Cleavage 300 Synthesis of* Heterogeneous Catalysts and Catalyst Supports 305 Preparation of a Zeolite, B/Al ZSM-11 312 Molecular Modeling Computational Laboratory

Part III Characterization Techniques 321

322 Conductivity oflonic Solutions 331 Measurements of Magnetic Susceptibility 337 Absorption Spectra of Transition Metal Complexes 345 X-Ray Powder Diffraction of Pillared Clays 348 Luminescence Spectroscopy 355 X-Ray Photoelectron Spectroscopy 372 Calibration of Vacuum Line Components 379 Characterization of a Gaseous Unknown

Index 389

TABLE OF CONTENTS