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 07458
 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