Synthesis and Technique in Inorganic Chemistry, 3rd edition

Previously by Angelici, this laboratory manual for an upper-level undergraduate or graduate course in inorganic synthesis has for many years been the standard in the field. In this newly revised "third edition," the manual has been extensively updated to reflect new developments in inorganic chemistry. Twenty-three experiments are divided into five sections: solid state chemistry, main group chemistry, coordination chemistry, organometallic chemistry, and bioinorganic chemistry. The included experiments are safe, have been thoroughly tested to ensure reproducibility, are illustrative of modern issues in inorganic chemistry, and are capable of being performed in one or two laboratory periods of three or four hours. Because facilities vary from school to school, the authors have included a broad range of experiments to help provide a meaningful course in almost any academic setting. Each clearly written and illustrated experiment begins with an introduction that highlights the theme of the experiment, often including a discussion of a particular characterization method that will be used, followed by the experimental procedure, a set of problems, a listing of suggested Independent Studies, and literature references.

Table of Contents:
Introduction; Safety; Laboratory Procedures; Research Notebook; Standard References Part I. Solid State Chemistry Experiment 1 – High-Temperature Synthesis of the Superconductor YBa2Cu3O7 Tube Furnace Preparation Superconductivity Iodometric Titrations Experiment 2 – The Layered Solids VOPO4(H2O)2 and VO(HPO4)(H2O)0.5 Powder X-Ray Diffraction Oxidation of Alcohols to Ketones Experiment 3 – The Molecular Sieve Zeolite-X Sol-gel Synthesis High Pressure Synthesis Ion Exchange in Microporous Solids Part II. Main Group Chemistry Experiment 4 – The Borane-Amine Adduct BH3NH2C(CH3)3 Lewis Acids and Bases Experiment 5 – Buckminsterfullerene, C60, and Its Electrochemistry Soxhlet Extraction Cyclic Voltammetry Experiment 6 – Vacuum-Line Synthesis of GeH4 Vacuum Line and Trap-to-Trap Purification Vapor Pressure and Molecular Weight Determination of a Volatile Compound Gas Phase IR Spectroscopy Experiment 7 – Tin Chemistry: Coordination Complexes and Organometallic Derivatives NMR Spectroscopy Linkage Isomerism Experiment 8 – Synthesis of (C6H5)2PCH2CH2P(C6H5)2 in Liquid Ammonia Synthesis in Liquid Ammonia Experiment 9 – Electrolytic Synthesis of K2S2O8 Electrolytic Preparation Part III. Coordination Chemistry Experiment 10 – Ion Exchange Separation of Chromium Complexes Ion Exchange Chromatography Experiment 11 – Metal-Metal Quadruple Bonds Molecular Orbital Theory Experiment 12 – The Magnetic Susceptibility of Mn(acac)3 Magnetism of Transition Metal Complexes The Gouy Method The Evans Methods Experiment 13 – Cobalt Ammines and their Ligand Substitution Kinetics Conductivity of Ionic Complexes Kinetics of Aquation of [Co(NH3)5Cl]2+ Experiment 14 – Optical Resolution of Co(en)33+ Separation of Diastereomers by Crystallization Optical Rotations Suction Filtration Experiment 15 – Metal Dithiolenes and the Use of Quaternary Ammonium Salts Quaternary Ammonium Salts Part IV. Organometallic Chemistry Experiment 16 – The Metal-Arene Complex [1,3,5-C6H3(CH3)3]Mo(CO)3 IR Spectra of Metal Carbonyls Experiment 17 – Organo-iron Chemistry: (C5H5)2Fe2(CO)4 and (C5H5)Fe(CO)2(CH3) Schlenk Line Synthesis Infrared Spectra of Solutions Experiment 18 – The Metal Carbonyl Cluster Fe3(CO)12 Mass Spectrometry Experiment 19 – Microscale Synthesis of Vaska's Complex Microscale Synthesis Solid State IR Spectra Experiment 20 – The Air-Sensitive Sandwich Complex Nickelocene Glove Bag Manipulations Sublimation Part V. Bioinorganic Chemistry Experiment 21 – Cobaloximes: Models of Vitamin-B12 Coenzymes Enzyme Models Experiment 22 – Amino Acid Complexes: Stability Constants of Ni(glycinate)n(2 - n)+ Amino Acid Chemistry pH Titrations pKa and Successive Stability Constant Determination Experiment 23 – Bioinorganic Coordination Chemistry: Copper (II) Tetraphenylporphyrinate Porphyrin Chemistry Thin-Layer Chromatography Column Chromatography Notes to the Instructor; Appendices; NMR and Mass Spectra; Index

About the Author :
GREGORY S. GIROLAMI, University of Illinois, Urbana-Champaign THOMAS B. RAUCHFUSS, University of Illinois, Urbana-Champaign ROBERT J. ANGELICI, Iowa State University

Review :
"Each experiment is well chosen and collectively they present a sufficiently broad spectrum of synthesis and compound characterization techniques to provide an excellent education for any student who completes them…The writing style is clear and concise and at a level that advanced undergraduate students can clearly comprehend. It is highly recommended as a textbook for a one-semester advanced inorganic synthesis course." --Synth. React. Inorg. Met.-Org. Chem., 30(3), 569-570 (2000) "This is an excellent update to a classic inorganic chemistry laboratory text. One of the strengths of this book is that there is something here for everyone. The experiments described in the third edition illustrate a wide variety of topics in inorganic chemistry ranging from classic coordination chemistry to more recent advances in the fields of organometallic, solid state, and bioinorganic chemistry." --Professor Margret J. Geselbracht, Reed College