Synthesis and Technique in Inorganic Chemistry, 3rd edition

Gregory S. Girolami, Thomas Rauchfuss, Robert Angelici

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Format: Paperback

Publication date: October 3, 1999

Pages: 288 pages

ISBN: 9780935702484 Related titles:


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.

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
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

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

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