Synthesis and Technique in Inorganic Chemistry, Third Edition

Summary

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 & 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.

Resources

List of Adoptions

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
• pK_a 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

Reviews

“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