The Manipulation of Air-Sensitive Compounds

Citation

Shriver, D. F., & Drezdzon, M. A. (1986). The Manipulation of Air-Sensitive Compounds (2nd ed.). Wiley.

Chapter Summary

The book is a practical manual of roughly 330 pages in two parts, followed by appendixes. Part One deals with working under an inert atmosphere; Part Two deals with vacuum-line work. Chapters are organised around equipment and operations rather than around classes of compounds.

Introduction

A short opening chapter of about six pages that introduces the subject before the two families of technique, inert-atmosphere handling and vacuum-line handling, are taken up.

Part One: Inert-Atmosphere Techniques (Bench-Top Inert-Atmosphere Techniques; Inert-Atmosphere Glove Boxes; Inert Gases and Their Purification; Purification of Solvents and Reagents)

Part One starts with what can be done at the bench with ordinary glassware and an inert gas supply, then moves to the glove box, an enclosed work space for operations that are awkward on the bench. A chapter on inert gases and their purification covers the atmosphere that both methods depend on, and a chapter on purifying solvents and reagents deals with the other common source of contamination. The publisher's description presents this part as the book's treatment of inert-atmosphere techniques.

Part Two: Vacuum-Line Techniques (Vacuum Line Design and Operation; Pumps for Rough and High Vacuum; Pressure and Flow Measurement and Leak Detection; Joints, Stopcocks, and Valves; Specialized Vacuum-Line Equipment and Operations)

Part Two covers the vacuum line, the apparatus used to handle volatile and gaseous materials. It begins with the design and operation of the line as a whole, then treats its components in turn: pumps for rough and high vacuum, the measurement of pressure and flow together with leak detection, and joints, stopcocks and valves. The last chapter of the part collects specialised equipment and operations.

Metal Systems

A chapter on metal systems closes the main text (it begins about two-thirds of the way through the book, after the vacuum-line material). The publisher's listing gives only the title.

Appendixes

The appendixes provide safety data, information on the materials used to build apparatus (plastics and elastomers; metals), and a table of vapor pressures of pure substances; a short section of pressure and flow conversions is also listed.

Key Concepts

Part One

• Inert-atmosphere handling: carrying out manipulations under a purified inert gas so that air- and moisture-sensitive materials never meet oxygen or water.
• Glove box: an enclosed work space with a controlled atmosphere for operations that are impractical on the open bench.
• Purification of gases, solvents and reagents: removing the contaminants that would otherwise defeat an inert atmosphere.

Part Two

• Vacuum line: a manifold of pumps, traps and valves for handling volatile and gaseous compounds.
• Rough and high vacuum: the two vacuum regimes and the pumps that serve them.
• Pressure and flow measurement; leak detection: monitoring a vacuum system and locating faults in it.
• Joints, stopcocks and valves: the connections and closures on which the integrity of an apparatus depends.

Critical Analysis

Strengths

• Organised by technique. The two-part structure (inert atmosphere, then vacuum line) matches how the work is done in a laboratory, so a reader can go straight to the equipment or operation at hand. The publisher describes the book as presenting methods for handling air-sensitive compounds, "including gases".
• Equipment is treated in detail. Pumps, pressure and flow measurement, leak detection, joints, stopcocks and valves each have their own chapter, and the appendixes tabulate construction materials and vapor pressures. This makes the book usable as a working reference at the bench.
• Safety is treated as part of the subject. The publisher lists safety data among the appendixes.
• Established authorship. Shriver is the author of the earlier edition of this title, which Google Books lists under 1969; the 1986 edition adds M. A. Drezdzon as co-author and presents itself as a revision.

Limitations

• Dated edition. This is the 1986 second edition, and the publisher's listing is dated November 1986. Equipment suppliers, materials and safety regulation have changed since, so current laboratory safety guidance and the supplier's present catalogue should be consulted before building or buying apparatus.
• Scope is handling, not chemistry. The book is concerned with apparatus and manipulations. It does not teach synthesis, characterisation or the chemistry of particular air-sensitive compounds, and readers need a separate source for those.
• Print monograph. The publisher lists the second edition as a hardcover, so readers should plan on a library copy rather than assuming an open or inexpensive edition.

Where It Fits in the Course

Within the laboratory-practice course the book is the specialist reference for one family of techniques. Laboratory Safety for Chemistry Students and Prudent Practices in the Laboratory cover safety management and hazard assessment in general, and are the right place to start before any hands-on work with hazardous materials. Practical Skills in Chemistry is a one-volume guide to the practical, analytical and data-handling skills needed across a degree, and Advanced Practical Organic Chemistry is a guide to planning, running, working up and purifying reactions written for students moving into research.

Shriver and Drezdzon is the book to turn to when a project involves compounds that react with air or moisture and the general texts no longer go into enough detail on the apparatus. It sits after the general laboratory and safety texts, and alongside synthetic work in a research group.

How to Use This Book

The book is aimed at research students and practising chemists who will prepare, purify, transfer or characterise air- or moisture-sensitive compounds. Prior synthetic laboratory experience and familiarity with basic safety practice are assumed; it is not an introduction to the teaching laboratory.

A practical plan:

• Start with the Introduction and Part One if the work will be done mostly with inert gas at the bench or in a glove box. Read the chapters on inert gases and on purifying solvents and reagents before the bench-top and glove-box procedures are used in earnest, since they set the quality of the atmosphere everything else relies on.
• Read Part Two in order before building or modifying a vacuum line: design and operation first, then pumps, measurement and leak detection, joints and valves, and finally the specialised equipment chapter.
• Use the appendixes as a reference: the safety data and the tables of materials and vapor pressures are for lookup while planning and running experiments, not for reading straight through.
• Combine with current sources. Check procedures against present institutional safety rules and with an experienced colleague, and use a general safety text for hazard assessment before running a new operation.