Books: Modern NMR methods - Analytical Chemistry (ACS Publications)

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Books

Sampling and analysis of volatiles

Static Headspace-Gas Chromatography: Theory and Practice Bruno Kolb and Leslie S. Ettre Wiley-VCH 605 Third Ave. New York, NY 10158 1997, 298 pp.. $79.95

In the preface of this well-wrrtten, moderately sized book, the authors note that static headspace-gas chromatography (SH-GC) is not new. Yet SH-GC remains an attractive sampling-analysis method because it allows for straightforward sample preparation (most often), high sample throughput, automation, and hence significant cost reduction per sample run. In addition, volatile analytes are in a form ready for analysis by GC. This book is very well organized as befits the extensive experience and involvement of both authors but primarily Bruno Kolb, who has devoted about 30 years of his professional work to developing SH-GC methods. Chapter 1 presents a brief general introduction to the principles of static and dynamic headspace analyses, although the rest of the book focuses only on static headspace. An interesting historical presentation is given along with a discussion of the important books and review articles that have documented the advances and applications of SH-GC. One section describes the many worldwide regulatory methods that use SH-GC, especially forensic analyses of ethanol in the blood of automobile and truck drivers. 472 A

Chapter 2 gives a complete theoretical background of static headspace and provides a useful summary of physiochemical relationships, such as the influence of a volatile analyte's concentration on temperature and volume of the headspace phase. A well-developed description of the multiple headspace extraction (MHE) method, long championed by Bruno Kolb, is included. Chapter 3 is perhaps the most useful chapter because it contains informative discussions of the many variants of SH-GC and presents experimental details such as the extent of analyte adsorption to glass walls, the best types of septa to use, and under what conditions septa may be pierced more than once without leading to appreciable analyte loss. There is an interesting comparison between balanced pressure sampling and positive pressure/loopfilling sampling systems. The last 15 pages of this chapter compiles the iritiny forms of derivatization that have been used to en~ hance volatilization and detection for headanalyses. However solid-phase microextraction for static headspace pling of considerable interest is not discussed in the book Chapter 4 discusses variations of sample handling and preparation in SH-GC, including the influence of the sample matrix. Total and full evaporation techniques, which are often used to eliminate matrix effects that plague SH-GC, are adequately presented. Chapter 5 involves quantitative analysis in SH-GC, especially for MHE. MHE plots are presented and show how MHE can be used to determine if an analyte's distribution coefficient is constant and independent of concentration. Chapter 6 gives general guidelines for method development as illustrated by the development of SH-GC methods for measuring residual monomer content of polystyrene pellets. Chapter 7 describes when nonequilibrium conditions are useful for example when the overall analysis and equilibration

Analytical Chemistry News & Features, July 1, 1998

time is too long for a practical analytical method or when working with heat-sensitive analytes, which might be damaged if full equilibrium is achieved. Chapter 8 discusses interesting applications of SH-GC. In summary, the authors have completely presented the theory of SH-GC and have clearly illustrated why SH-GC is such a valuable method for measuring volatile components of liquid or solid samples. This is a book that not only will be useful for the practitioner but also for those learning about or trying to evaluate the potential of SH-GC. The book includes a very useful list of the compounds analyzed by SH-GC. Reviewed by James D. Stuart, University of Connecticut

Modern NMR methods

Handbook of Nuclear Magnetic Resonance Ray Freeman Addison Wesley Longman Higher Education Division Edinburgh Gate Harlow Essex CM20 2JE United Kingdom 1997, 338 pp.. $75

NMR spectroscopy is becoming increasingly important for providing structural and stereochemical information in practically all fields of chemistry. Modern NMR as-

signment techniques commonly employ spectroscopy and the clear and precise extwo-dimensional NMR methods, often in planations, for example in the sections "Coconjunction with pulsedfieldgradients or herence" and "Pulsed Field Gradients". multiple-quantum coherence spectroscopy. Classical vector model description is only The exponential expansion of these new NMR possible with the density matrix treatment. techniques has generated the urgent need to Nonetheless, many common textbooks provide and maintain a thorough underattempt in vain to explain these experistanding of the most popular NMR techments with the conventional vector model. niques. It is to satisfy this demand that Ray In this respect, the introduction of the Freeman has written a second edition of his product operator formalism for the explaHandbooo ofNuclear Magnetic Resonance. nation of pulse sequences is the biggest merit of this book. In contrast to other textbooks dealing with advanced NMR experiments, this What the book needs are some newer handbook is arranged alphabetically in 59 references (e.g., in the section on "Cohersections. This alphabetical arrangement ent Decoupling"); a section on the basic requires that the reader be familiar with theory of NMR imaging; a short descripthe basic principles of NMR theory and tion of solid-state NMR spectroscopy (a applications in order to profit from the de"Hartmann-Hahn" together with a "Spinscription of the more complex experiLocking" section is already part of the ments. Given a basic knowledge of NMR, present edition); and a section dealing with the relevant section can be more or less the design of NMR probes for the applicaeasily understood. tion fields of high-resolution, suspendedstate, solid-state, and in vivo NMR spectrosThe question also arises whether these sections deal with those physical NMR con- copy together with NMR imaging. A handbook of NMR should briefly deal with all cepts most important for advanced underexisting NMR techniques. graduates, postgraduates, and research workers in organic, physical, analytical, Overall, I recommend the handbook to and pharmaceutical chemistry. advanced graduates and research workers From my own 25 years of practtcal NMR engaged in high-resolution multidimenexperience in the above-mentioned fields, I sional NMR spectroscopy, as a way to imdoubt whether the present selection of topprove their understanding of the newer ics adequately suits the needs of a research NMR techniques. worker, for example in analytical chemistry. Reviewed by Klaus Albert, Universität Nobody employs spin tickling experiments Tübingen (Germany) anymore, whereas high-resolution magicangle spinning as well as hyphenated techniques such as HPLC-NMR coupling are BOOKS RECEIVED routinely employed, at least in all industrial analytical labs. These techniques are just Protein Purification, 2nd ed. mentioned in the section "Sensitivity EnJan-Christer Janson and Lars Rydén, Eds. hancement" under "Limited Samples". I per- John Wiley & Sons sonally miss a description of the theory of 605 Third Ave. continuous-flow NMR spectroscopy together New York, NY 10158 with the concept of dynamic nuclear polar1998, 695 pp., $74.95 ization outlined by Harry C Dorn On the other hand I really enjoy the Principles, high-resolution methods, and treatment of multiple-quantum coherence applications of protein purification are the

basis of this book, which is a revised and updated version of the 1989 edition. Stateof-the-art coverage of protein separation, including electrophoretic and chromatographic techniques, as well as characterization methods focusing on structure and function are included. Bioluminescence Methods and Protocols Robert A. LaRossa, Ed. Humana Press 999 Riverview Dr., Suite 208 Totowa, NJ 07512 1998, 310 pp., $79.50

Innovative methods involving the use of luciferase and green fluorescent protein for sensitive biochemical assays are included in this volume, which is number 102 in the series Methods in Molecular Biology. Applications from analytical biochemistry, molecular toxicology, medicine, microbiology, and environmental . monitoring are described, and numerous notes on potential pitfalls and ways to avoid them are included. A Complete Introduction to Modern NMR Spectroscopy Roger S. Macomber John Wiley & Sons 605 Third Ave. New York, NY 10158 1998, 382 pp., $49.95

The basics of NMR spectroscopy are laid out in this textbook in a straightforward manner without complicated mathematics. It is intended to provide the knowledge necessary to solve any molecular structure problem based on a complete set of NMR data. Topics are illustrated with figures and actual spectra. In addition, summaries and review problems with answers are included at the end of each chapter to reinforce key concepts.

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Books

Nonlinear and Two-Photon-Induced Fluorescence Joseph R. Lakowicz, Ed. Plenum Publishing 233 Spring St. New York, NY 10013 1997, 544 pp.. $135

This book is thefifthvolume in the series Topics is Fluorescence Spectroscopy. Compared with the previous volumes, this one covers more advanced methods and applications of fluorescence spectroscopy, including multiphoton excitation. Pumpprobe and stimulated emission methods for cellular imaging and biological studies of macromolecules also included. NMR Spectroscopy: Processing Strategies For more information call:

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Peter Bigler John Wiley & Sons 605 Third Ave. New York, NY 10158 1997, 249 pp., $99

This interactive tutorial contains written text and software tools to provide newcomers with information, theoretical background, and opportunity to gain experience in NMR data handling. The text includes practical hints, examples, and problems to reinforce basic concepts in NMR spectrOSCODV An accompanying CD-ROM provides a comprehensive database and software for transforming NMR data into ID or 2D spectra extracting parameters and obtaining structural information Spectra Interpretation of Organic Compounds Ernö Pretsch and Jean Thomas Clerc John Wiley & Sons 605 Third Ave. New York, NY 10158 1997, 175 pp., $90

This interactive tutorial contains text, software, and data for interpretation of 13 C- and ^-NMR, IR, MS, and UV-vis spectra of organic compounds. This book is designed to be a self-study course for students or beginners interested in the identification of organic compounds and elucidation of their structures. A CDROM accompanies the text making this book a multimedia tool for those wanting experience in the combined application of spectroscopic methods