ANALYTICAL CHEMISTRY A d v a n c e s in Magnetic Resonance. Val. 1 . John X. Waugh, Ed. xi 413 pages. Academic Press, Inc., 111 FiJth Ave., X e w York, N . Y . 10003. 1966. 816.
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Reoiewed by Wallace S . Brey, Jr., Department of Chemistry, University of Florida, Gainesoille, Flu. This volume is described as the first of a series which will cover nuclear and electron spin resonance, quadrupole spectroscopy, and related areas such as molecular beams, optical pumping, and microwave spectroscopy. The contributions in the first volume include several with a mathematicaltheoretical viewpoint, several extensive compilations of data, and one review which is more general in nature. This review is likely t o be of most interest t o analytical chemists; by D. R . Eaton and W.D. Phillips, it deals with “Xuclear hIagnetic Resonance of Paramagnetic blolecules,” covering both basic theory and typical applications. The longest section, “Geminal and T’icinal Proton-Proton Coupling Constants in Organic Compounds,” by A. A. Bothner-By includes some hundred pages of tables of constants critically selected from the literature, mostly that of 1962 and 1963. This extensive catalog is preceded by a concise review of available generalizations about coupling constant E. Unfortunately , any catalog of data of this type must appear unwieldy a t first inspection. Then, too, a more up-to-date coverage might have been desirable, but neither of these facts detracts from the usefulness of this compilation to a {Torker in the field. A similar compilation of hyperfine splitting constants is presented in “Electron Spin Resonance of Radical Ions” by K. IT. Bowers. The table is “hopefully complete through midsummer, 1964.” Entitled, “The Theory of Relaxation Processes,” the first section in the book is a revised version b17 A . G. Redfield of his often-referenced paper which appeared originally some years ago in an IBAI journal. It is very helpful to have the presentatioll in readily available form. The next contribution, “Chemical Rate Processes and ;\lagnetic Resonance,” by C. 8. Johnson, although spiced with a few examples, is essentially a discussion of the principles and mathematical relations involved in the application of both nuclear and electron resonance, and of both continuous wave and transient methods, to the determination of rates of relatively
rapid reactions. 11. Barfield and David &I.Grant, in “Theory of Nuclear Spin-Spin Coupling,” review a field in which both have made significant contributions. Methods, equations, limitations, and advantages of various approaches to the calculation of coupling Constants, either ab initio or with aid of other molecular parameters, are treated. This is a valuable volume, a t least for anyone who is actively interested in magnetic resonance, carefully produced, and, by today’s standards, reasonably priced. One might hope, however, that a January 1966 publication date would imply more extensive coverage of 1964 and early 1965 literature than is found in several of the chapters.
Purification of Laboratory Chemicals. D. D. Perrin, W . L . F . Armarrego, Dawn R. Perrin. vti 362
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pages. Pergamon Press Inc., 21st St., Long Island City,iVew York 11101. 1966. $11.
Reviewed b y David H . Freeman, National Bureau of Standards, Washington, D . C . 20234. This book presents a compilation of 3000 compounds, arranged alphabetically, and their respective purification procedures. There are 60 pages of elementary introduction. Most of the compounds are organic, and most of the procedures are surprisingly brief. For example, 40% of the entries are like the following: “Glutamine. Cryst. from water.” For one compound out of seven, reference to the literature is given. This tabulation of purification recipes is compiled from the literature without further comment. At best, the work is uncritical, and the recipes are frequently of uncertain usefulness. The conventional aspects of chemical purification, such as the identification of likely contaminants, measurement of their concentrations, optimized methods of lolvering their concentrations, and helpful technical details, are dismissed with the understanding that the reader may already be familiar with them. I n an isolated but serious instance, the procedure given for drying hydrogen bromide gas with magnesium perchlorate is apt to lead t o an explosion [M. J. Stross and G. B. Zimmerman, Ind. Eng. Chem. 17, 70 (1939)l unless the necessary and unmentioned precautions are taken.
This book is aimed a t an important gap in the literature. Its success in closing this gap is unfortunately limited and fragmentary. Melting. Hermann Schddknecht. xii + 222 pages. Academic Press. 111 Fifth Ave., New York, S . Y . 10003. 1966. $9.
Zone
Reviewed b y Henry E . W o o d , Dow Chemical Co., LMidland, Mich. The first section of this book sets forth the theory necessary to an understanding of the zone-melting process through a discussion of normal freezing and concise descriptions of the various types of solid-liquid phase equilibria that occur in binary and ternary mixtures. The theory is then applied t o the zone melting of eutectics and systems involving mixed crystal formation. The second section is concerned with the equipment needed to produce, maintain, and move the narrox, sharply bounded molten zone that is essential to the success of the zone-melting process. Since heat conduction is the major problem in this connection, there is also some theoretical discussion of the temperature gradient in the melt, and of the methods of heating and cooling. Photographs and drawings are included of zone-melting apparatus constructed by numerous investigators for a variety of purposes. The number of successful applications of this relatively new separation process that are cited in the final section are a convincing demonstration of its utility. All aspects of zone melting are adequately and succinctly covered in this book. Although the German original was not available for comparison, the quality of the translation appears to be excellent; only a few sentences were noted that had a definitely Teutonic turn of expression. The format and printing are satisfactory, and the proofreading was done with care. This book is especially recommended to the attention of those m-ho are about to use the technique of zone melting for the first time. After mastering its contents, the novice should be able to construct an apparatus and process his sample with no more difficulties than normally are encountered in such undertakings. Even an experienced practitioner might read it with profit. It was the author’s expressed intention t o emphasize those features of the theory, apparatus, and application of zone melting that are of greateat interVOL. 38, NO. 13, DECEMBER1966
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