Books
Basic Principles of Proton NMR An Introduction to Proton Nuclear Magnetic Resonance Spectroscopy. Addison Ault and Gerald O. Dudek. viii + 141 pages. Paperbound. Holden-Day, Inc., 500 Sansome St., San Francisco, Calif. 94111. 1976. $4.95 Reviewed by Jerry P. Heeschen, The Dow Chemical Co., Analytical Laboratories-574, Midland, Mich. 48640 Here is a lucid introductory text designed to acquaint the student with the simplest basic principles of obtaining and interpreting proton NMR spectra. Written as a useful adjunct to a first-year course in organic chemistry, it also could serve as a self-teaching device for persons who use NMR as an incidental part of their work or for instrument operators not engaged in interpretation. A knowledgeable resource person should be available to answer inevitable questions, particularly for answers to the problems at the ends of chapters. The book is well organized. Each chapter develops in complexity from start to end, and the subject matter proceeds likewise from one chapter to the next. The problems following each chapter deal with basic concepts and are instructive, but answers are not given. There are many illustrations. Most spectra appear to be at 60 MHz, although this is not stated. The presentation is entirely descriptive. The only "precise" relationships given are first-order splitting patterns, chemical shift additivities for methylenes, and a formula for determination of molecular weight by use of an internal reference. Nonfirstorder patterns such as AB, AB 2 , AB3, A2B3, and ABC are discussed and illustrated, but not even the simple expressions for the line positions and intensities of an AB system are offered. There are charts of chemical shifts and a tabulation of proton-proton coupling constants. Four chapters are noteworthy. One examines magnetic equivalence well, and this is a key aspect of the utility of NMR. The chapter "Interpretation of Proton NMR Spectra in Terms of Molecular Structure" discusses several known structures before venturing into the unknown. Two chapters on sample preparation and scanning spectra are useful for the novice. In addition to these chapters, an Epilo-
gue alludes briefly to spin decoupling, computer techniques, quantitative analysis, other nuclei, and shift reagents. Only one editorial error was noted— the spectra for Figures 4-9 and 4-11 are interchanged. The informal writing style reads well, although there are occasional grammatical errors. This reviewer finds the remarkable dearth of simple mathematical relationships regrettable, because the math can be instructive and should not be incomprehensible to any undergraduate science student. One case in point is the AB quartet mentioned above. In another instance, the origin and detection of spinning sidebands are discussed, but it is not stated that their separation from the central line is equal to the spinning rate. There are few unfortunate instances of inaccurate or over-simplified statements on complex topics. These generally are not critical to the argument at hand, but could be confusing for the serious student. In one place it is stated vaguely that for solids "intermolecular forces produce broad lines". Elsewhere, the ringing after passage through a sharp line is described as a pen oscillation rather than as a response of the nuclei which have just been irradiated. It is surprising that there is no bibliography referring the serious student to standard textbooks or to collections of spectra. Only two references are given—one to the two Varian volumes of spectra and the other to an article on magnetic equivalence. In summary, this is a well-written descriptive introduction to proton NMR, suitable for first-year organic chemistry students and incidental users of the method. It is not suitable as a quantitative introduction to the method or as a general reference book. Radio and Microwave Spectroscopy. David J. E. Ingram. 167 pages. Halsted Press, 605 Third Ave., New York, N.Y. 10016. 1976. $12.95 Reviewed by W. H. Flygare, School of Chemical Sciences, University of Illinois at Urbana-Champaign, Urbana, III. 61801 This book attempts to summarize, in a very qualitative way, spectroscopic applications of the radio and micro-
wave regions of the electromagnetic spectrum. This is roughly in the 50MHz region for NMR and the 20-GHz region for ESR and microwave spectroscopy. The book is aimed at the college undergraduate in about his second year. The strong points include good summaries of the beginnings and initial developments of the fields of ESR, NMR, and microwave spectroscopy including good illustrations of the original apparatus in each case. The author has a fine grasp of the subject, and his attempt to give a qualitative picture of the physics involved, without any help from the basic theory, comes off fairly well. The author has also been astute in his discussion of the pure and applied aspects of the fields of radio and microwave spectroscopy. There are also some weak points. In spite of mentioning several of the original workers' names, no references are given anywhere. I certainly think that the average undergraduate would appreciate a few references to follow-up areas that interest him. There are only two tables of data in the entire book. More data pointing toward the information on molecules and about the structure of molecules would have been very useful in illustrating the principles (at least to chemists). It is hard to fit this book into a standard curriculum in the U.S. as a unit course as suggested by the au-
ANALYTICAL CHEMISTRY, VOL 49, NO. 2, FEBRUARY 1977 · 235 A
Books thor. T h e book is too qualitative for a unit course in a chemistry curriculum. It would provide good outside reading, however, for a student in his second or third year of the chemistry curricu lum. Most courses in physical chemis try, taken in the second or third year, have a relatively quantitative b u t short presentation of the principles of ESR, N M R , and microwave spectros copy. This book would provide good outside reading for the origins and ini
tial developments of these fields as well as providing the reader with a summary of applications which, unfor tunately, are weak on the side of mole cules and molecular structure. Environmental Pollutants: Selected Analytical Methods. Wilfred Gallay et al. 277 pages. Ann Arbor Science Pub lishers Inc., P.O. Box 1425, Ann Arbor, Mich. 48106. 1975. $22.50 Reviewed by Rudolph H. Stehl, Ana
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ANALYTICAL CHEMISTRY, VOL. 4 9 , NO. 2, FEBRUARY
1977
lytical Laboratory, Dow Chemical U.S.A., Midland, Mich. 48640 This book, a compilation of meth ods by a subcommittee of the Interna tional Council of Scientific Unions, contains 45 specific methods for ele ments or compounds. It includes methods for airborne lead, cadmium, zinc, copper, nickel, manganese, co balt, beryllium, vanadium, chromium, selenium, arsenic, mercury, fluoride, nitrate, ozone, sulfur- and nitrogenoxides, and benzo-a-pyrene. T h e r e are also methods for some of the above species as well as phosphate, pesti cides, and PCB's in water and/or bio logical fluids. Each of the methods is presented in the same format, which greatly facili tates the comparison of sample collec tion, treatment, and measurement procedures. In addition to accepted techniques and procedures using atomic absorption spectroscopy for metals, a number of methods of esti mation using t h e Weisz ring-oven technique are presented. Gas chroma tographic methods are presented for pesticides and PCB's, while fluores cence is recommended for the mea surement of benzo-a-pyrene. In general, the methods presented are accompanied by quantitative ex pressions of the overall and the instru mental precision and the observed limits of detection for the specified types of samples. Some discussion is devoted, in each of the methods, to sample collection, sample treatment, instrument operat ing conditions, and calculation and ex pression of results. In addition, notes on the procedure are given with com ments on critical or troublesome parts of the procedure. Each method is ac companied by a limited number of ref erences to the original literature. T h e only criticism which might be made of this collection of methods is t h a t too little attention is paid to the sampling procedure itself. However, the complexity of t h a t topic and re cent other references to methodology on sampling ("Residue Reviews", Vol u m e 55) make the editor's cautionary comments on sampling very appropri ate. With the increasing instrumental sensitivity available, the importance of representative and accurate sam pling procedures must be appreciated by the analyst. This book will serve as a valuable addition to the library of analytical as well as environmental scientists to provide a collection of documented, validated methods for some potential ly hazardous compounds and ele ments.
