Books
Encyclopedia of Microchemical Principles and Methods Microscale Manipulations in Chemis try. T. S. Ma and V. Horak. xiii + 488 pages. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1976. $27.50
Reviewed by Walter T. Smith, Jr., Department of Chemistry, University of Kentucky, Lexington, Ky. 40506 Over the years we have come to ex pect excellent scientific writing from T. S. Ma, and this book by Ma and Horak is no disappointment. This sin gle volume of under 500 pages is a ver itable desk-top encyclopedia. It covers even more material and provides even more information t h a n one has a right to expect from the title. T h e coverage is not limited to analytical chemistry, but encompasses all aspects of chemis try on a small scale. Ma's definition of microchemistry is a lasting and sensi ble definition. He says, "Microchemis try . . . is concerned with the principles and methods of using the minimum quantity of working material to obtain the desired chemical information." T h e further statement t h a t the "mi crochemical approach can be applied whenever an experimental d a t u m is required, be it for the composition of matter (chemical analysis), prepara tion of a compound (chemical synthe sis), or study of reaction mechanisms" provides some idea of the broad scope. T h e book is intended to be a guide book "for the practicing chemist, a lab manual for advanced students, and a comprehensive treatise on microchem ical manipulations". It does an admi rable job of fulfilling these intentions. Throughout the book many analyti cal principles are enunciated. T h e in troduction also points out what a com plex and demanding job the microanalyst has. This material should make the microanalyses job easier by facili tating the meeting of those demands. There is brief coverage of some topics and ample coverage of other topics. One might disagree with the authors as to their selection of topics to be covered briefly and those Ίο be cov ered more fully. Any such selection would be biased by the reader's per sonal interests. It is hard t o find spe cific faults with the selection, particu larly since all of the topics touched on are amply referenced.
Certain parts read like a highly con densed review article, but this is no doubt necessary in a book as encyclo pedic and comprehensive as this is for its size. This comment can hardly be considered a criticism. One may wonder about the useful ness of an illustration showing a fun nel in top of a chromatographic col umn or the picture of an ultraviolet lamp, but on the other hand, a great many helpful illustrations are provid ed. Topics covered range from the mun dane to the exotic, as illustrated by the following selected examples: sam ple storage, collection of GC samples, atmospheric sampling, clathrates, mo lecular sieves, dialysis, how to obtain reproducible low temperatures, and a sieve p u m p based on acoustic loud speakers. Many modern subjects are covered, but the old fundamental techniques are not neglected. T h e section on crys tallization from solution provides good general instructions for the beginner, regardless of whether the crystalliza tion is on a micro or macro scale. Appendix Β is a list of supply houses and manufacturers of micro chemical equipment throughout the world. This useful list literally covers suppliers from A to Z. A warning should be issued to desk bound chemists. Browsing through the descriptions of clever techniques in this book may result in a case of itchy fingers and a desire to try out some of these ideas in the lab. Topics in Carbon-13 NMR Spectrosco py, Vol. 2. George C. Levy, Ed. xi + 485 pages. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1976. $27.50
Reviewed by George A. Gray, Varian/ Instrument Division D-298, 611 Han sen Way, Palo Alto, Calif. 94303 T h e rapid growth and development of 13 C N M R into a powerful research and analytical tool in many branches Of chemistry and biochemistry have made keeping a current awareness an awesome task. "Topics in Carbon-13 N M R Spectroscopy" a t t e m p t s to ease this endeavor and certainly has suc ceeded in this second volume of the
series. While laying the physical foun dation in the first volume, the second offers a needed followup in the biolog ical areas along with additional breadth in basic practice and theory of NMR.
Roxanne Deslauriers and Ian Smith of NRC, Ottawa, review the extensive work accomplished in the study of conformation and structure of pep tides. In addition to the classical N M R parameters, they lay heavy em phasis on the use of spin-lattice (Ti) relaxation time measurements to probe the dynamics and structure of cyclic and linear peptides. For many years Ernest Wenkert and coworkers have been utilizing l 3 C N M R in the complex task of natural product struc ture determination. They have con tributed a chapter detailing much of that work and t h a t of related investi gations, centering on fatty acids, pheromones, coumarins, various terpenes, and alkaloids. Here, the l 3 C shifts are covered in depth as well as some cou pling data. Biosynthetic studies probe synthetic pathways leading to natural products, and 13 C N M R has been ex ploited intensely here by the Halifax group of A. G. Mclnnes, J. A. Walters, and J.C.L. Wright from the Atlantic
ANALYTICAL CHEMISTRY, VOL. 48, NO. 14, DECEMBER 1976 · 1 1 8 1 A
Books Regional Laboratory of t h e N R C and L. C. Vining of Dalhousie University. They review their work and related activity including labeling techniques, measurement of isotopic enrichment, and biosynthesis with singly and dou bly labeled precursors. R. A. Komoroski, Ian Peat, and George Levy present a chapter on 13 C . N M R studies of biopolymers, comple menting the article on synthetic poly mers by J a k e Schaefer in Volume 1. T h e y cover proteins,.high-molecularweight polypeptides, nucleic acids and polysaccharides, and review the appli cations of T\ techniques in the analy sis of molecular motions peculiar to these large, slowly rotating polymers. Considerable attention is paid to in teractions with large biomolecules by paramagnetic metal ions and enzymesubstrate interactions. In addition to the above, there are several articles of general interest. Otto Gansow and William Vernon re view applications of 13 C N M R to organometallic and transition metal compounds. Recent applications to static and fluxional metal carbonyls in solution are discussed. These prob lems have long plagued investigators in this area. Group I-IV organometallics are covered as well as metal coor dination compounds and cyclopentadienyl complexes. Felix Wehrli of Varian, Zug, has contributed a valuable article on organic structure assign ments using 13 C spin-relaxation data. After a description of the phenome non, mechanisms, dipolar contribu tion, and measurement of I 3 C relaxa tion times, he describes the qualitative relaxation information available in the normal F T spectrum, shows how T\ may be used to assign quaternary car bons through neighbor proton count ing, and describes the importance and utility of the nuclear Overhauser ef fect measurement. l 3 C relaxation data of many intermediate molecular weight compounds are given with the assignment rationale. James Cooper of Tufts University reviews basic facts about computers in the Fourier transform experiments, including data acquisition, signal av eraging, dynamic range, digitization, and Fourier transform procedures. He presents an analysis of techniques for handling large dynamic range situa tions such as proton F T of water solu tions. T h e volume finishes with a t r e a t m e n t of the theory of indirect nu clear spin-spin couplings in 13 C N M R by Paul Ellis of the University of South Carolina and Robert Ditchfield of Dartmouth College. After present ing the possible spin coupling mecha nisms, they present a general theory both at ab initio and semiempirical
levels. ^ Ο - Ή , 1 3 C - 1 3 C , 1 3 C - n B , 13 C- 1 5 N, and 1 3 C- 1 9 F couplings are predicted and compared with experi mental values. Volume 2 of this series nicely fills definite needs and should be useful not only to experienced workers in 13 C N M R but also for those entering the field. Analytical Methods for Pesticides and Plant Growth Regulators, Vol. VIII. Gunter Zweig, Ed. xiii + 510 pages. A c ademic Press, Inc., 111 Fifth Ave., New York, N.Y. 10003. 1976. $46.50
Reviewed by William J. Trotter, Ana lytical Chemistry & Physics Branch, Department of Health, Education, & Welfare, Public Health Service, Washington, D.C. 20204 With Volume VIII the editors have excellently updated and expanded their survey series of pesticide analyti cal chemistry. T h e book is a necessary addition to the library of anybody in terested in the field of pesticide chem istry. Two new areas of discussion for this series are included in this volume. These areas are Federal regulations and pheromone analytical methodolo gy· T h e discussion of regulations is well written and informative. However, it is somewhat general and brief. T h e author informs the reader of the gen eral effects and impact of the enact ment of the Federal Environmental Pesticide Control Act (FEPCA) of 1972. Also emphasized is the impact of the Environmental Protection Agency (EPA) relative to pesticide regulation. Most of the discussion is devoted to reviewing the general requirements of applications for pesticide registration and petition for tolerance in food. Also reviewed are the relationship between the Food and Drug Administration and E P A , and the National Pesticides Monitoring Program. T h e section on pheromone analyti cal methodology is excellent. An ex tensive table of pheromones, their structures, species affected, and relat ed references are presented. T h e dis cussion deals primarily with the meth odology for the isolation from the source material, purification, and identification of pheromone com pounds. For example, the pheromone may be solvent extracted from insects. Subsequent purification or cleanup of the pheromone compound may in clude an extraction into another sol vent, distillation, a chromatographic procedure, or a combination of these. Identification and confirmation of the pheromone may be achieved by chro matographic and/or spectrometric procedures. T h e technical level of the
1 1 8 2 A · ANALYTICAL CHEMISTRY, VOL. 48, NO. 14, DECEMBER 1976
presentation presupposes a knowledge of general analytical chemistry proce dures. T h e survey of experimental procedures is extensive and extremely well documented. Many illustrative examples of the current methodology and trends with respective phero mones are included. Perhaps most of the potential read ers of Volume VIII have already read other volumes in the series. These people, therefore, are already familiar with t h e series' t r e a t m e n t of analytical methodology for specific pesticides. Volume VIII presents the current ana lytical methodology for 31 chemicals. Most are insecticides and herbicides; some are fungicides and plant growth regulators. Some of these chemicals are used internationally b u t have not been registered for use in the United States. A few of the pesticides have al ready been discussed in previous vol umes, but information on these is updated in Volume VIII. Both formu lation and residue methods are pre sented. T h e methodology in most cases is detailed. T h e reader should have a general knowledge of pesticide analytical chemistry. In addition to methodology, other extensive d a t a about each pesticide are also included. T h e data presented are the empirical formula, alternate names, source of analytical standard, history of the pes ticide, biological, physical and chemi cal properties, and formulation. T h e scope and depth of the presentation are excellent. Statistical Calculations: How to Solve Statistical Problems. E. Joe Middlebrooks, viii + 1 2 0 pages. Ann Arbor Science Publishers, Inc., P.O. Box 1425, Ann Arbor, Mich. 48106. 1976. $12.50
Reviewed by John Mandel, Institute for Materials Research, U.S. Depart ment of Commerce, National Bureau of Standards, Washington, D.C. 20234 Referring in his introduction to the "numerous textbooks and popular books on the subject of statistics", the author states, " W h a t most of these books are lacking is a detailed presen tation of the application of the materi al presented." Presumably, this book intends to fill t h a t gap and does by going through the arithmetic involved in a variety of statistical techniques, with heavy emphasis on tests of signif icance. T h e author disclaims any " a t t e m p t to present theory or derivations in the examples of statistical calculations" and recommends t h a t the reader ac quire his understanding of statistics by consulting either one of two books,
Books specifically mentioned in his introduc tion. One must conclude t h a t the present book is written with the mod est aim of providing a guide to the ap plication of algebraic formulas to nu merical data. This, in fact, is the case. For exam ple, in applying an unpaired t test to the comparison of two methods for measuring the latent heat of fusion of ice, the book, without any discussion of substance, goes in detail through the steps of calculating the two aver ages, the two sums of squares and variances, and then compares the vari ances by means of the F test. T h e variances are then pooled, and the standard error of the difference is cal culated. This is followed by t h e arith metic for calculating a confidenc in terval for the difference between the means. Similar detailed computation al explanations are provided for t h e comparison of more t h a n two means by analysis of variance, for Duncan's multiple range procedure, for linear and nonlinear, multiple and partial re gression, as well as for a variety of de signs. T h e use of statistics for the inter
pretation of d a t a is fraught with great difficulties and uncountable pitfalls. Occasionally, one encounters crude mistakes, such as erroneous formulas, or formulas incorrectly calculated. T h e present book may help in reduc ing the frequency of such mistakes. B u t the type of mistake t h a t is far more dangerous, because it is harder to detect, is the subtle one involving statistics t h a t is technically correct b u t is used in conjunction with poor logic or poor scientific judgment. Though the book's subtitle is "How to Solve Statistical Problems", the read er should be careful not to conclude t h a t correct arithmetic is all t h a t is needed to "solve" a problem involving statistical methodology.
New Books Infrared and Raman Spectroscopy, Part A. Edward G. Brame, Jr., and Jeanette Grasselli, Eds. ix + 345 pages. Marcel Dekker, Inc., 270 Madison Ave., New York, N.Y. 10016. 1976. $33.75 This book initiates a new series en titled, "Practical Spectroscopy Se
ries", which promises to review all possible applications of the varied as pects of spectroscopy. P a r t A of Vol ume 1 (two more parts to be pub lished) is devoted entirely to infrared and Raman spectroscopy and contains four chapters. Appropriately, it pre sents the introductory chapter for the entire volume, written by Bryce Craw ford, Jr., and Douglas Swanson. This chapter discusses the nature of molec ular vibrations, their appearances in the infrared spectrum and the R a m a n spectrum, and some of the experimen tal aspects of measuring them. Chap ter 2, written by Robert L. Carter, treats the application of infrared and R a m a n spectroscopy to inorganic ma terials. Chapters 3 and 4, both au thored by Walter F. Edgell, cover the applications of molecular spectroscopy to organometallic materials. T h e book is a good quality photo-offset copy of typewritten text. Managing Metrication in Business and Industry, χ + 203 pages. Marcel Dek ker, Inc., 270 Madison Ave., New York, N.Y. 10016. 1976. $25 T h e American National Metric
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