# Book Review Principles of Nuclear Magnetic Resonance Microscopy. By P. T. Callaghan

код для вставкиСкачатьIn “Models as tools” the concept of a model is developed, and the types of models generally used for the design of experiments are described. The reader first encounters statistics towards the end of this chapter, in connection with the validation of models. The two chapters on factorial designs (together with Chs. 4, 7, and 8) contain a detailed treatment of factorial screening, and in particular they explain the connection between calculated primary effects and interaction effects and the response surface models that are treated in more detail in Chapter 12. This chapter also introduces quadratic models and uses this concept to describe the yields of various reactions. Chapter 15 is concerned with principal component analysis, and its application to selecting a few test systems from a very large number of possibilities (different catalysts, solvents, etc.). Chapter 17 then considers how one investigates the effects of the reaction conditions on the most important product characteristics (descriptors), and explains the PLS (partial least squares or projections to latent structures) method. The rest of the chapters serve to put the statistical methods described into the context of organic chemistry. Thus, there are three chapters on strategies (Chs. 1,I3, and 16); these are concerned with general strategies for organic synthesis, strategies for optimizing reaction conditions, and strategies for selecting test systems. Unfortunately, however, there are also three short chapters on optimization methods, which interrupt the flow of the book to some extent, and do not have any direct applications (p. 242: “... applications in organic chemistry are, however, remarkably few”). Possibly these methods have been included in the book so that in later chapters they can serve as a sort of heuristic basis for the selection of suitable test systems, in connection with applications of principal component analysis. To summarize, this book makes worthwhile reading for the organic chemist who would like to plan his or her work a little more systematically, or who simply wishes to find out what statistical methods applied to the design, interpretation, and optimization of experiments are all about. Andreas Orth Hoechst AG Frankfurt am Main (FRG) Principles of Nuclear Magnetic Resonance Microscopy. By P. 7: Cnllaghan. Clarendon Press, Oxford, 1991. XVII, 492 pp., hardcover E 60.00.--ISBN 0-19-853944-4 This monograph is the first handbook devoted to N M R imaging at microscopic resolution. It covers recent technical developments as well as a broad range of applications to biological, mineral, and synthetic materials in a rapidly growing area of research. Examples range from small laboratory animals to eggs, from pathological tissue specimens to plants, and from sandstones to polymers. N M R microscopy is defined as the acquisition of proton N M R images with volume elements smaller than (0.1 mm)3. While two-dimensional images often exhibit an in-plane linear resolution that is about one order of magnitude better than the chosen slice thickness, three-dimensional imaging aims at isotropic spatial resolution. Although the achievable resolution is much coarser than for optical and electron microscopy, significant advantages of the N M R approach are due to (i) the examination of the full three-dimensional structure of a sample without restriction to its surface, (ii) the non-destructive investigation of biological materials or even 1394 f.. VCH Vedagsg~sellsciiufimhH. W-6940 Weinhebn, 1992 living systems. and (iii) the potential for dynamic studies of functional properties. Although not specifically indicated, the book is structured into three main parts. complemented by a small section on hardware considerations. The first part of the monograph comprising Chapters 1-3 (170 pages) deals with imaging principles, basic NMR, and magnetic field gradients in N M R imaging, respectively, and thus covers the whole range of essentials for microscopic imaging by NMR. More difficult theoretical parts may be skipped by the neophyte, but will turn out to be useful for a rigorous treatment at later stages. In addition, principles such as the Fourier transformation and the convolution theorem are discussed with many illustrative examples and figures. The introduction to N M R is confined to some basic quantum mechanics emphasizing the classical treatment (Bloch equations) of magnetizations subject to simple radiofrequency (r.f.) pulse sequences (excluding two-dimensional N M R spectroscopy). The use of magnetic field gradients for N M R imaging is discussed in great detail. Starting from spin density projections of a sample obtained by acquiring its N M R signal in the presence of a magnetic field gradient, the chapter describes slice-selective excitation, N M R image reconstruction, and actual r.f. pulse and gradient sequences popular in medical N M R imaging. The second part formed by Chapters 4 and 5 (150 pages) focusses on the principles and applications of N M R microscopy. Limitations of the spatial and temporal resolution are addressed that are due to the achievable signal-to-noise ratio (SNR), short N M R relaxation times, molecular selfdiffusion and other motions (macroscopic movements, flow, intracellular streaming, fluid penetration of solid materials. swelling of polymers, etc.), and the presence of magnetic field inhomogeneities caused by susceptibility differences in the sample. An almost complete summary of applications is given that creates a realistic picture of the state of the art (1990). by presenting numerous examples from both the “liquid” phase and the solid state. Where appropriate, the applications are accompanied by further detailed descriptions of more complex N M R techniques. For example, microscopy studies of nuclei other than protons may require heteronuclear polarization transfer to improve the SNR, while N M R imaging of solid specimens may be performed in conjunction with spectral line-narrowing by multi-pulse techniques and/ or magic angle spinning synchronized to rotating magnetic field gradients. The third part, Chapters 6-8 (120 pages), expands in considerable detail on the relevance of translational motions for N M R microscopy. Following largely theoretical discussions of various types of mobility and their effects on the N M R signal, more practical aspects are concerned with NMR imaging methods to visualize or even quantitatively determine properties such as anisotropic and/or restricted diffusion. or spatial distributions of flow velocities. The final chapter (20 pages) discusses the design of optimized gradient coils for generating strong, uniform, and time-varying magnetic field gradients as required in high-resolution N M R imaging. A strength of this book is a detailed and comprehensive coverage of N M R imaging, including fundamental N M R techniques and mathematical treatments. This provides the necessary background information, particularly for those readers who are primarily concerned with microscopy as a problem-solving tool, but have little or no experience in NMR. However, my feeling is that many parts will be best appreciated by physicists, but not so easily followed by specialists from other areas of this multidisciplinary field. Microscopy studies are extensively discussed in a major part of the book and include many up-to-date examples. The tabu- 0570-0X33/92!101(~-1394 5 3.50f .ZS,/O Ari,qew. Ciiem. I n t . Ed. EngI 1992, 3f. No. 10 lated summaries provide an excellent overview and facilitate access to the original literature. While some of the examples may soon become outdated due to continuous and rapid progress, the adequate outline of the principles and problems will make this book a useful investment for those interested in the future potential of N M R microscopy. Jens Frahm Max-Planck-Institut fur biophysikalische Chemie Gottingen (FRG) The Chemistry of Amidines and Imidates. Vol. 2. (Series: The Chemistry of Functional Groups; series editor: S. Patai). Edited by S. Patai and Z. Ruppoport. Wiley, Chichester, 1991. XIV, 918 pp., hardcover L 225.00.-ISBN 0-47192457-1 This bulky second volume on amidines and imide esters, in Patai’s well-known and comprehensive series, fulfills two functions. Firstly, nine of the sixteen chapters expand on topics treated in Volume 1 (1975) by including work published up to 1989, mostly with new authors. Secondly, the remaining seven chapters deal with new aspects of the title compounds that were not covered in Volume 1. Many of the chapters also report on the guanidines, which are closely related chemically, and also in some cases on (hetero)cyclic amidines and imidates. Eight of the chapters are concerned with physicochernical and spectroscopic properties, while the other eight deal with syntheses and mechanisms. The first three chapters are concerned with the structures and dynamics of the title compounds. Chapter 1 (G. Hafelinger and F. K. H. Kuske) contains a clear and comprehensive presentation of general aspects and of theoretical results. mainly from a b initio calculations, which are then compared with the available experimental data. Chapter 2 seems somewhat anomalous. In it the authors (T. M. Krygowski and K . Wozniak) present results, in a condensed form, obtained by applying statistical methods to analyze more than 600 crystal structures. Only 22 literature references are given, mainly to the authors’ own publications, and thus one is not given proper access to the original literature. Although Chapter 3, by C. L. Perrin, overlaps in places with Chapter 1, it is interesting since the emphasis is mainly on dynamic and stereoelectronic aspects. Chapter 4 (I. BuSko-Oszczapowicz and J. Oszczapowicz) deals with chromatography and spectroscopy, and Chapter 5 (S. Fornarini) with mass spectrometry. Other chapters are devoted to thermochemistry (Ch. 6, K. Pihlaja), the acidbase and complexation chemistry of the title compounds (Ch. 12, J. Oszczapowicz), and to electronic effects (Ch. 13, J. Shorter). The synthesis of amides, imidates, and guanidines, and their reactions are treated in Chapters 7 and 8 (G. V. Boyd), 9 (D. G. Nelson), 10 (Y. Yamamoto and S. Kojima), and 11 (I. Min-kin and I. E. Mikhailov). Here the great importance of these classes of compounds for the synthesis of a wide variety of heterocyclic ring systems of pharmaceutical significance becomes clearly evident. The book concludes with some more specialized chapters on radiation chemistry (Ch. 14, Z. B. Alfassi), catalytic properties (Ch. 15, P. Ahlberg and L. Swahn), and electrochemistry (Ch. 16, J. S. Jaworski and M. K. Kalinowski). Comparing the coverage with my own collection of literature references shows that in general the authors have been thorough in their searches and careful in their selection. The fact that a number of East European authors have contributAn,ye:pM Cliim In1 6 d Engl 1992. 31. N o 10 ( ed shows that science too is deriving benefits from political changes, as also is the thorough coverage of publications from the East. This volume in the Patai series therefore succeeds well in the aim of providing a key to the original literature, although some of the chapters (e.g. Chs. 1, 3.6, 12, 13) have more of a monograph character. and thus invite more careful study. This excellent work is indispensable for scientific libraries. Ernst- Ulrich Wiirthwrin Institut fur Organische Chemie der Universitit Munster ( F R G ) My 132 Semesters of Chemistry Studies. By I/: Prelog. American Chemical Society, Washington, DC, 1991. XXIV, 120 pp., hardcover $24.95.--ISBN 0-841 2-1 772-6 In an article o n the Czech chemist Emil VotoEek (G. B. Kauffman and F. Jursik, Clzem. Br. 1989, 25. 495). I mistakenly referred to Vlado Prelog as deceased. Our library provided me with the supposed date of his death, and in view of the lengthy duration of his career and the near-classic status of his contributions to chemistry (he is truly a legend in his own time), I neglected to verify the date. I am now delighted to report that this prolific and still active octagenarian has written his scientific memoirs as the shortest volume published to date (Prelog is succinct and modest about his achievements) in Jeffrey I. Seeman’s projected series of 22 autobiographies of prominent organic chemists, Profiles, Pathways, and Dreams.‘*’ With characteristic, self-deprecating humor, he chose the title of his book to reflect his post1976 “retirement” position of “postdoctoral student” at Zurich’s Eidgenossische Technische Hochschule (ETH). The Latin subtitle, “Studiurn chyrniae nec nisi cum morte finitur” (The study of chemistry is concluded only with death) underscores his lifelong commitment to chemistry. As a perfectionist, he was unwilling to draft his manuscript in English despite his superb fluency in this language. His German text was felicitously translated by his friend David Ginsburg, who died before completing the translation, which was finished by Otto Theodor Benfey. Born on July23, 1906 in Sarajevo, Yugoslavia. Prelog served as a “flower boy” on the occasion of the ill-fated visit (June 28, 1914) of Austrian Archduke Franz Ferdinand, whose assassination provided the spark that ignited World War I. Following his parents’ separation in 1915, he lived with his aunt in Zagreb, Croatia, where he spent his first three years of high school (Realgymnasium)and at the age of 12 began his first experiments in his home chemistry laboratory. A 1938 portrait of this juvenile chemist (without goggles!) is one of the book’s 34 formal and informal illustrations. His first article (Chem.-Ztg. 1921, 45, 736) was written when he was 15. After completing high school in Zagreb in 1924, he entered the Chemical Engineering School of Prague’s Institute of Technology, from which he received his 1ng.-Chem. (1928) and doctorate (1929). He remained in Prague carrying out research until 1935, when he became a poorly paid lecturer (docent) (1935-40), and subsequently Associate Professor (1940-41) at the University of Zagreb. With the help of Nobel laureates Richard Kuhn and Leopold RuiiEka, in 1941 he emigrated from German-occupied Zagreb to Zurich, where he has remained ever since at the ETH (Privat-Dozent 1942; Associate Professor 1947; Professor 1950-76). [*] See also: H. Hopf, A n g w . Chcm. I n l . Ed. Engl. 1991, 30. 1190 VCH &~rlagsgesi~llsehuf~ mhH, W-6940 Wrmheim 1992 0S70-0s33/92liolO-l39S $ 3 SO+ 2510 1395

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