BOOKS
Thermal Analysis, Chromatography, and Phosphorimetry Computer-Assisted Method Development for High-Performance Liquid Chromatography. J. L. Glajch and L. R. Snyder, Eds. xxiv + 682 pp. Elsevier Science P u b l i s h i n g , P.O. Box 882, Madison Square Station, New York, NY 10159. 1990. $80 Reviewed by F. Vincent Warren, BristolMyers Squibb, P.O. Box 191, Building 101, Room 123, New Brunswick, NJ 08903 This book was previously published as a special volume (No. 485) of the Journal of Chromatography. The editors have added an excellent overview chapter, thereby making the contents considerably more accessible. As a collection of papers from the refereed l i t e r a t u r e , this volume is not designed as an introduction or overview of contemporary approaches to comp u t e r - a s s i s t e d m e t h o d s development. Other recent publications would better serve t h a t purpose, and the editors refer to some of these in the introduction. This volume brings together a mixture of review articles and new contributions from scientists who are actively involved in developing and applying computerized methods development approaches. The 43 papers t h a t make up the book have been organized by the editors into four categories: optimization procedures, expert systems, related procedures, and applications. The anticipated emphasis on optimization strategies is nicely complemented by the other sections. The section on expert systems, spanning some 150 pages, may present the best current collection of papers related to the relatively new application of expert systems to liquid chrom a t o g r a p h y . The inclusion of an applications section is noteworthy, as many previous texts describing comp u t e r m e t h o d s for LC h a v e been short on practical examples. In the i n t e r e s t of objectivity, the editors
have gone to some length to include applications examples from chromatographers not involved in the development of any particular optimization strategy. The section on optimization procedures begins with five review papers t h a t provide an overview of several of t h e most significant optimization strategies, including simplex optimization (Berridge), iterative mapping (Billiet and DeGalan), and simultaneous mapping (Glajch and Kirkland). Each of these reviews encapsulates progress since the early 1980s, the time at which the editors feel t h a t computer-assisted method development actually began. The two remaining reviews describe a commercially available software product, but these are written in a tutorial m a n n e r t h a t r e n d e r s t h e m useful even to readers who have no interest in the product itself. The remainder of the section includes papers on gradient elution, retention prediction, and comparison of optimization approaches. The expert s y s t e m s section includes papers t h a t address diverse aspects of chromatographic methods, including validation, optimization of system parameters (flow rate, pressure, etc.), troubleshooting, and retention prediction. Because this is a new area for chromatographers, the papers in this section tend to have thorough and descriptive introductions. In addition, several papers tackle well-known chromatographic situations (such as troubleshooting and validation) and work through an example in sufficient detail to provide good instruction to the reader who has little familiarity with expert systems. Although some of the expert s y s t e m s p a p e r s r e p o r t w h a t may seem to be r a t h e r modest accomplishments, it may be more appropriate at this early stage to focus on the excellent promise that these papers show for the application of powerful
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new techniques to the representation and use of current chromatographic knowledge. The section on related techniques gathers papers that are of great relevance to the topic of methods development, but t h a t do not fit neatly into the established categories. Included are papers on chromatographic response functions (CRFs), a necessary evil of all computer-assisted procedures. The CRF assigns a numerical quality ranking to each chromatogram used in decision making. Sekulic and Haddad propose a method for modifying the resolution calculation used in many CRFs so that peak tailing is taken into account. Peak tracking (the process of locating each solute in each chromatogram) is a central requirement of many optimization schemes, and there is currently no ideal approach. Two papers address this important topic, including one on the application of fuzzy theory by Lankmayr et al. Another topic is the selection of experimental conditions for optimizing the separation of a mixture of unknowns. Bartha and Vigh describe a procedure for classifying each unknown solute as acid (strong or weak), n e u t r a l , or base (strong or weak). The final section presents eight papers describing the application of various computer-guided strategies to specific optimization problems. Five of the eight papers deal with gradient elution, possibly reflecting a greater willingness of chromatographers to seek the help of software when gradient methods are developed. The paper by Thompson and Ellenson provides a good case study for the use of such software. When gradient optimization software was applied meticulously to the separation of eight solutes, an optimized gradient method was obtained as a result of a straightforward, methodical approach. Other papers describe detailed isocratic optimizations
BOOKS based on multiparameter mapping techniques, as well as challenging gradient separations of amino acids, oligonucleotides, and other sample types. Overall, I found that this book provides a top-notch collection of contemporary papers related to compute r - a s s i s t e d methods development. The section on expert systems was p a r t i c u l a r l y informative. My only problem with the book is that I cannot clearly picture its intended audience. For those interested in specific papers, the material is already available via the Journal of Chromatography. Those seeking an introductory text should look elsewhere, as this book is too specialized to suit that purpose. I can strongly recommend this book to those who have a serious interest in computer m e t h o d s r e l a t e d to LC methods development, and to those who need an excellent collection of u p - t o - d a t e papers spanning many aspects of t h a t topic.
Thermal Analysis. Bernhard Wunderlich. xii + 450 pp. Academic Press, 1250 S i x t h Ave., S a n Diego, CA 92101. 1990. $48 Reviewed by David Dollimore, Department of Chemistry, University of Toledo, Toledo, OH 43606 When Bernhard Wunderlich began his joint appointment at the University of Knoxville and Oak Ridge National Laboratory, we expected to see new developments. A steady stream of p u b l i c a t i o n s a n d a s t r e n u o u s round of lectures in various establishments have been climaxed by the publication of his new book, and it is one of the few good textbooks on the subject. In addition to a problem set, each c h a p t e r contains references. These are not comprehensive, but they guide the s t u d e n t to further study. This is a book by one of the best t e a c h e r s on the subject, designed especially for his students. The book covers all aspects of the topic. It starts by describing the theories that must be mastered before dealing with thermal analysis (thermodynamics, irreversible thermodynamics, and kinetics) and then disc u s s e s t h e b a s i c t e c h n i q u e s of t h e r m o m e t r y , differential t h e r m a l analysis, calorimetry, thermomechanical analysis, dilatometry, and thermogravimetry. The typical student using this book would be an undergraduate senior. The book could also be used for a graduate course in
thermal analysis. Such courses are becoming a regular feature in many graduate research establishments. However, t h e majority of those working in the field have not had the advantage of such formal training and they themselves should possess this book. It tackles very basic questions that should cause them to look carefully at the immediate product produced by the computer workstation "in charge" of the equipment. In the early chapters, it is refreshing to note that the student is introduced to irreversible thermodynamics. The author's language is very direct, and he competently puts important facts and theories into very few words. Thus, he is able to introduce the concept of time dependence in irreversible thermodynamics and make a bridge between it and kinetics. However, the author does not reiterate these concepts enough to really force the new student to appreciate the points being made. The conciseness of language and the succinct manner of presentation have resulted in a book of moderate length that is easy to read. The author states that the book covers all aspects of thermal analysis, but his own wealth of experience keeps coming to the surface with examples of organic molecules. This will satisfy the practicing t h e r m a l analyst in America, where 90% of the work done is with polymeric materials; but it might not be so appealing to a European audience for whom a sizable proportion of thermal analysis studies is in geology and inorganic chemistry. The book is written in such a refreshing approach, however, that it will prove useful to all practitioners of the art of thermal analysis.
Phosphorimetry: Theory, Instrumentation, and Applications. Robert J. Hurtubise. 370 pp. VCH Publishers, 220 E a s t 23rd St., New York, NY 10010. $60 Reviewed by Gabor Patonay, Department of Chemistry, Georgia State University, Atlanta, GA 30303 Luminescence spectroscopy has found extensive use in practically all areas of analytical chemistry. In addition to conventional luminescence, many studies have demonstrated the usefulness of phosphorescence meas u r e m e n t s . This book provides an overview of theory, instrumentation, and applications of phosphorimetry. It also attempts to give an extremely
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brief overview of special applications, e.g., the application of phosphorescence m e a s u r e m e n t s in protein or polymer research. The rest of the book is aimed both at readers who want to gain information about the latest developments and those who are specialists in specific areas of phosphorimetric applications. Therefore the last two chapters, although important, are somewhat inconsist e n t with the general goal of the book. I found the major portion of this book to be informative and will recommend it to my students who are interested in luminescence. Nevertheless, there are some problems that need to be mentioned. In the first part of the book, the second, third, and fourth chapters on theory and instrumentation of luminescence are adequately detailed for the nonspecialized reader to establish a proper foundation for understanding the rest of the chapters. An ample number of references in these chapters allow the reader to investigate further. However, some of those who are familiar with luminescence may find that these chapters repeat the basics. The following chapter provides a partial representation of the state of the art in low-temperature phosphorescence. However, the discussion is limited in some areas of practical applications. Analytical chemists, not just spectroscopists, need to become familiar with this technique in order to deepen their understanding of luminescence. This chapter is an excellent place to s t a r t , a l t h o u g h the timeliness of the references seems somewhat inadequate. The later chapters that cover the most exciting topics of phosphorimetry (e.g., solid-surface room-tempera t u r e phosphorescence, sensitized phosphorescence, and phosphorescence in organized media) are written from the difficult perspective of being up to date with the latest developments while giving a general overview of the applications. Both goals have been largely achieved in this most valuable part of the book. As a c o n d e n s e d b u t e x h a u s t i v e source for less familiar techniques, it may be the most useful section for the analytical professional in industry and academe alike. The extremely useful applications of phosphorimetry in analyzing environmentally important constituents are evident in the examples described. Nevertheless, a lack of detail about some applications makes it almost impossible for the reader to successfully apply any method based on the information
given. These chapters are definitely a useful overview for most analytical graduate students. They are also extremely useful for those professionals who wish to find new techniques for the analysis of compounds that are capable of phosphorescing. I n a d d i t i o n to c o m m u n i c a t i n g valuable information on relatively lesser known methods, some of the chapters include many useful references to special applications. In spite of the large number of citations and the diversity of topics covered, some of the value of the book has been lost as a result of the author's aspiration to satisfy both expert and nonexpert readers. In general, this a very good book for learning about phosphorescence. It would have been an even better book if the author h a d put more emphasis on modern developments in phosphorimetry at the expense of the first four chapters.
Countercurrent Chromatography: Apparatus, Theory, and Practice. W a l t e r D. Conway. 475 pp. VCH Publishers, 220 East 23rd St., New York, NY 10010. 1990. $75 Reviewed by Alain Foucault, Laboratoire de Bioorganiques et Biotechnologies, Ecole Nationale Supérieure de Chimie de Paris, 11 rue Pierre et Marie Curie, 75231 Paris Cedex 05, France Two years after publication of the anthology by Y. Ito and Ν. Β. Mandava (see the book review in Anal. Chem. 1989, 61, 655 A), this new pub lication by Conway is very welcome for people working with countercur rent chromatography (CCC), or sup port-free liquid-liquid chromatogra phy. This technique originated in the 1960s with the pioneering studies by Y. Ito and co-workers, and became known to nonspecialists in the 1980s, when modern apparatus like the Ito multilayer coil planet centrifuge be came available, and when a seminar was started at the Pittsburgh Con ference. Conway spent a sabbatical leave in 1981 in Ito's laboratory, where he be came familiar with both the mechan ical f e a t u r e s a n d a p p l i c a t i o n s of CCC. The author dedicated the book to Peter Carmeci, who has been a pi oneer in the commercial development of CCC since he created the P.C. Cor poration in the mid-1980s and start ed to manufacture the multilayer coil planet centrifuge, which has played a major role in the actual development of Ito's methodologies.
The nine chapters are relatively self-contained and need not be read consecutively. Chapters 2 - 5 , which describe the evolution of CCC, col umn motion and centrifugal fields, and liquid distribution and phase mixing, will overwhelm the nonspecialist. These chapters give a com plex image of CCC, which is in other respects very easy to practice, as ex plained in Chapter 9 (Getting Start ed in CCC). These three chapters are more or less a rewrite of the large Chapter 3 in the 1988 book, written by Ito. I was disappointed that the nomenclature carefully defined by Ito to characterize all the flow-through centrifuge schemes free of rotary seals ( I - L - J and I - X - J series), to classify all CCC instruments into two main groups (i.e., HSES for hydro static equilibrium systems and HDES for hydrodynamic equilibrium systems), and to indicate what kind of centrifugal field (constant or vari able) is produced by an instrument, is nonexistent here. It has been re placed by an alphabetic classification (Fig. 2-17, page 26), or by a mixture of old and new nomenclature (Fig. 4-20, page 147), or by a "planet-gear and planet-pulley" nomenclature (Chapters 4 and 5). This gives the reader a messy impression (which I remedied promptly by looking back to Ito's literature). Chapter 6 refreshes the reader's memory with some useful mathemat ical relationships commonly used in chromatography in general, and with a customized digression on the reso lution equation Rs = (1/4) (a - 1) N1'2 [k ; / (k J + 1)] The author attributes this to Knox, but it originates from J. H. Purnell (J. Chem. Soc. 1960, 1268). Chapters 7 to 10 (solvent systems, practice, and applications) constitute the main part of the book. Many ter nary diagrams are given, and the au thor carefully guides the reader to a clear understanding of how to use a diagram to make up a binary liquidliquid system. He also provides sim ple rules for selecting a solvent sys t e m for a g i v e n s e t of s o l u t e s . Applications are classified by type of c h r o m a t o g r a p h i c compounds with many examples and practical obser vations. The 422 references are clas sified by subject instead of being chronological, which gives the reader a simple and powerful tool to create his or her own bibliography. A sub ject index allows easy access to the book, which will enhance the library of any laboratory dealing with sepa ration and purification problems.
CHRONICLING ADVANCES IN CHEMISTRY 13
C-NMR OF NATURAL PRODUCTS by Atta-ur-Rahman and Viqar Uddin Ahmad Volume 1 MONOTERPENES AND SESQUITERPENES This ground-breaking, comprehensive volume presents the latest data on the 1J C-NMR of monoterpenes and sesquiterpenes. Readable and well-organized, the text classifies compounds in easy-tolocate categories according to their structure, molecular weight, carbon number, and alphabetical name. 0-306-43897-6/829 pp. + index/ill./1991/S135.00
Volume 2 DITERPENES Chemists researching the structure of new compounds will find this volume, which covers the 13C-NMR data of diterpenes, a valuable reference source. Retaining the well-organized format and accessible presentation of Volume 1, distinguished contributors provide comprehensive coverage of "C-NMR chemical shift values in structures. 0-306-43898-4/675 pp. + index/ill./1991/S125.00
Forthcoming. . . ION SPECTROSCOPIES FOR SURFACE ANALYSIS edited by A.W. Czanderna and D.M. Hercules This treatise reviews techniques of surface compositional analysis involving the detection of scattered or sputtered ions. Volume 2 in the series Methods of Surface Characterization. 0-306-43792-9/approx. 450 pp./ill./l991
ADVANCES IN COAL SPECTROSCOPY edited by Henk Meuzelaar Leading experts in the field review the development, testing, and applications of spectroscopic techniques for coal and coal derivatives, and cover the role of spectroscopy in coal use impact programs. A volume in the series Modern Analytical Chemistry. 0-306-43796-1/approx. 425 pp./ill./1991 Book prices are 20% higher outside US & Canada.
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