ANALYST, FEBRUARY 1993, VOL. 118 17N Book Reviews Atomic Absorption Spectrometry. Theory, Design and Applications Edited by S. J. Haswell. Analytical Spectroscopy Library. Volume 5. Pp. xx + 530. Elsevier. 1991. Price US$177.00; Df1345.00. ISBN 0-444-8821 7-0. This book is based on the successful book of similar title, edited by John Cantle, which appeared some ten years ago and has a not dissimilar format. However, this volume has been extensively re-written (over SO%, according to the preface) and is not just an updated version of the earlier work, but a new book. The first two chapters provide a brief, but clear introduction to the basic theory and the instrumental requirements for the practice of atomic absorption spectrometry, whereas the third chapter deals with the basic practical aspects of the technique.These chapters justify the claim that ‘the book represents a complete text on AAS’, but in view of the depth of coverage that can be given in the relatively short space available (71 pp. for the three chapters), the absence of references in Chapters 2 and 3 is both puzzling and disappointing. In some cases the absence of references could be misleading to the less experienced user; for example the table of sensitivities, which is highly instrument dependent, is presented with no descrip- tion of the equipment used to generate the data. Figures for salt tolerance of burner systems are also presented with a similar lack of detail and are much poorer than can be reached with better designed nebulizer-burner systems. The following chapters deal with applications and com- mence with an excellent and well-referenced chapter on the analysis of waters, sewage and effluents, which covers the entire field from sampling to quality control protocols and is essential reading for anyone entering this field of analysis.The use of AAS and other methods of atomic spectroscopy in marine analysis is covered in Chapter 5 , which is an excellent summary of this field of analysis but is marred by the inclusion of a table of detection limits based on material that is not only 15-20 years old, but incorrectly referenced for good measure! The analysis of airborne particles in workplace atmospheres and the analysis of foods are covered by two readable and comprehensive chapters, which contain sufficient information for the procedures described to be implemented without recourse to the extensive references.The use of AAS in metallurgy is detailed in chapters dealing with ferrous metallurgy, which is very comprehensive with references up to 1989 and one on non-ferrous metallurgy, which is somewhat shorter, but still most informative and worth reading. Applied geochemistry is dealt with in a chapter that is a little less up-to-date than most of the others, but this does not detract from its usefulness, as the whole analytical process is described in detail and most of the more recent developments in this area have been in the field of ICP-OES (or ICP-MS), rather than in AAS. The chapter on the use of AAS in the petroleum industry clearly illustrates the limitations as well as the advantages of the technique and contains references as recent as 1991.The analysis of glass and ceramics is described in a short chapter, which details a thoroughly competent method for such analysis. Clinical analysis is dealt with in an informative chapter describing the rapid FAAS methods used in the clinical laboratory and this is followed by a long chapter dealing with body fluids and tissues using ETAAS. The two chapters compliment each other well and are referenced up to 1988. The chapter on forensic analysis is written in an entertaining style but is still informative to the non-specialist. The analysis of a wide range of chemicals and related products is dealt with in a chapter with nearly 300 refs., so that even if there is insufficient detail to implement a procedure described in the text, the reader should have little difficulty in finding additional reading.The final chapter on the analysis of polluted soils gives a general introduction to the subject, followed by useful notes on individual elements. Despite of some minor criticisms this is a well-produced book that should be useful to anyone working in the field of trace metal analysis even if they are not an AAS specialist, as great care has been taken to describe both the procedures that can be used along with limitations that are found in practice. It will also be useful to the specialist working in one field who is sometimes called upon to perform work outside of their normal expertise, an increasingly common situation these days! By current standards for scientific books, this one is not unreasonably priced and I have no hesitation in recommend- ing that it should be added to the library of anyone who uses atomic absorption spectrometry.Colin Watson Liquid Chromatography Column Theory By R. P. W. Scott. Separation Science Series. Series Edited by R. P. W. Scott and C. F. Simpson. Pp. x + 279. J. Wiley and Sons. 1992. Price f34.95. ISBN 0-471-93305- 8. A well written book should provide for the reader a comprehensive and lucid coverage of the title subject. Ray Scott has provided here all the algebra and calculus that chromatographers interested in column design and perfor- mance could want in a logically developed format. Following a brief introductory chapter on concepts and nomenclature, Chapter 2 introduces Plate Theory to define solute retention volumes, capacity and separation ratios.No modern text on column chromatography would seem to be complete without a discussion on dead volumes, the subject of Chapter 3. Whilst not resolving the controversies, a useful discussion of the different volumes is provided. Chapters 4 and 5 return to Plate Theory to provide a detailed description of the chromatographic processes themselves, including peak shape and column efficiency, resolving power and peak capacity. These chapters are heavily loaded with mathematics, which I assumed to be correct, and I found them somewhat unrewarding. The generality of Plate Theory is, however, well demonstrated by its extension to the description of the properties of the heat of absorption detector, although J suspect this section will have only a minority appeal.Chapter 6 introduces Rate Theory, which can be used to explain the dispersion processes that occur during a separation and to explore factors that can be optimized so as to maximize efficiency. This, and the subsequent chapters describing the van Deemter equation and alternative equations for peak dispersion (e.g. , Giddings and Knox) provided for me a much more practical insight into prospects for improving chromato- graphic performance. Here we find a lucid explanation of why higher efficiencies require larger, not smaller, particles-a concept many chromatographers still struggle with. Chapter 9 examines the experimental validity of the various Rate Theory equations, leading to the conclusion that the van Deemter equation remains the most appropriate for column design purposes.Chapter 10 concludes the examination of dispersion processes by looking at extra-column dispersion. This is a very readable chapter with good practical information on items such as connecting tubing parameters and configurations. The final four chapters discuss the practical processes of designing liquid chromatography columns; packed, open18N ANALYST, FEBRUARY 1993, VOL. 118 tubular and preparative. These are valuable chapters for the practical chromatographer as well as the column designer. Equations and graphs describe the relationships between separation difficulty and variables such as particle size, column length and radius, and solvent consumption.I looked in vain, however, for a discussion on tapered columns. It is interesting to recognize that, with an optimized column system, even the most difficult separation should require no more than 7.5 cm3 of mobile phase. For each type of column a BASIC computer program is presented that incorporates the essential design equations and which will provide the design and operating conditions to enable a given separation to be achieved in the minimum time and with the minimum solvent consumption. The book concludes with a list of symbols (but be careful as the symbols are not unique) and three appendices of physical data. References are provided at the end of each chapter although I found them to be not particularly up-to-date. The extensive mathematics inevitably will make the book heavy reading for many.It is then even more unfortunate that there are many errors of spelling, grammar, syntax and typography, no more evident than in Chapter 1. The presentation of the book is also spoiled by the use of a dot matrix printer, with varying numbers of characters per inch and lines per page. Nevertheless, there is much useful information to be discovered and the book should appeal to those enthusiasts interested in designing their own columns or selecting optimum column or operating parameters for a particular separation. John C. Berridge Analyses of Hazardous Substances in Air. Volume 1 Edited by A. Kettrup. Pp. 224. VCH. 1991. Price DM98.00. ISBN 3-527-2701 5-9 (VCH, Weinheim); 0-89573-901 -1 (VCH, New York). Almost thirty years ago, the Deutsche Forschungsgemein- schaft created the Commission for the Investigation of Health Hazards of Chemical Compounds in the Work Area. Part of the work of the Analytical Chemistry Working Group established by the Commission has been to recommend methods for the analysis of hazardous substances in air.Criteria for the selection of methods include suitability for routine use, reliability, and meeting requirements for quality control, and for these reasons the methods are recommended under German legislation. The volume under review results from an initiative of the Commission to make its methods available to an international audience. The preface to the book makes clear that the Working Group’s philosophy has not necessarily been to seek simple, cheap and quick methods.Preliminary chapters cover the theory of diffusion samplers, although I would have liked to see more information on their practical use, in what is essentially a practical text. Indeed, the subsequent analytical methods include details. of active sampling techniques exclu- sively. It appears that the Working Group require more tests of diffusion sampling in environments where mixtures may compete for adsorption. The first part of the book also includes details on statistical evaluation of the methods and quality indexes. Most of the book is devoted to practical methods. Infrared spectrophotometric determination of gases and vapours using portable long-pathlength cuvettes is described, with details of sampling options, calibration and calculation of results.The important role of atomic absorption spectrometry and gas and high-performance liquid chromatography are highlighted in the Preface, and three-quarters of the book is devoted to descriptions of their use. Curiously, only one method (for hexamethylene diisocyanate) using the last-named technique is described in the book, with the main emphasis being on gas chromatographic methods. Methods for the determination of ten individual or groups of substances are described, including dimethylamine, phenol, ethylene glycol derivatives and poly- cyclic aromatic hydrocarbons. Inevitably chapters of this type appear repetitive, but are comprehensive in detail. Finally, methods for the measurement of Pb, Ni, Co and Cr by atomic absorption spectrometry are described. By present day standards, the price of this book is not excessive and justifiably will find its way onto the bookshelves of many involved with the analysis of atmospheres.R. S. Barratt Gas-Liquid-Solid Chromatography By V. G. Berezkin. Chromatographic Science Series. Volume 56. Marcel Dekker. New York. 1991. Pp. viii + 231. Price US$99.75 (US and Canada); US$114.50 (all other countries). ISBN 0-8247-8425-1. Many practitioners of gas-liquid chromatography (GLC) are aware that the stationary liquid is not the only important item in a GLC column. The supposedly inert solid support can also have several major effects on analyses. Firstly, retention contributions often arise from adsorption by the support surface or gas-liquid interface. Secondly, the structure of the support controls the liquid distribution and hence the column efficiency.Thirdly, the support sometimes causes irreversible adsorption or catalytic activity. Finally, the supported liquid tends to age with time. These factors can all interfere with peak identification, qualitative and quantitative analysis, preparative and production scale separations, and with the measurement of equilibrium and other physico-chemical properties by gas chromatography. The cloud, however, also has several silver linings. The selectivity of a liquid phase can be improved by combining it with the powerful selectivity of a solid surface in the form of a modified active adsorbent. Adsorption at gadliquid and liquid/solid interfaces can advan- tageously be studied in GLC systems.In the first chapter of the book, Berezkin argues that these effects are so prevalent in GLC that the technique should be renamed ‘gas-liquid-solid chromatography (GLSC)’. In the remaining eight chapters he reviews the present state of knowledge of each effect in turn, including both solutions to problems caused by support effects and the exploitation of the effects for selectivity and physico-chemical study. Both packed and capillary columns are considered. The author is an established authority in the field; coverage of work over many years in the Soviet Union is comprehensive, of that in the West a little less so. The content is sound, except for the neglectful omission of the sorption effect in finite concentration equa- tions. The material is well organized and presented, though some repetition could have been avoided.Despite inadequate proofreading the English is good on the whole and only occasionally a barrier to comprehension. It is a pity the index is so sketchy and a list of symbols absent. The book emphasizes the fundamentals of GLSC but the practical implications are made clear. Each chapter normally begins at the level of basic chromatographic principles, with standard equations recapitulated where necessary. The book will be of much interest to specialists in the GLSC area of GC for whom it provides an excellent survey of an important and extensive body of work that is less widely known outside Eastern Europe than it should be. More generally the book should also be comprehensible to all chromatographers with a good basic understanding of GC wishing to study the role of the support in depth.J . R. ConderANALYST, FEBRUARY 1993, VOL. 118 19N FT-ICR/MS: Analytical Applications of Fourier Transform Ion Cyclotron Resonance Mass Spectrometry Edited by Bruce.Asamoto. Pp. x + 306. VCH. 1991. Price DM134.00; f47.00. ISBN 0-90573-767-1 (VCH Publishers); 3-527-27919-9 (VCH Verlagsgesellschaft). Most people who make use of mass spectrometry to solve problems in analytical chemistry are aware of the advantages offered by FT-ICWMS. The technique can provide high mass analysis, high resolution and mass accuracy, fast scan times, positive and negative ion capability and compatibility with pulsed ionization techniques-almost a wish list for the analyst. Yet very few of us have ever seriously considered it as a routine analytical technique presumably because of its perceived difficulties. There has been an obvious need for those workers using FT-ICWMS to describe how the tech- nique is proving of benefit in their work in order that the rest of the analytical community can assess its utility, versus other MS methods, for specific applications.This publication, edited by Asamoto, attempts to fill this gap by detailing some of the applications to which FT-ICR/MS has been applied. Two introductory chapters cover, respec- tively, the historical development of FT-ICR and other techniques based on the cyclotron principle of mass analysis, and a detailed review of the range of FT-ICR instrumentation currently available. These chapters are well written, manage to explain the technique and the equipment without the use of a highly mathematical approach and provide an excellent introduction to FT-ICR.As the stated aim of this book is to emphasize work being done to solve real problems, most of the authors of the eight following chapters on the applications of FT-ICWMS are, like the editor, involved in industrial analysis. This occasionally means that the amount of detail given about any analysis is less than would be provided by an academic author but this reviewer did not find this to be a problem. One chapter covers the linking of modern sample handling and ionization tech- niques with FT-ICWMS, and there are specific chapters on GUMS, laser desorption using a pulsed C 0 2 laser, surface analysis by ultraviolet laser microprobe, chemical ionization and on peptide analysis.The final chapter by a group from American Cyanamid describes the use of their laboratory- built instrument to solve problems arising from the agrochem- ical and biotechnology areas. These chapters stress the advantages to be gained from the unique features of FT-ICW MS but do not neglect to point out where difficulties have been encountered. Despite the excellent appearance of the book (it is fully typeset), there are errors in certain of the tables and figures. I would point specifically to Tables 3.1 and 9.5 where several of the ionic formulae are clearly wrong, and to Fig. 7.4 where the ion at mlz 325 is incorrectly assigned in the legend. These are, however, only minor quibbles.This is a first-rate book and I recommend it without reservation both to the general analytical chemistry community and to all users of mass spectrometry. The editor and his co-authors should be congratulated on achieving the aims they set themselves and on producing such a readable and timely publication. John J . Monaghan Principles of Polarography By R. C. Kapoor and B. S. Aggarwal. Pp. xi + 185. Wiley. 1991. Price f28.50. ISBN 0-470-21732-4. The University Grants Commission, New Delhi, provided the incentive and a grant for the writing of this book, which was a collaborative effort between a senior author and a young chemist for the benefit of honours and postgraduate students of chemistry in Indian Universities. It contains 13 chapters and some 180 pages.It has been published by Wiley Eastern Ltd. in a compact 9 X 6 inch edition and overall, I found it written in an easy-to-read style and of value to students of the subject whether in higher education or in industry. The majority of the text is concerned with polarography (€15 pp.). Chapter 1 introduces the subject, Chapter 2 is concerned with polarographic apparatus, Chapter 3 with currents in polarography such as charging, migration, diffu- sion, kinetic, catalytic and adsorption currents. Reversible systems are dealt with in Chapter 4, and irreversible systems in Chapter 6 together with their associated mathematics. Chapter 5 deals with the polarography of complex (as in metal complex) systems and derives mathematical relationships from which for example overall stability constants can be calculated.This is an area of study in which the authors themselves have been actively involved, e.g. , Kapoor and Aggarwal, Indian J. Chem., 1972, 11, 71, on Ce”’ and Ce’” complexes of N , N-dihydroxyethylglycine. Chapters 7 and 8 concern themselves further with kinetic, catalytic and adsorp- tion currents whereas Chapters 9 and 10 deal with polaro- graphy in non-aqueous solvents and polarography of organic compounds, respectively. Chapter 11 is entitled Other Indicator Electrodes and is involved with the construction and use of the hanging mercury drop electrode, platinum, gold and carbon electrodes, etc. Special polarographic techniques are the subject of Chapter 12 with pulse and differential-pulse polarography receiving only four pages of consideration, square-wave polarography only one and stripping techniques only three.This is hardly in proportion to their current usage. The book concludes with a chapter on amperometry. Pages 164 and 165 mention the older polarographic literature and little mention is made of more recent publications, particularly in the applications area. The Appendix on polarographic characteristics of metal ions, anions and organic compounds could have been added together with the addition of a table concerned with stripping voltammetry of metal ions and organic molecules. W. F. Smyth HPLC in the Pharmaceutical Industry Edited by Godwin W. Fong and Stanley K. Lam. Drugsand the Pharmaceutical Sciences. Volume 47. Pp. viii + 309. Marcel Dekker. 1991. Price US$99.75 (US and Canada); US$114.50 (all other countries).ISBN 0-8247-8499-5. This volume has been prepared in 4 parts each containing between two and four chapters. Part One is entitled ‘Contemporary LC Techniques in Pharmaceutical Analysis’ and has three chapters. The opening chapter by P. Kucera and N. Licato, ‘High Speed HPLC using Short Columns Packed with 3 vm Particles’ discusses theoret- ical aspects and design of instrumentation for high-speed separations. The importance of equipment specifically desig- ned for high-speed separations is particularly emphasized by considering the dispersion processes that operate within different parts of a system. The title of this chapter might be considered misleading since the content includes much material concerned with microbore columns. However, since this does not interfere with Chapter 2 and it certainly enhances this chapter, this reviewer would only suggest a change of title.Chapter 2 by T. V. Raglione and R. A. Hartwick concerns ‘Microbore HPLC in Pharmaceutical Analysis’. This chapter essentially reviews the advantages of microbore systems such as improved mass sensitivity for bioanalytical applications and the facility to interface with other detection systems. Chapter 3 by F. K. Chow concerns ‘Column Switching Techniques in Pharmaceutical Analysis’. This is an unusual but worthwhile topic to include in such a publication on HPLC20N ANALYST, FEBRUARY 1993, VOL. 118 and discusses various column and valve geometries that can be used for chromatographing analytes in complex matrices.Part Two is entitled ‘Specialized Detection Techniques’ and includes four chapters. Chapter 4 by P. T. Kissinger and D. M. Radzik discusses and provides several examples of applica- tions using electrochemical detectors and Chapter 5 similarly describes radiochemical detectors. In Chapter 6, L. Huber and H. P. Fielder describe the photodiode array detector and using antibiotic examples they discuss the various data manipulations that are possible with the information collected by this detector. Chapter 7 by K. S. and V. F. Kalasinsky concerns HPLC coupled with FTIR. Interface designs are described that involve solvent removal, especially water, from eluate frac- tions and deposit analytes on a suitable substrate for diffuse reflectance spectroscopy.Part Three includes two chapters on ‘Automation in Pharmaceutical Analysis’. Chapter 8 by W. A. Hanson concerns ‘Applications of HPLC to Dissolution Testing of Solid Dosage Forms’. Advantages of monitoring dissolution samples by HPLCp. are provided, such as for products containing low concentrations of active ingredients, products with excipients that can interfere with other analytical methods and multicomponent products. Chapter 9 by R. A. Felder concerns ‘Robotic Automation of HPLC Labora- tories’. Different types of laboratory robot are defined and, in particular, their use in sample preparation is discussed. Part Four includes two chapters on ‘HPLC of Peptides, Proteins and Enantiomeric Drugs’. Chapter 10 by K. H. Bui concerns LC resolution of enantiomers.Various column and mobile phase combinations are reviewed, the advantages and disadvantages of systems based both on chiral and non-chiral stationary phases being discussed. Chapter 11 by K. Benedek and J. K. Swadesh concerns HPLC of proteins and peptides. This chapter relates method development with peptide structure including conformation and presence of prosthetic groups. In addition, problems of denaturation and peptide heterogeneity are discussed. This book provides excellent reviews of several aspects and applications of HPIX of pharmaceutical interest many of which are not normally to be found within textbooks on HPLC. Criticisms include: ( a ) some chapters contained several typographical errors, some of which could be quite misleading; (b) many of the figures are taken from previous publications and in some cases the legends are inadequate to satisfactorily explain them (this is presumably because addi- tional explanatory details were provided elsewhere in their original publications); and (c) in some chapters references are not sufficiently up to date.In spite of these shortcomings it is considered that this volume will be of great value particularly to analysts with experience of HPLC as an introduction to some specialized techniques used in pharmaceutical analysis. G. P. R . Carr A Handbook of Silicate Rock Analysis By P. J. Potts. Pp. x + 622. Blackie. 1991. Price f45.00. ISBN 0-21 6-93209-2. The fact that P. J. Potts’ ‘A Handbook of Silicate Rock Analysis’ has appeared in paperback, some five years after the original hardcover edition, probably says more about its merits than any review.Those geoanalysts who baulked at the hardcover price now have no excuse but to acquire this outstanding volume. Potts’ subject matter is extensive and his coverage encyclo- paedic. He is able to convey a general message without sacrificing a sense for detail. The result is a wcll-balanced work, conveying the concepts of geoanalytical techniques on the one hand, whilst providing a wealth of procedural detail on the other. Potts is a diligent writer, able to communicate scientific principles clearly without resorting to simplification. He prefaces the book by noting that the introduction of microcomputers and the resultant lack of interaction between user and machine has encouraged a ‘black box’ attitude towards analytical chemistry.His stated purpose has therefore been to provide an appreciation of what happens between ‘samples in’ and ‘results out’. He claims: ‘All analytical techniques available for routine silicate rock analysis are discussed. Sufficient detail is included to provide practitioners of geochemistry with a firm base from which to assess current performance, and in some cases, future developments’. This is no mean claim and the book lives up to it admirably. It is a remarkable foundation for those involved in the analysis of silicate rocks and is ideal as a course text. However, this is primarily a book for the analyst, written from a laboratory perspective. As such it is eminently practical. Its focus is on contemporary geoanalytical tech- niques, and 17 of its 20 chapters deal with specific instrumental techniques.In general the level of detail is appropriate to the subject, although in some cases I would have hoped for more. For example, in the wavelength-dispersive XRF section, the measurement of background is discussed but not the problem of needing to know the background at the peak position, but being unable to measure this in the sample itself. Potts’ approach necessarily results in an emphasis on specific procedures at the expense of a more holistic approach to methodologies. The choice is logical, given the ‘Handbook’ format, and Potts does devote 40 pages to general concepts, including sampling, contamination, reference materials and analytical data reporting in his opening chapter. There is an excellent expusk on ‘detection versus determina- tion limits’, which should be requircd reading for all who set foot in a geoanalytical laboratory. Typically, this focuses on the limits associated with an individual technique rather than those associated with a complete ‘method’ ( i e . , including sample preparation, preconcentration, measurement and data manipulation). In terms of production quality, the book has a clean presentation style for its text and the large, 8 X 11 in, format reduces the amount of page-turning required by the reader within each section. The binding could be stronger for a work that will be referenced frequently. The figures are generally well-presented; however, despite the large format, the layout of tables is frequently poor. Considering that this is essentially a second printing it is disconcerting to find a number of typographical errors. Generally speaking, the five years since this book first appeared have done little to date it. However, it is unfortunate that there are no references to ICP-MS work later than 1983 and that the text is necessarily light on recent advances in robotics. Of all the recently published books with relevance to geoanalysis, I can think of none to equal Potts. Chris Riddle