Analyst, October 1996, Vol. 121 143N Book and Software Reviews AAS SoftBook By Cognitive Solutions Ltd. Revised and Updated. January 1995. Price f295.00 (plus VAT); US$ 529.00 This is a software-based text on AAS which takes the novice from basic theory through to a number of applications. The software is very simple to install, aided by the manual which takes the operator through a step-by-step procedure. The manual itself contains no subject matter, but is a well written guide to the structure and operation of the software package. Once installed, the operator is then given the option to go straight into the programme or to run through a tutorial, which explains such things as how to use a mouse, the basic concepts of using Windows-based software and a brief explanation of how the software works.Once the tutorial has been completed, the user is returned to the home page. If the main body of the software is then opened, one of four discrete modules may be chosen. These are ‘Theory of AAS’, ‘AAS Instrumentation’, ‘Analysis with AAS’ and ‘Questions and Answers’. Any of these modules may be opened by clicking on the appropriate icon. It will then load, producing a module overview page. Each module is comprised of 20-30 topic areas. These topic areas may be accessed individually by clicking on the appropriate icon, or alternatively may be accessed in series by clicking on one and then repeatedly clicking on the ‘next’ icon. In many of the topic pages there are so-called ‘hotwords’. If clicked upon, these will reveal a further page explaining more about the specific hotword.Some of the topic areas also have demonstration buttons. An example is a demonstration of the avalanche effect that occurs in a photomultiplier tube. Simple demonstrations such as this are a good use of this media and save substantial effort reading through reams of text. When finished with a particular topic, the user can return to the module overview page by clicking on the home icon at the bottom of the screen. Once the user finishes the last topic area the program will state that the module has been finished and will give the option of returning to either the main menu or to the home page of the module. If required, the next module may then be investigated in a similar fashion. When using the package, clear and concise instructions appear in boxes on most pages to aid the user.The questions and answers module is somewhat limited (only 10 questions for theory and a further 10 for applications) but does give the user an opportunity for self assessment. There is also an option to print a certificate of achievement! A pass mark is given at 50% for both the theory and applications tests. It must be said that this computer program is easy to follow and is very user friendly. Some of the material is, however, rather thin. In the monochromators section, for example, the Czerny-Turner style is shown, but there is no mention of the other types (e.g., Littrow and Ebert). Little detail is given about Zeeman background correction, and although the fundamental theory is probably unnecessary for this program, there is no mention that the magnetic field can be applied to either the atom cell or the source, or in a longitudinal or transverse manner.The program explains (nicely) how a hollow cathode lamp works, but fails to mention anything about electrodeless discharge lamps. But perhaps most importantly there is a complete absence of the use of isothermal operation (i.e., platforms or probes) in ETV. Since many applications use isothermal operation (and other elements of the STPF concept), I feel this really should have been included. Omissions aside, the program is refeshingly free of errors although the equation hidden under ‘photons’ in the electromagnetic radiation part of the theory section is expressed as E = h/v rather than E = hv. Overall, I feel this is a useful and well structured teaching package.It would benefit from a more comprehensive questions and answers section, perhaps interactive with the main text and suggesting further reading. However, overall the package is good value for money and I am sure it will prove popular with students and trainees who respond to material in this format and who wish to know more about the fundamentals of AAS. Steve Hill 5199074C University of Plymouth Selective Detectors. Environmental, Industrial and Bio- medical Applications Edited by Robert E. Sievers. Volume 737 in Chemical Analysis: A Series of Monographs on Analytical Che- mistry and its Applications. Series editor J. D. Wine- fordner. Pp. xxi + 262. Wiley. 1995. Price f49.95. ISBN 0-47 1-01 343-9.Although the title suggests that this book provides a com- prehensive review of selective detectors and their application in chemical analysis, it focuses on some of the more recent developments and is therefore a text for the specialist rather than the novice chromatographer seeking an overview of the subject. Overall there is too much emphasis on atomic (rather than molecular) detectors and I was surprised to see no contribution on molecular mass spectrometric or infrared detection systems. However, the book is well produced with clear illustrations and the balance between the operational principles and applications of the detectors described is good. The first two chapters deal with sulfur-selective chemilu- minescence (CL) detection and concentrate on ozone-induced CL.In the first contribution the authors describe two detectors they have developed, one of which converts sulfur compounds dissolved in aqueous solutions to SO using high temperatures and pressures and has been employed for selective detection in analytical and preparative HPLC systems. The second chapter is devoted to flameless sulfur CL detection and describes applications of this detector in combination with GC and SFC. Most of the third chapter covers applications of detectors employing the NO-ozone CL reaction. These include the analysis of N-nitroso compounds; organonitrogen species in petroleum samples; nitrate and nitrite ions in water and foodstuffs; and nitric oxide, nitrogen dioxide and ammonia in the atmosphere. Indirect analysis, by measuring the NO produced when samples are oxidized by nitrogen dioxide, is also discussed.‘it focuses on some of the more recent developments and is therefore a text for the specialist rather than the novice chromato- grapher seeking an overview of the subject’ The oxygen-sensitive flame ionization detector (0-FID), the recent development of which has been catalysed by the need to determine oxygenated hydrocarbons in fuel, is the subject of chapter four. The major application areas of 0-FID (i.e., oxygenates in automotive petroleum and flavours and fra- grances in natural products) are outlined and the chapter concludes with some useful remarks on 0-FID operation which should help the newcomer to avoid many of the pitfalls experienced by the author.144N Analyst, October 1996, Vol.121 Chapter five is essentially a paper describing the experimen- tal optimization of a metal-selective FID for the determination of elements such as aluminium, iron, tin, lead and manganese. This contribution contains little information on applications of the detector and will be of interest to only a few readers. GC-atomic (plasma) emission spectroscopy is described in chapter six, which concentrates on the widely used microwave- induced helium plasma. A good list of references is given to papers where GC-atomic emission detection has been used to determine metallic and non-metallic elements, and the author concludes with the view that this detection technique will be used increasingly as commercial instrumentation becomes more widely available.The following chapter continues the theme of plasma sources but deals with mass spectrometric (MS) detection. The great analytical power available from the combination of chromatography (for speciation) with in- ductively-coupled plasma (1CP)-MS (for selectivity and sensi- tivity) is emphasized, and the significance of this combination illustrated with a brief account of the biological significance of different chemical forms of a range of ‘environmentally sensitive’ elements. HPLC rather than GC is most frequently combined with KP-MS, as witnessed by the variety of HPLC separations reported in this chapter. The concluding sections of this comprehensive account focus on the combination of GC and SFC with ICP-MS detection systems. The penultimate chapter deals with peroxyoxalate CL detection and somewhat overstates the sensitivity of this technique compared with fluorescence.Following a fairly detailed account of the mechanism of the peroxyoxalate reaction, the remainder of this contribution deals with the design and optimization of instrumentation for peroxyoxalate CL and describes some applications of the technique. The book concludes with a fascinating chapter which is essentially a mini-autobiography of James Lovelock’s scientific career. This pioneer of selective detection provides a fascinating insight to how some of the analytical devices that we nowadays take for granted have their origins in completely different areas. He also emphasizes the value of regular personal contact between supervisor and trainee, which is something we frequently overlook in these days of increased workloads and reduced staff numbers.S. Forbes 5190044A Shell Research Limited Chester Modern Infrared Spectroscopy By Barbara Stuart. Analytical Chemistry by Open Learn- ing. Edited by David J. Ando. Pp. xx + 180. Wiley. 1995. Price f 17.95. ISBN 0-471-95917-0. Modern Infrared Spectroscopy is one of the latest books in the ACOL (Analytical Chemistry by Open Learning) series. In common with the other texts the book concentrates on a limited area of analytical chemistry and then aims to make it accessible to readers who may be following a course, doing a self-tuition programme, or are otherwise new to the area. For readers unfamiliar with Open Learning, the text follows a pattern established by bodies such as the Open University.Thus a complex set of ideas is presented in a series of well- defined blocks. Each block is broken into smaller segments which allows the student to make effective use of even small increments of study-time. Regular use of self-assessments related to the material helps the student gain confidence in how much has been assimilated during their study. Dr. Barbara Stuart of the University of Technology, Sydney, deserves congratulations for writing a very readable and interesting book on modem infrared spectroscopy. The empha- sis of the book is on the choice of effective sampling methods. The main instrumental method is almost assumed to be FTIR, although sufficient information on dispersive systems is included. There is a section on the identification of unknown materials via correlation charts and typical vibrations, but this does not form the bulk of the text as it might have done a few years ago.There are a lot of clear drawings and some good-quality spectra to assist the novice in all stages of infrared analysis. Background theory, including signal processing, is integrated into the text in a readily assimilated format. All the major sampling methods are discussed and critical appraisals given of their strengths and weaknesses. There are also about 30 original problems in the book. These range from simple numerical conversions through to complex questions involving calibration graphs and the identification of unknowns. These problems form the core of the self-assessment process and so fully worked answers are provided.In comparison with some of the courses provided by instrument manufacturers, ACOL texts offer a cost-effective resource which can be used to produce in-house training packages. There are also courses run by the RSC which can lead to the award of LRSC. J . E . Newbery 5190098K Greenwich University Practical Gamma-ray Spectrometry By Gordon Gilmore and John Hemingway. Pp. viii + 314. Wiley. 1995. Price f60.00. ISBN 0-471-95150-1. This book is based on notes used for a series of practical gamma-ray spectrometry courses run by the authors at the Universities Research Reactor at Risley. The authors’ intention was to provide more of a workshop manual than an academic treatise. In this they have eminently succeeded. The book contains all the information which a newcomer to the technique of gamma-ray spectrometry would need to understand the principles underlying the technique and to set up and run a practical operating system for real applications.Chapters are included on radioactive decay and the origin of gamma- and X-rays; interactions of gamma radiation with matter; semiconductor detectors for gamma-ray spectrometry; electronics; counting statistics; spectrometer calibration; co- incidence summing; computer analysis of spectra; scintillation spectrometry; choosing, setting up and checking the specifica- tion of a detector; resolution; troubleshooting; low-count rate systems; high-count rate systems; and ensuring quality in gamma-ray spectrometry. Five appendices provide useful sources of further information, decay data for detector calibra- tion standards, data on background gamma-rays including those from Chemobyl fallout, a list of chemical names and symbols and details of suppliers of spectrometry equipment.‘would be invaluable for anyone setting up, or operating, a gamma-ray spectrometry system for practical applications, Much of this material is, of course, also contained in other texts and comparison can be made with, for example, ‘Gamma- and X-ray Spectrometry with Semiconductor Detectors’ (K. Debertin and R. G. Helmer, North-Holland, 1988). The strength of Gilmore and Hemingway’s book lies in the wealth of practical information and advice which appears throughout the text and which is collected together at the end of each chapter in a section entitled ‘Practical Points’.Their chapters on scintilla-Analyst, October 1996, Vol. 121 145N tion spectrometry (still important for many applications) and on troubleshooting do not appear in the Debertin and Helmer text. The latter book is a detailed treatise on gamma- and X-ray spectrometry and one would expect to find it on the shelves of radionuclide metrologists and nuclear physicists. The Gilmore and Hemingway book, on the other hand, would be invaluable for anyone setting up, or operating, a gamma-ray spectrometry system for practical applications such as neutron activation analysis, environmental monitoring or measurements related to the nuclear fuel cycle. The chapter on low count rate systems, for example, will be particularly relevant to measurements on environmental radioactivity; whilst that on high count rate systems will have particular relevance to measurements of nuclear fuel.The book must be highly recommended to anyone involved with gamma-ray spectrometry. Desmond MucMuhon 5190045 J Imperial College NMR Techniques in Catalysis Edited by Alexis T. Bell and Alexander Pines. Pp. viii + 432. Marcel Dekker. 1994. Price $165.00. ISBN 0-8247-9173-8. Nuclear magnetic resonance (NMR) spectroscopy has emerged as a powerful technique to investigate the structure of solid materials. in view of the importance of heterogeneous catalysis to modern chemical processes, it has proved to be a major growth area for the application of solid state NMR techniques. As well as providing unique information on the chemical environment of specific nuclei in catalysts or species adsorbed on the catalysts, NMR can monitor the connectivities and dynamics of these environments and species.This book is the first that has attempted to cover the many diverse applications of NMR in heterogeneous catalysis. After a brief introduction, by the editors, to basic NMR concepts and the type of information that can be obtained from modern techniques, the book comprises six chapters written by leaders in the field (Maciel, Karger, Fyfe, Haw, Eckert and Haddix) on the application to specific areas in heterogeneous catalysis. These include zeolites and related areas, molecular diffusion, in situ measurements, bulk oxide catalysts, silica and alumina surfaces and layered materials (clays, aluminophos- phates and metal sulfides).The chapters highlight the major role 29Si and 27A1 NMR play in the characterization of aluminosili- cates, the growing number of other catalytically-important nuclei that can be investigated by NMR (e.g., 3lP, 17O,5lV) and the key role of lH, l3C and 31P in probing adsorbed species and acidity (Bronsted and Lewis acid sites), together with the skill and ingenuity that has gone in to providing information on diffusion and in situ measurements. The final chapter of the book provides a very brief overview of emerging techniques. ‘the book represents a valuable and unique reference source on the application of NMR techniques to heterogeneous catalysis’ Although under the themes chosen for the chapters, it is clearly impossible to include every application of NMR to catalytic science, there are relatively few omissions.Perhaps a chapter devoted specifically to NMR could have brought together more of the work on adsorbed species and the importance of the technique for characterizing catalytic coke. Some of the overlap between the different chapters on the presentation of essential theory for the various applications covered (particularly cross-polarisation, magic-angle spinning) could have been avoided by having an expanded introductory chapter. The final chapter of the book is somewhat disappoint- ing in that the reader not conversant with NMR is left with barely a superficial understanding of the emerging techniques. Further, no attempt has been made to cross-reference these techniques to where they appear in other chapters and the other chapters, particularly those covering aluminosilicates, could have been intergrated to a greater extent.Putting aside these relatively minor criticisms, the book represents a valuable and unique reference source on the application of NMR techniques to heterogeneous catalysis and its purchase is highly recom- mended for those working in the field. Colin E. Snupe 41901 06A University oj Strathclyde ICUMSA. International Commission for Uniform Meth- ods of Sugar Analysis By ICUMSA. Pp. xxxvi + 438. ICUMSA Publications. 1995. Price f42.00; ISBN 0-905003-14-4. The proceedings of the twenty-first session of the International Commission for Uniform Methods of Sugar Analysis (ICUMSA), held in Havana in May of 1994 is published by ICUMSA itself, and runs to xxxviii pages of introduction, followed by 424 pages of the proceedings of the meeting, accompanied by an index.The introductory pages incorporate a revealing blow-by-blow account of the structure, politics, allegiance, and financial viability of ICUMSA itself. Discussion of the last point dwells considerably on the substance and construction of this very volume; its cost and the likely return against those costs. Whilst of minimal curiosity value to the general reader, none of these topics is of general interest and would be better reported, in the opinion of this reviewer, internally to the ICUMSA as minutes to relevant management committee meetings. Regrettably that style is maintained throughout this produc- tion. Its content can be briefly described as being a mixture of ICUMSA’s definitions of the requirements for sugar analysis, accompanied by elaborate internal disucussion as to how to establish those criteria.The text covers many, but not all, of the required categories. Those that it does deal with are, to the credit of the authors, presented in clear and acceptable format. They range widely from raw sugar determination to chromatographic techniques for sugars. The principal drive is, however, directed not to analysis itself, but to the formulation of particular protocols for sugar analysis, the intention being their adoption as self-imposed internal regulatory controls, and presumably directed to the general acceptance, by others, of those protocols. It is clear that ICUMAS’s efforts would be well served by a wider view of the development of the science, by others, in each of those many categories covered by this text.Instead the organisation takes an introspective view, and at length, tends only to discuss and report those analytical developments conducted by its own members, in the period between this and their previous report. This reviewer is of the opinion that this text will be of considerable value to the delegates of the meeting in question, of some minimal interest to those in the sugar industry, but only of curiosity value to anyone working in the wider fields of carbohydrate chemistry and their analysis. in summary, this text will necessarily appear to the general reader as a peculiarly introspective account of a meeting held by just another vested interest group.Ivor Lewis 51 90068I King’s College London146N Analyst, Octohei. 1996, Vol. 121 Advances in Chromatography. Volume 36 Edited by Phyllis R. Brown and Eli Grushka. Pp. xvii + 444. Marcel Dekker. 1995. Price $175.00. ISBN 0-8247-9551-2. After 35 volumes this series can certainly be called well established. Like previous volumes it contains a series of chapters across a broad spectrum of interest. This volume is no exception and covers mathematical methods and detection principles as well as more mainstream topics. This diversity make(; reviewing difficult as many of the eight topics covered are of a highly specialist nature. The first chapter, by Cserhiiti and Forgiics (Central Research Institute for Chemistry, Budapest, Hungary) on the use of multivariate methods for the evaluation of retention data focuses heavily on the applications of a variety of techniques and assumes that the reader has at leust a reasonable working knowledge of the methods used although references to more detailed works are given as well as to data sources.Chapter 2 is a very readable account of the liquid chromatography of the fullerenes by Jinno and Saito (Toyoha\hi University of Technology, Japan). It is well illustrated and gives an excellent insight into liquid-crystal bonded phases. The next 2 chapters and chapter 8 concern themselves with the application of capillary electrophoresis (CE) to biomolecules. Cohen, Smis- mek and Wang (Hybridon. USA) describe the use of CE-MS in sequencing of oligonucleotides whilst Oda, Madden and Landers (Mayo Foundation/Mayo Clinic, Rochester, USA) cover the analysis of glycoproteins and glycopeptides.Lunte and Lunte (University of Kansas, USA) discuss microdialysis sampling in pharmacological studics and its applicability to HPLC and CE. Whilst specialist in nature, they are all well written and well referenced. ‘Overall, this volume continues the tradition and standards set by previous volumes in the series and will find a place in many library collections a Chapter 5 is somewhat different as it is a detailed review of LC methods (413 references) for the screening of biological fluids for drugs of abuse (Binder. Bio-Rad Laboratories, Hercules, USA). It covers specific drug separations as well as broad spectrum screening.It is very readable as well as being most informative. The role of electrochemical detection for molecules of biological interest is the subject of the next chapter by Chen, Woltman and Weber (University of Pittsburgh, USA). The application of electrochemical methods for detection of a wide variety of moleculec at low levels of concentration is discussed and the conflict of sensitivity and specificity is explored. Chapter 7, by Lindon (Wellcome Research Laboratories), Nicholson (Birkbeck College) and Wilson (Zeneca Phar- maceuticals) tJK, discusses the development and application of the hybrid technique of HPLC-NMR. After discussion of the basic theory and experimental aspects, its application to drug metabolism studies and biochemical analysis is discussed.Overall, this volume continues the tradition and standards set by previous volumes in the series and will find a place in many library collections. C . R ui;qes s 619001 2G Co. Dur-ham Encyclopedia of Nuclear Magnetic Resonance. Volume 1. Historical Perspectives Edited by D. M. Grant and R. K. Harris. Pp. xii + 814. Wiley. 1996. Price f125.00; ISBN 0-471-93871-8. ~~~~ ~~~~ ~~~~ ~~ ~ ~~~ I find that students at all levels respond enlhusiastically to the teaching of NMR spectroscopy via an historical perspective: the failure of Gorter to detect nuclear resonance in the 193Os, the success of Felix Bloch and co-workers at Stanford and of Edward Purcell and colleageus at Harvard in the 1940s, followed by the unexpected discovery of the chemical shift and of spin-spin coupling, phenomena which we all take for granted these days.Then there was Albert Overhauser, the young (in 1953) theoretician who predicted that, in a metal, the saturation of the ESR resonance of the electrons should lead t o an enormous increase in nuclear polarization; nobody believed him (his presentation to the American Physical Society went down like a lead balloon!) until Charles Slichter demonstrated it to be so later that year. Without the (nuclear) Overhauser effect, we would not now be using multinuclear NMR methods to solve the structures of proteins as big as 25 kDa. ‘definitely the volume for introducing all aspects of NMR to students’ NMR spectroscopy is one of the few techniques which has continued to evolve; almost every year useful new advances in the instrumentation or pulse sequences (but remember the days of continuous wave NMR) seem to appear. A large number of research workers have made important contributions and most of them are detailed in this volume, not only for high resolution spectroscopic studies of liquids but also for solids (e.g., the major impact of magic angle spinning introduced by Raymond Andrew in Nottingham in 1960), and imaging. Paul Lauterbur says that ‘The invention of NMR imaging (MRI) can be traced back through a variety of specific incidents to a set of underlying interests developed in my childhood.’: enough to arouse the curiosity of any reader! This is a heavy volume, one for the library and not for carrying home very often, but definitely the volume for introducing all aspects of NMR to students. I can see a market for a slimmer version which can be carried home (and is affordable), perhaps a fifth the size, with just the key people (can we agree on them?). As Silvio Aime pointed out in hi\ contribution ‘The personal pathway sketched in this brief report may closely resemble the story of many (hundreds, thousands‘?) of researchers who had the fortune to meet the splendid armoury of NMR spectroscopy early in their career.’ Long may the good fortune continue. Peter J . Sadlei- 6190035 F Ut?iversity of Loidon