Analyst, November 1996, Vol. 121 155N Book Reviews Supercritical Fluid Extraction By Larry T. Taylor. Techniques in Analytical Chemistry. Pp. xiv + 182. Wiley. 1996. Price f40.00. ISBN 0-47 1 - 1 1990-3. This is a welcome volume on supercritical fluid extraction (SFE) as it is written by a single author. Previous volumes have often been edited collections of chapters by a number of authors and therefore present the subject in a complex way. By contrast, this is a clear and less complicated account, which nevertheless addresses the important issues. The author has published research papers in supercritical fluids, although this is part of a wider analytical interest. He has run a series of successful analytical courses at this Institute, including ACS short courses on SFE and chromatography.He is thus well placed to provide an introduction to the subject. Reviewing this book inevitably raises the question of where SFE for analytical sample preparation is heading at the moment. It is undoubtedly going through a bad patch at present and seeing competition from new small-scale liquid separation techniques, which also reduce the use of organic solvents. The reasons for this are rather unfair. Firstly, it is apparent from research that SFE is only partially successful and the matrix does not always release all the analytes. This is unfair in comparison with liquid extraction because the detailed informa- tion about percentage recoveries obtainable from SFE is not available from liquid extraction because the latter technique is too time-consuming. Often SFE does better than liquid extraction.The second reason is that SFE appears very complex because of the way it is presented, often in ‘difficult’ papers. I hope the clear account given in this book will repair this second problem. For the analytical chemist this volume is an excellent and painless introduction to SFE for analytical sample preparation. It would be my first choice for someone contemplating the use of SFE. Those who routinely use liquid extraction should read this book to get a straightforward view of the SFE alternative. 6190038K A . A. Clifsord University of Leeds New Frontiers in Agrochemical lmmunoassay Edited by David A. Kurtz, John H. Skerritt and Larry Stanker. Pp. vii + 318; AOAC International. 1995. Price $93.00 (USA, Canada and Mexico); $97.00 (outside North America).ISBN 0-935584-58-7. Immunoassays in one form or another have been described for the vast majority of agrochemicals. In turn, many of these methods have been employed worldwide in routine analytical testing programmes. This book opens with a section devoted to outlining the analytical requirements of screening tests used in regulatory work. Pesticide and herbicide immunoassays are used as examples but the concepts discussed are applicable to most hapten immunoassays. The second section of the book addresses the chemical manipulation of haptens to yield high molecular weight conjugates suitable for generating immune responses and producing enzyme conjugates. This detailed review makes this an excellent reference point for those wishing to produce hapten derivitives suitable for developing an immunoassay.Section three is concerned with immunoassay formats. An interesting chapter within this section outlines some of the emerging techniques in developing field immunoassays. A further chapter deals with some aspects of immunoassay troubleshooting. There are notable absences of alternate immunoassays formats, particularly those using labels other than enzyme based. Similar descriptions for fluorescent, time resolved fluorescent and chemiluminescent applications would be a useful addition to future editions. Section four details some of the methods used to prepare samples for analyses by immunoassays. Solid phase extraction and immunoaffinity chromatography are described in reason- able detail.Many other techniques appear to have gone unmentioned. The penultimate section is centred on recent advances in immunoassay methods and here truly lies some of the ‘new frontiers’. The development and application of recombinant antibodies should be of particular interest to many workers in the field of immunoassay development. The book closes with descriptions of some of the methods used to analyse data generated by immunoassays. Though less exciting to read than some other areas of the book the importance of this subject should not be underestimated. This book covers many of the important aspects of develop- ing, validating and implementing immunoassays into routine monitoring programmes. There appears to be a strong bias towards pesticides and herbicides.Compounds such as antibiot- ics and steroids are notable absentees. Despite these limited shortfalls this book is quite an excellent guide to developing immunoassays in general and an even better guide to what might be possible in the future. 5190095F Chris Elliott Department of Agriculture of Northern Ireland Innovations in Supercritical Fluids: Science and Tech- nology Edited by Keith W. Hutchenson and Neil R. Foster. ACS Symposium Series 608. Pp. x + 470. American Chemical Society. 1995. Price US$125.95. ISBN 0-841 2-3324-1. This book is not primarily for the analytical chemist, as its subtitle implies. It has no chapters directly on supercritical fluid chromatography or analytical supercritical fluid extraction. It is a significant addition to the important volumes on supercritical fluids in the ACS Symposium Series.In this case it contains selected papers from those present at the ‘Symposium of Supercritical Fluid Science and Technology’ held as part of the 1994 Annual Meeting of the American Institute of Chemical Engineers. There is an introductory chapter by the editors reviewing current research on supercritical fluids. There are sections on molecular interactions and phase behaviour, chemical reactions, and an unusual section on ‘ Supercritical Fluids in the Forest Products Industry’ with an introductory chapter reviewing the area. Chapters of peripheral interest to the analytical chemistry are those on the choice of cosolvents for the extraction of pesticides, extraction from polymer matrices, two chapters on the extraction of contaminants from soils and extrdction from yew.For those working in general in supercritical fluids the book is an indispensible addition to their library. It would be of interest in those analytical laboratories which get involved in preliminary studies of possible processes. For analytical chemists, unless involved specifically in the applications listed above, this volume is only of minor interest. 61900220 A. A. Clifford University of Leeds156N Analyst, June 1996, Vol. 121 Electric Field Applications in Chromatography, Industrial and Chemical Processes Edited by Takao Tsuda. Pp. xiv + 312. VCH. 1995. Price DM298.00. ISBN 3-527-28687-X. At first sight this book may give the impression that the unsuspecting potential reader has acquired a kind of scientific ratatouille.On closer exploration into the various items presented, it transforms into a scientific kaleidoscope. Finally for those scientists interested in separation techniques the ingredients metamorphose into a collection of carefully selected themes, expressing the wide interests of Professor Tsuda. In mass transport phenomena, underlying all separation processes, almost always fundamental ‘classical’ driving forces are used. Amongst others a choice can be made from, e.g., gravity (centrifuge), pressure (gas, liquid chromatography), electric field strength (electrophoresis), or magnetism (mass spectrome- try). Nature makes it possible to create and apply these forces in different ways and magnitudes, to cover a wide range of solutes with a wide range of molecular weights.In experiments, sometimes phenomena occur that have to be suppressed or stimulated, e.g., electroosmosis. Applying just one kind of separation principle does not deliver the desired result. A combination of the above mentioned forces with physical phenomena such as adsorption, sieving, chemical reactions in well defined compartments, may result in a specific separation technique, which sometimes we believe we understand com- pletely. In these new horizon areas, this book has a lot to say. Although performance properties can create conditions for a specific separation principle, the rules of mass transport still form the basic assumptions, defining the potential and limits of separation. Nevertheless, the variations themselves are realised through a vast and highly diversified array of instruments and procedures described in the scattered literature.It is therefore sometimes difficult to collect information for a specific problem in separation science in order to optimize the solution, because as always many roads lead to Rome. In this book an attempt is made to create an intersection of applications and experiments, in which electric field and chromatography have been chosen for industrial and chemical processes. In addition to a well written clear introduction and summary (Chapter l), this book comprises three sections: in Chapters 2-6 main attention is paid to electrochromatography; in Chapters 7-1 1 applications in industrial processes are discussed; in Chapters 12-14 applica- tions to concentration, immunoassay and molecular orientation are given.‘On closer exploration into the various items presented, it transforms into a scientific kaleidoscope. ’ In Chapters 2 4 , dealing with electrochromatography, the reader is introduced into a world of analytical separation where zone profiles, created both with and without electroosmotic flow, play an important role. As a comparison, pressurised flow is discussed. The (dis)advantages are shown not only in simple formulae, but the information is larded with many pictures and photographs. In Chapter 5 attention is paid to the preparative separation of biomolecules. In Chapter 6 it is shown that combining various principles can be fun if you like to construct home-made equipment and are not simply hoping that elaborate equipment will produce all pre-programmed work. In the following chapters work is presented especially to stimulate young scientists of our computerized world.Optimization of processes such as industrial electroosmotic dewatering, electro- phoretic formation of ceramics, novel materials for electrorheo- logical fluids, electric fields and their role in both solvent extraction and in resolution of water-in-oil emulsions, is still possible. In Chapter 12 attention is paid to industrial concentra- tion or desalting purposes, a feature rather unknown amongst many scientists in analytical separation techniques, making use of electrophoretic and/or chromatographic principles. In Chap- ter 13 pulse immunoassay and pulse electrovoltage for cell manipulation is presented, techniques which will need more attention and will attract (as iontophoresis already does), more interest in the next decade.Finally, in Chapter 14, an interesting discussion on electric field organised photochemistry is pre- sented, an important item, as it can be linked to the growing interest in chiral chemistry. To conclude this review, I think that for those scientists looking for a profound treatise in theoretical aspects of electrical field applications in chromatography, this book may be disappointing, as it will be for those eager to collect detailed information on the items discussed. But for those interested in aspects of influencing, combining, reducing or amplifying electric, magnetic and chromatographic parameters it will give satisfaction.The unifying feature of the role of the electric field, as presented in this book is the displacement of solvent or migration and/or orientation of solutes. Much more thrilling phenomena are described and can be read between the lines. Therefore this book is especially valuable because important information is given with an introduction to up-to-date literature for creative readers. Moreover it may bring scientists in laboratories with different disciplines together. Therefore it is important to have this book in a scientific library to supply a good summary to researchers in this fascinating area from leading researchers in this field. 6190001 A F. M . Everaerts Eindhoven University of Technology The Netherlands A Practical Approach to Chiral Separations by Liquid Chromatography Edited by G.Subramanian. Pp. xvi + 406. VCH. 1994. Price DM178.00. ISBN 0-527-28288-2. This book consists of twelve chapters written by a mixture of European and North American authors. It is almost entirely concerned with high performance liquid chromatography (HPLC) though thin layer chromatography and capillary electrophoresis are mentioned. The first chapter is a brief introduction to chirality, industries in which chirality is important, the stationary phase types used in HPLC, and chiral mobile phase additives. Many aspects of this chapter are also covered in the introductions to other chapters; it nonetheless sets the scene for the forthcoming material. Chapter three is a short review of the regulatory implications of chirality focused on medicinal products.There is no mention of chiral separations in this chapter and it could perhaps have been combined with chapter one. Chapter two is concerned with molecular modelling of enantiodifferentation in liquid chromatography. This gives a necessary introduction to modelling and computational tools before reviewing the progress made in modelling Type I, I1 and 111 chiral stationary phases. The author discusses pitfalls as well as successes and the chapter is very readable even to those with little experience of molecular modelling. Chapter four is concerned with molecular imprinting and the possibility oi preparing tailor-made phases. ‘This is a worthwhile addition to the expand- ing chiral literature and the book should be of value to those working in this field.’ The larger part of the book then consists of chapters on some, but not all the different phase types.There is no chapter on theAnalyst, November 1996, Vol. 121 157N Type I phases first developed by Pirkle, for example, though they do get some mention in several other chapters. Cyclodex- trin, polysaccharide, protein, and polymer/silica composite phases are all covered in separate chapters. Mobile phase additives, ion-pair chromatography (as a separate chapter) and applications to pharmaceutical and biomedical analysis are then covered in the four subsequent chapters. As a compilation of contributions from different chapter authors, the book would have benefited from tighter editing. There is overlap between several chapters (e.g., the biological importance of chirality is covered repeatedly).There are inconsistencies in the use of English (conventional and American) and the lack of a chapter on Type I phases is an obvious omission. A chapter on preparative separations would also have been of interest as would more examples of applications outside of the drug area. Overall though, this is a worthwhile addition to the expanding chiral literature and the book should be of value to those working in this field. There are many references with each of the individual chapters and the book is well produced with plenty of helpful figures and tables. Both the contents list and the index are well prepared and helpful. Derek Stevenson 4190209B University of Surrey Special Trends in Thermal Analysis By Ferenc Paulik.Pp. xiii + 460. Wiley. 1995. Price f90.00. ISBN 0-471-95769-0. As the title implies this is not a book for the beginner. The author, and his brother Jeno, who is the silent partner in this text, are well known to thermal analysts not only in their native Hungary but throughout the world. The text comprises three sections and eighteen chapters. Part One is introductory in character and provides a well balanced history of the development of derivative thermogravimetry (DTG), simultaneous thermal methods (thermogravimetry; TG, DTG, and differential thermal analysis; DTA) and the factors affecting the result. Of particular importance is the treatment of sample size, heating rate and the development of variable mass- area crucibles.A wide range of well chosen examples emphasise the applications of the techniques. Although much of this material will be familiar to most experienced thermal analysts the content and tone of this section characterises the text as a whole and contains concepts which the author subsequently develops. Part Two deals with the kinetics and mechanism of thermal reactions. Treatment of this section is inevitably selective rather than comprehensive. In an attempt to develop a coherent framework, eight fundamental types of inorganic reactions are considered of which the treatment of dehydration and dehydrox- ylation reactions are arguably the most extensive and success- ful. The development of experimental techniques, in combina- tion with theoretical arguments, again leads into crucible design and simultaneous thermal methods.‘The price may deter all but University libraries but the book should be read by all serious workers and research students in the field. ’ Part Three is the most up-to-date and of the most interest to experienced thermal analysts. The quasi-isothermal, stop-start heating method (Q-TG), first introduced in Part One and now called Hi-Res TG, is further developed. The basis of the technique is the variation of heating rate as the rate of sample decomposition varies. The section refers to ideas and techniques introduced previously, especially in relation to sample size, heating rates, crucible geometry, etc., and develops them further. This enables the production of Q-TG/Q-DTG profiles. The interpretation of special profiles (e.g., beak-shape profiles) that improve the deconvolution of previously complicated decomposition profiles, especially in dehydration and nuclea- tion processes, and aid their understanding, are also dealt with. The section continues with other aspects of high resolution thermal analysis such as Q-DTG/Q-DTA, the combined techniques Q-TG/Q-DTG/Q-TA and thermomagnetic methods.Many examples and references, with excellent illustrations, are also provided in order to demonstrate the improved sensitivity and accuracy of the methods. The reader is left in no doubt that quasi-isothermal, and quasi-isobaric methods are the thermo-analytical methods of the future. The price may deter all but University libraries but the book should be read by all serious workers and research students in the field.E. S . 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