Books
Useful Text for the Beginning Electroanalyst
Laboratory Techniques in Electroanalytical Chemistry. Peter Kissinger, William Heineman, Eds. xv + 751 pp. Marcel Dekker, 270 Madison Ave., New York, N.Y. 10016. 1984. $34.75
Reviewed by Fred Anson, California Institute of Technology, Division of Chemistry and Chemical Engineering, Room 127-720, Pasadena, Calif. 91125 Editors Kissinger and Heineman and the illustrious group of authors they have assembled have made a major contribution to electroanalytical chemistry with the appearance of this volume. The two editors also serve as authors or coauthors for 8 of the 24 chapters, which are admirably consistent in the style and level of the presentations. Some of the editors' intentions for their collection, as stated in the preface, do a good job of conveying the flavor of the book: " . . . this book was conceived in 1970 . . . to provide a means of enabling a neophyte . . . to get started in the lab. During the decade over which this effort has spanned the emphasis . . . expanded to include a pedagogical component." "The emphasis of this book is entirely on analytical and mechanistic (homogeneous), kinetic (homogeneous), and synthetic (laboratory scale) applications." "The organization of the book flows from principles through methodology to applications." This book differs from most of its predecessors in studiously and unapologetically eschewing mathematical derivations as much as possible. In their place one is offered clear, carefully considered qualitative descriptions of the physical situations that are the cause and the result of the passage of current through electrochemical cells. The treatment is both appealing and stimulating. The more rigorous mathematical treatments available in the well-known books by Delahay and Bard and Faulkner may well receive added appreciation and
understanding from readers who have been guided in their direction after being introduced to the topics in the informative and seductive forms employed in this book. I concur with the editors' opinion "that Chapters 2 through 5 are suitable for use in graduate-level introductory courses in electroanalytical chemistry." (Indeed, several other chapters, e.g., 6,16, and 12, could also serve this purpose admirably.) Chapters 2-5, written by the editors (and their associates in one case), treat the fundamental concepts underlying essentially all dynamic electroanalytical techniques with pedagogic insights and an arresting style uncommon to most previous monographs on electroanalytical chemistry. For example, a derivation of Fick's second law of diffusion is followed by these sentences: "The solution of diffusion equations has fascinated academic electroanalytical chemists for years and they naturally have a tendency to expound upon them at the slightest provocation. Fortunately the chemist using electrode reactions can accomplish a great deal without more than a cursory appreciation of the mathematics." The succeeding chapters in the collection amply support this contention. The topics treated cover virtually everything a beginning researcher needs to know to undertake laboratory work in electroanalysis: analog instrumentation; the virtues and limitations of electrodes made of mercury, carbon, or films; electrochemical cells and solvents; and useful techniques involving vacuum lines, controlled atmospheres, electron spin resonance, photochemistry, conductance, and digital simulation. Illustrative examples are used in discussions of organic electrode reaction mechanisms, transition metal electrochemistry, analysis of pharmaceuticals, applications of electrochemical detectors to chromatography, electrochemical preconcentration, and constant-current coulometry. I have already found this book high-
ly useful in assisting students and colleagues in trying out an unfamiliar electrochemical technique because the descriptions provided are both clear and encouraging. The book deserves the popularity with which it will undoubtedly be received. My advice to fellow electrochemists is to buy two copies—one to keep for handy reference and a second to lend to the army of friends and colleagues who are apt to descend upon us in search of the answers that they've heard the book can provide. Small Bore Liquid Chromatography Columns: Their Properties and Uses. Raymond P.W. Scott, Ed. xiii + 271 pp. John Wiley & Sons, 605 Third Ave., New York, N.Y. 10016. 1984. $48.50
Reviewed by Richard Hartwick, Department of Chemistry, Rutgers University, New Brunswick, N.J. 08903 "Small Bore Liquid Chromatography Columns" is a timely addition to the Chemical Analysis Series, edited by one of the founders of the field of
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Books "microbore" HPLC. As stated by Scott in the preface, the term microbore has probably been rendered obso lete by advancing technology. He sug gests instead that "small bore" col umns be used as the generic appella tion of columns in the range of 1-2-mm i.d. There is still no general consensus on the nomenclature of HPLC using columns smaller than the current standard of 3-5-mm i.d. Scott's suggestion is probably a good one, except that the term microbore in connection with 1-mm-i.d. columns is already so well established in the lit erature that a change at this late date is probably ill-advised. Besides, small bore is still a comparative, rather than an absolute, term and may in several years represent "conventional" or even "semipreparative" LC, depend ing on how far the trend toward min iaturization continues. The book sets out with a deliberate bias in that it deals almost exclusively with 1-2-mm-i.d. column technology, as implied by the title. The extensive literature on packed fused-silica col umns of several hundred micrometers i.d. is not addressed. This is not neces sarily a weakness, because the book gains a certain strength from limiting its focus to one specific column type. However, this is mentioned for the sake of the reader who might expect a comprehensive treatise on all aspects of microbore column technology. The book consists of 11 chapters, with the first six focusing on the the ory and instrumentation of small-bore columns, whereas Chapters 7-11 re view particular applications of these columns. In general, the information contained in the chapters is useful to the practicing chromatographer. The first four chapters, dealing with band dispersion and instrumentation, re view basic chromatographic equations, expressed in terms of small-bore LC. The theoretical treatment suffers from being spread over several chap ters by three different authors; howev er, the equations are unified in their nomenclature. A more comprehensive treatment by a single author of all the instrumental theory covered could have strengthened this aspect of the work. In fairness, however, such cohesiveness is virtually impossible to sus tain in any multiauthored volume. Some sections, such as that on serpen tine tubing, assemble in one place a variety of useful equations normally scattered about the literature. The chapters on applications do a good job of covering 1-mm-i.d. column technology. Some of the more exciting work in narrow-bore instrumentation, such as laser-based detectors, is not
CIRCLE 2 ON READER SERVICE CARD 584 A · ANALYTICAL CHEMISTRY, VOL. 57, NO. 4, APRIL 1985
adequately covered, since much of this is being done with packed fused-silica columns. Also, the field of LC/MS, which seems destined to become one of the primary driving forces for the trend toward micro-LC, is only super ficially mentioned. A full chapter de voted to this topic could have added depth to the volume. A strength of the book is the com prehensive manner in which all major aspects of chromatography with 1-mm-i.d. columns are covered. A chromatographer needing to do work with this type of instrumentation could successfully begin work in this area using only this book as a guide. Thus, the book should be useful for those chromatographers who are con templating starting up a 1-mm-i.d. in strument in their own labs. In summary, this volume should be a useful addition to the library of the chemist needing a handy reference to the literature and use of 1-2-mm-i.d. columns. As with any rapidly advanc ing field, some material is undoubted ly dated, but this does not detract from the utility of the book as a basic work. Overall, the editor and the con tributors effectively present the ad vantages and limitations of small-bore columns and the role they play in the development of HPLC separations. Regulatory Compliance Monitoring by Atomic Absorption Spectroscopy. Sid ney Katz, Stephen Jenniss. vii + 278 pp. Verlag Chemie International, 303 N.W. 12th Ave., Deerfield Beach, Fla. 33441. 1983. $37.50 Reviewed by Theodore Martin, U.S. Environmental Protection Agency, Environmental Monitoring and Sup port Laboratory, Cincinnati, Ohio 45268 This book is a descriptive collection of various atomic absorption method ologies used for the analysis of envi ronmental samples. The majority of the methods included are analytical procedures used for compliance moni toring. The text, which consists of eight chapters, is introduced by a gen eral discussion on some practical as pects of atomic absorption analyses and concludes with a suitable discus sion on the needs and requirements of a laboratory quality assurance pro gram. Two chapters are specifically devoted to sampling, sample preserva tion, and preparation procedures, whereas the remaining four chapters address the analytical requirements of the monitoring methods for air, water, solid-type samples, and tissue analy ses. (continued on p. 587A)
Environmental Sampling for Hazardous Wastes
Hi»·1· G l e n n E. S c h w e i t z e r a n d J o h n A . S a n t o l u c i t o , Editors U.S. Environmental Protection Agency Underlines the concern and need for improved methods of environmental sampling. Surveys the problems of collecting representative samples, ensuring the chemical integrity of samples from collection to analyses, and characterizing and monitoring contamination sites. Examines the important aspects of designing and implementing sampling programs, emphasizing surface and subsurface sampling for hazardous wastes. Looks into the experiences of federal and state agencies, and academic and institutional organizations. Cites several successful field programs for sampling dioxin, lead, and cyanide. CONTENTS Hazardous Waste: Questions and Issues from the Field · Uses of Environmental Testing in Human Health Risk Assessment · Assessing Cyanide Contamination from an Aluminum Smelter · 2,3,7,8-Tetrachlorodibenzo-p-dioxin Sampling Methods · Field Measurement of Polychlorinated Biphenyls in Soil and Sediment Using a Portable Gas Chromatograph · Using Geostatistics in Assessing Lead Contamination near Smelters · Lead Levels in Blood of Children Around Smelter Sites in Dallas · An Approach to Interdisciplinary Design of Multifactor Experiments · Statistical Methods in Environmental Sampling · Soil Sampling Quality Assurance and the Importance of an Exploratory Study · Quality Assurance for Measurement Program · New Ways of Assessing Spatial Distributions of Pollutants · Detecting Elevated Contamination by Comparison with Background Based on a workshop sponsored by the ACS Committee on Environmental Improvement, the U.S. Environmental Protection Agency, and the University of Nevada—Las Vegas ACS Symposium Series No. 267 144 pages (1984) Clothbound LC 84-20480 ISBN 0-8412-0884-0 US & Canada $34.95 Export $41.95 Order from: American Chemical Society Distribution Office Dept. 18 1155 Sixteenth St., N.W. Washington, DC 20036 or CALL TOLL FREE 800-424-6747 and use your VISA, MasterCard, or American Express credit card.
Books The methods included are not limited to those published by the U.S. Environmental Protection Agency (EPA) and the National Institute for Occupational Safety and Health; methods from foreign governments, in particular the Canadian Department of the Environment, with references to work by professional scientific societies and other researchers, also have been included. The authors do not present a critical review of the methods, but list similar methods for each analyte for a comparative review by the reader. An important feature of the book is the interspersing of appropriate comments and references to related research work throughout the text. The book is intended to be an aid to analysts in presenting the required details of official methodology with a brief statement on the purposes of regulatory compliance monitoring. The book is easy to read and for the most part accomplishes its goal. As with all texts a few typographical errors do appear as in the table on regulatory limits (p. 4), where the drinking water maximum contaminant level concentrations for cadmium and selenium are incorrect, and chromium is listed as a hexavalent measurement. Also, important sentences from the introduction to the EPA chelation extraction procedure (p. 65) as well as reagent preparation steps have been omitted, which significantly affects the reader's ability to understand the procedure. Overall the book is useful and should be considered a resource. However, the reader should not substitute its use for original referenced material from which the methods have been extracted. The reader must also be aware that periodic updating of approved methodology and regulatory changes may date some information in the text. The Federal Register should be consulted for appropriate changes as they develop.
Books Received
TKOMHïCA·- N O l f i S e
How to select LC filters to maximize resolution. A column inlet filter is usually necessary to capture contaminating particles, yet this filter may easily impair resolution if not wisely selected. Rheodyne's Tech Note 6 reports experiments measuring how much filters of various sizes and flow geometry affect the resolution achieved by columns of several sizes. The'newer microbore columns and short 4.6-mm columns prove to be most sensitive to filter performance. If their resolution is to be preserved, an inlet filter with very little sample dispersion must be used. The Tech Note helps the reader select the optimum filter for his application: one with little enough sample dispersion to preserve resolution, yet large enough capacity to prevent a rapid rise in backpressure.
Send for Tech Note #6 For a copy free of charge contact Rheodyne, Inc., PO. Box 996, Cotati, California 94928, U.S.A. Phone (707) 664-9050.
T h e Analysis of Plastics. T.R. C r o m p t o n . ix + 4 4 5 p p . P e r g a m o n Press, M a x w e l l H o u s e , F a i r v i e w Park, E l m s f o r d , N.Y. 1 0 0 2 3 . 1 9 8 4 . $ 4 9 . 5 0 Official Methods of Analysis of t h e A s sociation of Official Analytical C h e m ists. 1 4 t h e d . S i d n e y W i l l i a m s , E d . 1141 pp. Association of Official Analytical C h e m i s t s , 1 1 1 1 North 19th St., Suite 2 1 0 , Arlington, V a . 2 2 2 0 9 . 1984. $ 1 3 3 . 9 5 (U.S. m e m b e r s ) ; $ 1 4 8 . 5 0 ( U . S . nonmembers)
RHEODYNE THE LC CONNECTION COMPANY CIRCLE 177 ON READER SERVICE CARD
ANALYTICAL CHEMISTRY, VOL. 57, NO. 4, APRIL 1985 · 587 A
