Data Acquisition, Analysis, and Assurance

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BOOKS

Data Acquisition, Analysis, and Assurance Statistics for Analytical Chemistry, 2nd Edition. J. C. Miller and J. N. Miller. 227 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10158. 1988. $39.95 Reviewed by Bruce R. Kowalski, Dept. of Chemistry, University of Washing­ ton, Seattle, WA 98195 This book represents another attempt to educate analytical chemists in the use of simple statistics. As the authors acknowledge in the Preface, many sim­ ilar books have been written by chem­ ists, statisticians, and chemometricians. Because this book offers no ma­ terial that is not covered by its 20 or more competitors, does it have a niche in the marketplace? I believe it does, and I recommend it as an easy-to-read overview of the topics with which every analytical chemist should be familiar. It is the type of book that could be read on a train or a plane to refresh a rusty memory or to find out which methods should be employed in the laboratory.

. the type of book that could be read to refresh a rusty memory. %% Many topics are covered in this small book (i.e., small pages with large print); hence, it might not serve as the most indepth reference on statistics. The early chapters on errors in anal­ ysis, significance testing, and quality control are well written. A good intro­ duction to these topics is provided in the first 100 pages. Chapter 6 on nonparametric methods is quite useful; it provides justification and incentive to learn and use these methods. I found Chapter 7 to be a bit disappointing, because it covers very large and useful topics such as experimental design, op­ timization, and pattern recognition in only 30 pages. Fractional factorial de­ signs and principle component analysis are only mentioned, not discussed in detail.

This book can be easily read and can heighten one's awareness of many im­ portant topics from statistics to chemometrics. Because it comes complete with a number of good exercises (no programs), I also recommend it as a textbook for a short course.

Practical Statistics for Analytical Chemists. Robert L. Anderson. 243 pp. Van Nostrand Reinhold, 115 Fifth Ave., New York, NY 10003. 1987. $39.95 Reviewed by John Mandel, National Bureau of Standards, Gaithersburg, MD 20899 This book is well written and, by and large, accurate. It presents simple problems about data and solves them by using tests of significance. A spot check indicates that the solutions are correct. It is definitely superior to many books of this type. Books of this category raise ques­ tions, however. First, although the au­ thor discusses the concept of the power of a statistical test, he dismisses it (p. 53). Once or twice, in the sequel, he alludes to the smallness of the sample size and recommends that larger ex­ periments be performed. However, most of the experiments discussed in­ volve fewer than 12 measurements. Perhaps this is intentional so the read­ er can reproduce the computations with the aid of a hand calculator, but I wonder if the data obtained in a scien­ tific laboratory are always as straight­ forward as presented in this book. A result that turns out "nonsignificant" at the 5% level is ignored. The approxi­ mation involved in Satterthwaite's for­ mula is ignored. Multiple tests of sig­ nificance are performed without regard to how this affects the level of signifi­ cance. For those who wish to answer all questions arising in the chemical lab­ oratory or plant with the simple dichot­ omy "significant" or "nonsignificant," this book provides an answer for many practical situations. Those who wish to probe a little deeper by asking ques­ tions about the data—questions that

1040 A · ANALYTICAL CHEMISTRY, VOL. 60, NO. 18, SEPTEMBER 15, 1988

are often disturbing—will require an analysis that goes beyond a simple di­ chotomy. They will require a book that presents data as they are, including their flaws, and provides an in-depth discussion of the problems raised and how they can be addressed with the aid of statistics. I noted a couple of misprints in the equations on p. 169. The first sum has la1, and the second sum lacks the term 6σ2Βο and should have 4 as a multiplier for σ 2 ΑΒ0 . Quality Assurance of Chemical Mea­ surements. John Keenan Taylor, xx + 328 pp. Lewis Publishers, 121 S. Main St., P.O. Drawer 519, Chelsea, MI 48118.1987. $59.95 Reviewed by Muhammad A. Sharaf, 366 Euclid Ave., Oakland, CA 94610 Because analytical measurements are used in the process of making critical decisions, analytical chemists must be familiar with two levels of measure­ ments. The first level involves an un­ derstanding of the components and limitations of analytical measurement systems; the second level requires the ability to assess the quality of the data being generated and the parameters being estimated. Although academic curricula often provide for the realization of the first level, exposure to the second level oc­ curs mostly on the job, or is confined to specialists. This makes it difficult for the uninitiated to get an overview of the increasingly important field of quality assurance. John Taylor's book is a welcome contribution that should fill this need. The author's 57 years of experience at the National Bureau of Standards include the development and coordina­ tion of quality assurance programs. He has also presented a short course on the subject more than 70 times. Taylor pro­ vides a readable treatment of the phi­ losophy of quality assurance and de­ scribes the elements and tools needed to assess the reliability of analytical measurements. The 26 chapters and five appendices offer a wealth of inforCIRCLE 63 ON READER SERVICE CARD •

BOOKS mation for those considering improvement and development of quality assurance and quality control programs. The first seven chapters provide an overview of the concepts and goals of quality assurance and analytical measurements and introduce some basic statistical techniques and parameters. Chapters 8-10 discuss three of the central components of the analytical measurement process: sampling, calibration, and measurement. The coverage includes the estimation of vital analytical parameters such as sensitivity, limits of detection, and sample holding time. The relationship between sam-

66... a readable treatment of the philosophy of quality assurance. · · pling and cost is also presented. Two strongly related topics, blank correction and reference materials, are covered in Chapters 13 and 17. The principles of quality assurance and quality control are given in Chapters 11 and 12; the related topic of quality assessment is treated in Chapter 15. The other chapters are devoted to the various tools and components of quality assurance and quality control, such as control charts, quality audits, validation, and laboratory evaluation. Five appendices follow, and they include a useful glossary and an excellent annotated bibliography. Unlike authors, books are sometimes imperfect. In attempting to cover a large number of topics, the author has produced a good survey of the field at the expense of depth. As would be expected in such surveys, the depth varies from one topic to the next. However, references are given to supplement the discussions. There is also an imbalance in the use of examples, and the treatment is highly qualitative at times. This is not surprising, given the scope of the book. The presentation of qualitative concepts is enhanced by appropriate illustrations. Despite its shortcomings, the book is a valuable contribution to the analytical literature. It should prove useful to analytical chemists involved in developing or monitoring analytical measurement systems. Laboratory managers and supervisors will find the material indispensable for developing, implementing, and improving quality assurance programs. CIRCLE 63 ON READER SERVICE CARD

Experimental Design: A Chemometric Approach. Stanley Deming and Steven Morgan, xiii + 285 pp. Elsevier Science Publishers, 52 Vanderbilt Ave., New York, NY 10017. 1987. $100 Reviewed by Gary W. Small, Department of Chemistry, University of Iowa, Iowa City, I A 52242 The techniques of experimental design comprise a branch of statistics often ignored by analytical chemists. Formal experimental design principles are rarely included in the chemistry curriculum, either at the undergraduate or graduate level. Moreover, many researchers fail to take advantage of these techniques when investigating the experimental factors that affect chemical analyses. Deming and Morgan should be given high praise for bringing the principles of experimental design to the level of the practicing analytical chemist. In an exceptionally lucid, easy-to-read presentation, the authors develop experimental design techniques from the basics of response surfaces to advanced techniques for multiple-factor experiments. The book is designed as a text for teaching experimental design principles, either in a formalized course or in an independent study environment. As such, the book must be read from start to finish. Each chapter builds upon preceding material, and the text often refers to previous discussions. A major goal of the work is to allow chemists with limited statistical expertise to master the principles of experimental design. In this regard, chapters are included on basic statistics, model building, and hypothesis testing. Many examples are worked and discussed in the text. In addition, each chapter is accompanied by numerous exercises. An appendix summarizes the rudiments of matrix algebra necessary for performing the matrix least-squares operations that are common throughout the last half of the book. Students at the advanced undergraduate or beginning graduate level should be able to use the book effectively. I can envision the text being made part of an undergraduate instrumental analysis laboratory course or a graduate course on chemical data analysis techniques. In both cases, however, a second text would have to be used to cover the additional topics (e.g., error propagation) that are commonly included in such courses. In the selection of topics, the authors make no attempt to produce a reference work detailing every available ex-

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ANALYTICAL CHEMISTRY, VOL. 60, NO. 18, SEPTEMBER 15, 1988 · 1041 A

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perimental design technique. Thus the book does not replace advanced statis­ tics texts on experimental design. By reading this work, however, the prac­ ticing chemist will be well prepared to explore any of the more advanced texts on the subject. The book has many strengths. The authors realize that an understanding of model building and the set of de­ scriptive statistics resulting from mod­ el building is crucial to the correct use of experimental design strategies. These sections of the book are very well written. Moreover, their discussion of the principles of analysis of variance (ANOVA) is especially easy to under­ stand. In this discussion, traditional ANOVA tables are reconfigured into a very understandable tree-like presen­ tation. The book is well edited, and the presentation is organized in an attrac­ tive and effective manner. My criticisms of the book center on several omissions and on several points of emphasis. Because the book was de­ signed to be read in its entirety, an in­ troductory motivational chapter would have been helpful. Examples could have been discussed in which experi­ mental design techniques have proven especially helpful. Similarly, a conclud­ ing chapter summarizing the main points of the book would have been useful. An effective approach to this

The authors make the techniques of experimental design understandable. %%

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chapter would have been the develop­ ment of a set of practical rules or guide­ lines a researcher might use in devising an experimental design. A section on the design of response functions also would have been useful. In many cases, no direct measured signal is available to use as a response. For example, in a study of factors affecting a chromato­ graphic separation, a scheme must be devised to reduce each chromatogram to a single numerical response that characterizes the separation. The importance of replicating ex­ periments across the design should have been stressed to a greater extent. Nonconstant variance is an important problem in many analytical proce­ dures. It may be misleading to re­ searchers to recommend techniques in which only a small number of design points are replicated. I would also have

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1042 A · ANALYTICAL CHEMISTRY, VOL. 60, NO. 18, SEPTEMBER 15, 1988

liked increased emphasis on the use of residual plots as model diagnostics. This topic is mentioned briefly in one of the exercises, but it is not given suffi­ cient treatment. The next edition of the work would benefit from a companion set of com­ puter software that a chemist could use to implement the topics discussed in the text. Additionally, expanding the last chapter to include a more thorough discussion of blocking techniques would be appreciated. The authors have performed a valu­ able service to chemists by making the techniques of experimental design understandable. The book would be an excellent addition to the collection of every analytical chemist. I recommend it with great enthusiasm.

Books Received Mass Spectrometry in Biotechnological Process Analysis and Control. Elmar Heinzle and Matthias Reuss, Eds. xi + 241 pp. Plenum Press, 233 Spring St., New York, NY 10013.1987. $59.50 This 18-chapter book is based on an International Federation of Automatic Control (IFAC) workshop held in Graz, Austria, in 1986. The book is divided into four major sections: instrumenta­ tion and gas analysis, membrane inlet systems, applications and computer control, and pyrolysis MS and HPLC MS interfacing. References include material from 1987. Round-table dis­ cussions, as well as a five-page index, are included. Laboratory Information Management Systems: Concepts, Integration, and Implementation. R. D. McDowall, E d . xvi + 383 pp. John Wiley & Sons, 605 T h i r d Ave., New York, N Y 10158.1987. $59.95

This 26-chapter book is divided into five sections: concepts, essentials of computing, implementation and choices, validation, and the future. References include material from 1987. A 12-page glossary and a seven-page index are included. Laser Raman Spectrometry: Analytical Applications. Halina Baranska, Anna Labudzinska, and Jacek Terpinski. 271 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10158.1987. $64.95 This nine-chapter book was translated from Polish. The references cover ma­ terial up to and including 1984. Specif­ ic chapter topics include elements of group theory, identification of organic

BOOKS and inorganic compounds, and fundamental concepts in spectroscopy. An eight-page index is included.

two-page bibliography and a six-page index are included. The most recent bibliography entry is from 1986.

Electrochemical Sensors in Immunological Analysis. T. T. Ngo, Ed. xi + 360 pp. Plenum Press, 233 Spring St., New York, NY 10013. 1987. $62.50

High-Resolution Solid-State NMR of Silicates and Zeolites. G. Engelhardt and D. Michel, xiv + 485 pp. John Wiley & Sons, 605 Third Ave., New York, NY 10158. 1987. $117

This 25-chapter book includes references through 1986. The contents include separation-free enzyme-mediated immunoassays with electrochemical detection, liposome-mediated electrochemical immunoassays, applications of ion-selective membrane electrodes in immunoassays, and the combined use of a flow system and an electrochemical detector to monitor the immunochemical reaction. There is a sixpage subject index. Managing Safety in the Chemical Laboratory. James P. Dux and Robert F. Stalzer. viii + 154 pp. Van Nostrand Reinhold, 115 Fifth Ave., New York, NY 10003. 1988. $28.95 This 10-chapter book covers topics such as organizing for safety, preparing for emergencies, protecting personnel, and managing personnel for safety. A

Although the basic principles and methods of high-resolution solid-state NMR are presented in this volume, the emphasis is on applications. References are extensive and include material published in 1986. A seven-page index is included. Quantitative Analysis by Gas Chromatography, 2nd ed. Josef Novak, xi + 277 pp. Marcel Dekker, 270 Madison Avenue, New York, NY 10016.1988. $89.75 The scope of the second edition has been extended by the addition of a new chapter on automated processing of chromatographic data by Piet Leclercq. The volume was translated from Czech. Of the 178 references, nine are from the 1980s; the most recent is from 1986. There is a list of symbols and a seven-page subject index.

Analytical Isotachophoresis. P. Bocek, M. Demi, P. Gebauer, and V. Dolnik. xviii + 237 pp. VCH Publishers, Suite 909, 220 East 23rd St., New York, NY 10010-4606. 1988. $110 This 11-chapter book, the first in the "Electrophoresis Library" series published by VCH, was translated from Czech. References include material from 1987. A five-page index also is provided. Advances in Standards and Methodology in Spectrophotometry. C. Burgess and K. D. Mielenz, Eds. 403 pp. Elsevier Science Publishing, P.O. Box 1663, Grand Central Station, New York, NY 10163.1987. $95 Field-Flow Fractionation. Josef Janca. vi + 336 pp. Marcel Dekker, 270 Madison Ave., New York, NY 10016. 1987. $99.75 Wilson and Wilson's Comprehensive Analytical Chemistry. Vol. 21: New Developments in Conductimetric and Oscillometric Analysis. O. Klug and B. A. Lopatin. xv + 313 pp. Elsevier Science Publishers, 52 Vanderbilt Ave., New York, NY 10017.1988. $131.50

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