An Overview of the State of the Art - Analytical Chemistry (ACS

May 29, 2012 - An Overview of the State of the Art. Anal. Chem. , 1982, 54 (7), pp 839A–844A. DOI: 10.1021/ac00244a768. Publication Date: June 1982...
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An Overview of the State of the Art Chemical Derivatization in Analytical Chemistry. Vol. I. R. W. Frei, J. F. Lawrence, Eds. xi + 344 pp. Plenum Press, 227 West 17th St., New York, N.Y. 10011. 1981. $39.50

Reviewed by Norman Parris, Photo Products Department, E.I. Du Pont de Nemours & Co., Inc., Wilmington, Del. 19898 In the area of chemical derivatization, the editors of this book require no introduction. They have both long enjoyed the position of being foremost in the field, having developed many novel concepts and published very widely indeed. In 1979 Lawrence and Frei were the authors of a text entitled "Chemical Derivatization in Liquid Chromatography," and on the basis of titles one might easily draw the conclusion that the two texts are very similar. This conclusion would be a serious error; the two texts are quite distinct and each stands on its own merits. This book is divided into four chapters which, in fact, cover totally different aspects of the subject. These relate to derivatization in the gas chromatography of pesticides, the use of cyclic boronates in GC/MS. The latter two chapters are devoted to postcolumn derivatization (reaction detector) as applied to high-performance liquid chromatography. Each chapter is written by a different author and consequently the format and style vary markedly from chapter to chapter. The second chapter (cyclic boronate derivatives for GC/MS) gives clear experimental details on how to prepare derivatives and illustrates typical results through a series of well-selected examples. Adequate references are cited for those requiring further information. Overall the format is easy to follow, which in turn stimulates the reader to think of other similar areas of applicability. In the opinion of the reviewer, this is considerably more helpful than the format used for the first chapter, in which the author attempts to cram in as many references and examples as possible by citing nu-

merous references. Unfortunately, this approach creates a somewhat staccato style, making assimilation of the general approach, theoretical background, and experimental procedures less effective. In contrasting the styles of the first two chapters, it is interesting to note that the number of references per page of text is higher in chapter 2; however, their presence was far less obtrusive to the flow of the chapter. Chapter 3 (precolumn derivatization) is probably the best written in that after a short description of the purpose and equipment requirements, it systematically describes application of precolumn derivatization to different clinical types, based on chemical functionality—thus making it useful for the researcher who is seeking a way to derivatize a "unique" substance. The theoretical aspects and reaction mechanisms and kinetics are very clearly described. The choice of examples, showing procedures for enhancing adsorption and fluorescent properties as well as resolving enantiometers, are particularly effective. Chapter 4 reviews many of the reported approaches to the use of fast column reactions to enhance sample detection. Since many workers utilize custom-made apparatus, the chapter describes many of the devices and operating procedures along with the example described. This information will be particularly helpful for those who wish to set up their own operating systems. Overall the book provides stimulating reading and a good overview of the present state of the art. As such it would prove of considerable interest to those active in research or development of chromatographic methods. Rock and Mineral Analysis. 2nd ed. Wesley Johnson, J. A. Maxwell, xi + 489 pp. John Wiley & Sons, Inc., 605 3rd Ave., New York, N.Y. 10016. 1981. $52.50

Reviewed by Michael Reddy, U.S. Geological Survey, WRD, 5293 Ward Rd.,Arvada, Colo. 80002

This monograph examines elemental analysis of geologic materials and serves as a timely treatment of rock and mineral analysis and associated problems. The authors emphasize commonly used analytical methodologies and instrumental techniques. In keeping with a practical approach to the subject, instrumental theory is not presented. Several initial chapters are devoted to a description of laboratory set-up, equipment and method selection, sampling, sample preparation, and sample decomposition. The rationale underlying common sampling strategies is well presented. A helpful segment in the chapter on sampling is inclusion of a quantitative discussion of recent advances in sampling control. This material will be of particular interest to those involved in environmental sampling and analysis. Decomposition techniques are presented with sufficient detail to allow appropriate choice of analytical methodologies for most natural samples. A careful discussion of potential analyte loss during decomposition is quite useful. Numerous routine procedures, developed in laboratories associated with the authors, can be used as presented. Chapter 9 includes a summary of fractional extraction techniques, which are widely used in environmental and soils analysis. The authors have prepared a wellwritten and well-organized monograph, produced with attention to detail and accuracy. Line drawings and halftone illustrations are, for the most part, well-executed and informative. However, several tables produced by photographic reduction of typed text are not as legible as the majority of tables and illustrations. Inclusion of more than 60 pages of reprinted material, some typeset in an awkward fashion, seems out of place. Although the authors include a discussion of recent advances in analytical techniques that improve efficiency and reliability, other recent developments, such as Auto-Analyzer methods, ion chromatography procedures, and techniques

ANALYTICAL CHEMISTRY, VOL. 54, NO. 7, JUNE 1982 · 839 A

Books for the detailed characterization of the organic components of geologic mate­ rials are not discussed. In the section dealing with carbon determination, the absence of automated elemental analysis is a notable omission. The discussion of high blank values on ρ 285 is confusing. The monograph will be useful as a laboratory procedures reference to those analysts involved in sampling and elemental analysis of geologic ma­ terials including rocks, minerals, soils, and sediments. Comparisons of Fused Silica and Other Glass Columns in Gas Chromatogra­ phy. Walter Jennings, vii + 80 pp. Dr. Alfred Huethig GMBH, Postfach, 102869, 6900 Heidelberg I., FRG. 1981. $19

Reviewed by Milton Lee, Department of Chemistry, Brigham Young Uni­ versity, Provo, Utah 84602 The rapid increase in the use of cap­ illary columns in gas chromatography can be attributed mainly to the devel­ opment of flexible fused silica col­ umns. Until nearly three years ago, glass was the preferred material from

which capillary columns were fabricat­ ed. Although glass is considered to be fairly inert, much research has been done during the last 20 years to physi­ cally and chemically modify the sur­ face for improved chromatographic performance at trace analyte levels. The advent of the fused silica capil­ lary column stimulated much early re­ sistance and controversy over the ad­ vantages and disadvantages of this material. It appears that the purpose of this monograph was to evaluate and compare both glass and fused silica capillary columns for gas chromatog­ raphy. The subject matter is written at a level and style easily readable by anyone concerned with chemical anal­ ysis and is useful as a basic introduc­ tion to column technology in capillary column gas chromatography. This short monograph has a number of desirable features. The chapter on column evaluation is particularly use­ ful. It is one of the best-condensed treatments of this topic available and provides a clear picture of the impor­ tant aspects of column testing. The chapters on materials of construction and pretreatment of the capillary col­

umn are also good reviews of silica surface chemistry as applied to capil­ lary column preparation. The deficiencies in the monograph lie in several areas. The major criti­ cism is that although the book title implies a comparison of fused silica and glass, there is very little specific information about fused silica itself. The book is principally a review of * glass capillary column technology. The introduction and applications chapters are very brief and sketchy and are not particularly informative for those already practicing capillary gas chromatography. I found the chapter on cost comparisons some­ what inappropriate since many factors are involved in the proper assessment of production costs, and these vari­ ables can change drastically from sit­ uation to situation. Furthermore, one feels like one is reading an advertise­ ment for a product. Although the bib­ liography is quite extensive, several key references from which much of the material in the book was taken were omitted. In conclusion, the reviewer would recommend this monograph to new-

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Books comers to the field of capillary column gas chromatography, or to those inter­ ested in a general treatment of capil­ lary column technology. Basic Analytical Chemistry. L. Pataki, E. Zapp. xiii + 463 pp. Pergamon Press, Inc., Maxwell House, Fairview Park, Elmsford, N.Y. 10523. 1980. $25

Reviewed by Gary Christian, Depart­ ment of Chemistry, University of Washington, Seattle, Wash. 98195 This book has been translated from Hungarian into English by Gy. Jalsovsky. The authors have attempted to cover basically all areas of analytical chemistry in one reasonably sized vol­ ume, and they have done a remarkable job in at least touching upon most classical and modern analytical tech­ niques. There are six chapters: chemi­ cal equilibria in solution (77 pp), qual­ itative chemical analysis (90 pp), quantitative chemical analysis (128 pp), instrumental methods of analysis (89 pp), separation methods (28 pp), and analysis of organic compounds (elemental analysis, functional group analysis—26 pp).

Chapter 1 introduces several acidbase theories and describes simulta­ neous and multiple equilibria, redox potentials, and partition equilibria. The Bronsted-Lpwry theory is em­ phasized and is used in chapter 3 to present a unified view of the various fields of quantitative analysis. Chap­ ter 2 describes several inorganic quali­ tative group separations, but fails to present a unified separation scheme for the student. The use of organic re­ agents for qualitative identification is a useful addition. Chapter 3 contains an excellent discussion of the theory of solubility and particle formation, which is suited for the more advanced student. The term "radical weight" on ρ 190 for calculating the gravimetric factor is not clearly defined, and no example calculations are given. Like­ wise, use of the "titration factor" and its relationship to normality in volu­ metric calculations is not amply clari­ fied. There is a very good discussion of indicator theory, including factors that can affect the color change, as well as the limitations of redox reac­ tions in titrimetry and how to improve them.

The precision and attention to de­ tail in the earlier chapters are not as evident in the instrumental analysis chapter. Most necessary subjects that the student should know are men­ tioned, but frequently without expla­ nation. In the discussion of voltammetry, for example, it is pointed out that a high concentration of electrochemically inactive ions suppresses the mi­ gration current but it does not explain why. The residual current is men­ tioned, but nothing is said of what contributes to it nor that it limits the sensitivity. The condensor current is mentioned in a discussion of pulse polarography, but again without an ex­ planation of what it is. In discussing atomic absorption, it is pointed out that use of a graphite furnace results in increased sensitivity but with no in­ dication of why. A number of terms are left undefined. Thus, the instru­ mental section has a good deal of qual­ itative description, necessitated prob­ ably by the brevity needed to cover so many topics. Other instrumental subjects covered include electrogravimetry, coulometry, potentiometry, conductometry, polarimetry, refrac-

Mettler thermal analysis: Easy and affordable. Mettler TA3000 provides you with a micropro­ cessor-controlled, highly compact, simple-touse system for DSC, TG and TMA measurements. At very affordable prices—for instance, only $24,000 for a complete DSC systems. Self cali­ brating. Links and stores temperature programs and evaluation methods (up to 23). Plots thermo­ grams (scaled automatically or manually) and prints evaluated numerical results. For further information, contact Mettler, Box 71, Hightstown, NJ 08520, (609) 448-3000.

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tometry, emission spectroscopy, X-ray methods, absorption spectroscopy, fluorescence and light scatter meth­ ods, thermal methods, and radiochem­ ical methods. Magnetic susceptibility, NMR, ESR, and mass spectrometry are covered in three pages. The main drawback of this book as a text is that it contains practically no example calculations (I counted only four very elementary examples on pp 259 and 267-268). Very precise equa­ tions are given throughout, but these are difficult to teach from with no practical examples and would tend to overwhelm the student. There is no emphasis on dimensional analysis. An­ other drawback is t h a t there are no homework problems. This book contains a great deal of useful information, but I classify it more as a reference or supplemental book than a textbook.

Books Received Analysis of Complex Hydrocarbon Mixtures. Vol. 13. Pt. A. Slavoj Hala, Mecislav Kuras, Milan Popl. χ + 382 pp. Elsevier North-Holland, Inc., 52 Vanderbilt Ave., New York, N.Y. 10017. 1981. $95.75 Analysis of Complex Hydrocarbon Mixtures. Vol. 13, Pt. B. Slavoj Hala, Mecislav Kuras, Milan Popl. 458 pp. El­ sevier North-Holland, Inc., 52 Vanderbilt Ave., New York, N.Y. 10017. 1981. $95.75 Proceedings of the Fourth International Symposium on Capillary Chromatogra­ phy Held in Hindelang/Allgau, Germa­ ny, May 3 - 7 , 1981. R.E. Kaiser, Ed. 939 pp. Alfred Huthig Publishers, 611 Broadway, New York, N.Y. 10012. 1981. $39.50 Electroanalytical Chemistry. Vol. 12. Allen Bard, Ed. xi + 251 pp. Marcel Dekker Inc., 270 Madison Ave., New York, N.Y. 10016. 1982. $47.50 Short-Term Bioassays in Analysis of Complex Environmental Mixtures II. Michael Waters, et al. xv + 524 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1981. $59.50 Thermal Analysis in Polymer Charac­ terization. Edith Turi, Ed. viii + 159 pp. Heyden & Sons Inc., 247 South 41st St., Philadelphia, Pa. 19104. 1981. $33

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Introduction to FORTH. Ken Knecht. 142 pp. Howard W. Sams & Co., 4300 West 62nd St., Indianapolis, Ind. 46268. 1982. $9.95