An Instrumental Analysis Text Updated - Analytical Chemistry (ACS

May 25, 2012 - An Instrumental Analysis Text Updated. Anal. Chem. , 1981, 53 (8), pp 999A–1002A. DOI: 10.1021/ac00231a788. Publication Date: July 19...
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An Instrumental Analysis Text Updated Principles of Instrumental Analysis. 2nd ed. Douglas A. Skoog and Donald M. West, xi + 769 pages. Saunders College/Holt, Rinehart & Winston, 383 Madison Ave., New York, N.Y. 10017. 1980. $21.95

Reviewed by J. D. Ingle, Jr., Department of Chemistry, Oregon State University, Corvallis, Ore. 97331 This new edition of a well-known instrumental analysis textbook provides up-to-date coverage of a field that is always expanding. Thé coverage is generally similar to the first edition but with some reorganization and consolidation. The most notable new topics covered include electronics, ICP emission, electrothermal atomizers, thermal methods, and HPLC. There is enough material for a two-quarter course; the level of coverage is adequate for an upper division undergraduate course but not for a graduate course. The authors are to be commended for covering a very wide variety of topics at approximately the same level of detail and for their lucid writing style. Many concepts that students have difficulty with are clearly explained with many excellent figures, tables, and problems. Also many good references are given. I found very few typographical errors or incorrect equations— The addition of about 70 pages on electronics was sorely needed. The detail on ac electronics (e.g., LC circuits) is probably unnecessary for the undergraduate level, while the detail on digital electronics is inadequate. A good introductory section on noise sources is also included. The spectroscopy chapters are generally well organized with a couple of good introductory chapters tying together general principles and types of components. The sections oh ICP emission and electrothermal atomizations are too short relative to their established importance and use in modern analysis. The coverage of precision in molecular absorption measurements is the most complete I've seen

in a textbook, but unfortunately does not carry over to the rather antiquated techniques of differential absorption or to AA measurements. Important topics omitted include holographic gratings and the inner filter (preabsorption) effects in fluorescence spectrometry. Most electrochemical techniques are covered well, although the space devoted to anodic stripping voltammetry is not commensurate to its current importance. There is essentially no discussion of various types of carbon or graphite electrodes that are now greatly used, and it is stated incorrectly that most solid electrodes used for voltammetry are based upon the rotating platinum electrode. In some cases, all the assumptions necessary to use certain equations are not stated. The section on HPLC is a useful addition but could be expanded. In a fast-moving field like HPLC, a table of detector sensitivities from a 1964 reference does not reflect the current state of the art. It is incorrectly stated that silica gel is the most widely used absorbent in HPLC when in fact 90% of all separations are accomplished with bonded reverse phase packings. Examples of gradient elution with reverse phase packing should be included. There are a number of confusing or incorrect statements, a few of which are cited below. Reflective losses experienced by a light beam going through a sample cell are multiplicative and not additive (p 104). The diffraction or aberration limit of a monochromator should be mentioned so the student doesn't think one can reduce the slit forever and continue to improve resolution. Usually absorption filters have greater peak transmission than interference filters, contrary to what is stated (p 136). There is not always, as is stated, a linear relationship between absorbance and path length (p 153) since factors such as stray light will cause nonlinearity if A is large because of a large c or b. Johnson noise is often

important with phototube detectors (p 159). In Figure 6-7, Caption B, Johnson noise should be replaced by dark current noise. Figure 10-2 is misleading because the ratio of the sample and reference signals, not the difference, must be used to correct for source fluctuations, and normally one would riot attenuate the reference beam as this would cause S/N problems. In corrected fluorescence excitation spectra (p 290), one must also correct for the variation of monochromator transmission efficiency with wavelength. The effect of high pulse rates in photon counting (p 439) is not described adequately in terms of missing counts due to pulse pileup. The discussion of counters and scalers for X-ray methods (p 443) is outdated since high-speed electronic counters have replaced slow electromechanical counters. The standard deviation is equal to the square root of number of counts (p 462) for a Poisson, not the Gaussian distribution, although for large Ν the Gaussian distribution is a good approximation for the Poisson distribution. Potentiometric titrations (p 559) are not more time-consuming than titrations with indicators, partic­ ularly with automated instruments. Equation 19-12 does not follow from Equation 19-11. Many quoted prices for instruments are low by a factor of 2 or 3. The van Deemter equation (p 674) and Figure 26-6 as in most textbooks is incorrect because the A term is zero. This historical blunder should be cor­ rected since the equation for the A term applies only under conditions of turbulent flow, which do not exist in chromatography. It should also be pointed out that the constant C in the nonequilibrium mass transfer term is somewhat velocity dependent. Overall this is an excellent text­ book, which I am presently using. The . relatively few mistakes can be pointed out to students, and the areas in which the book is weak can be easily correct­ ed with a relatively small amount of supplementary material.

ANALYTICAL CHEMISTRY, VOL. 53, NO. 8, JULY 1981 • 999 A

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Corrosion Chemistry ACS Symposium Series No. 89 George R. Brubaker, Editor Illinois Institute of Technology P. Beverley P. Phipps, Editor IBM Corporation Based on a lecture series cosponsored by the Chicago sections of the American Chemical Society and the Electrochemical Society.

Physical chemists and chemical en­ gineers, as well as corrosion specialists will find pertinent informa­ tion on the latest developments in the field. CONTENTS Corrosion · Electrochemical Techniques in Corrosion Studies · High-Temperature Corrosion · Ionic and Electronic Conduction in Nonmetallic Phases · Disso­ lution of Iron · Ferrous Passivation · Corrosion of Valve Metais · Water in Atmospheric Corrosion · Corrosion Inhibition and Inhibitors · Stress-Corrosion Cracking · Cooling Water and Cooling-Water Treat­ ment · High-Temperature Corrosion in Coat Gasifica­ tion Plants

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Books Analytical Methods for Pesticides and Plant Growth Regulators. Vol. 11. Gun­ ter Zweig and Joseph Sherma, Eds. xii + 408 pages. Academic Press, 111 Fifth Ave., New York, N.Y. 10003. 1980. $46

Reviewed by George Yip, Division of Food Chemistry, Food and Drug Ad­ ministration, Washington, D.C. 20204 This book continues the series that began in 1963 for two purposes: to present analytical methods for specific pesticides and to update analytical methods as well as general techniques. The present volume meets most of the editors' objectives. Three general techniques are updated. The chapter, "Automated Pesticide Analytical Lab­ oratory," describes automation from extractions of solids, gases, and liquids to the final determinative step (GLC, HPLC or TLC). This topic is growing in importance because automation means increased efficiency. The infor­ mation provided can easily be applied in nonpesticide laboratories. The chapter "HPLC in Pesticide Residue Analysis" is primarily one of general review rather than an update of HPLC. Theory, column and solvent selection, and instrumentation are dis­ cussed generally. Readers would have been better served if more specific in­ formation had been included, i.e., types of solvent delivery systems and detectors (advantages and disadvan­ tages). The section describing the use of SEP-Paks appeared to be out of place in this type of article. The update, "Quantitative TLC," could have been made more specific by deleting or minimizing the material on sample extraction, sample cleanup, solvent systems, and Rf tables. Mate­ rial that should have received more emphasis includes instrumentation, effects of scanning rates, and expected accuracy of densitometry. The remaining chapters are devoted to recommended methods for specific compounds, many of which are rela­ tively unknown to the pesticide chem­ ist (etrimfos, promacyl, quinalphos, terbufos, thiocyclan-hydrogenoxalate, ethylenebisdithiocarbamates and deg­ radation products, fentin hydroxide, iprodione, tricyclazole, chloropropham, dibenzoquat, Drepamon, flurecol, oxyflurfen, Quintex, terbuthiuron, and JV-nitroso compounds). The infor­ mation on each compound is extensive and complete (alternate names, toxici­ ty, physical and chemical properties, formulations, and analyses). Most of the analyses use GLC in the determi­ nation step. There is a wealth of infor­ mation on each compound. The "Ethylenebisdithiocarbamates

Books and Their Degradation Products" is well written. The assembled informa­ tion is detailed and for the first time focuses on all the known degradation products (ethylenethiourea, ethyleneurea, 2-imidazoline, ethylenethiuram monosulfide, and ethylenebisisothiocyanate) and their chemistry. JV-nitrosoamines continue to be of concern. The timely chapter on "Anal­ ysis of N-nitroso Compounds in Pesti­ cide Formulations" provides readers with up-to-date information on ana­ lytical techniques, instrumentation, and formulation analysis. Biological Monitoring Methods for In­ dustrial Chemicals. Randall C. Baselt. χ + 301 pages. Biomedical Publica­ tions, P.O. Box 495, Davis, Calif. 95616. 1980. $47

Reviewed by Larry K. Lowry, Division of Biomedical and Behavioral Science, NIOSH, Mail Stop C-26, 4676 Columbia Pkwy., Cincinnati, Ohio 45226 The field of biological monitoring, defined as the analysis of specimens taken from workers (blood, urine, hair, breath, tissue) for evidence of expo­

sure to industrial chemicals, is an emerging discipline that has not been widely used in this country. The tradi­ tional techniques of environmental monitoring generally indicate airborne concentrations of industrial chemicals and not worker absorption. The use of biological monitoring as part of an oc­ cupational health and industrial hy­ giene program can provide objective evidence of exposure of the individual to industrial chemicals by all routes of exposure, particularly skin absorption. Baselt's book has been written to stimulate research and use of biologi­ cal monitoring to assess worker expo­ sure. It serves as an excellent, concise source book for both the novice and practicing chemist, as well as occupa­ tional health professionals. It includes chapters on 79 common substances found in the workplace including 21 inorganic substances, 17 pesticides and herbicides, and numerous suspect or recognized carcinogens. Each chap­ ter, consisting of 1-3 pages, summa­ rizes information and exposure guide­ lines on a single chemical. The chap­ ters consist of single paragraph de­ scriptions of (1) occurrence and usage, (2) blood concentrations, (3) metabo­

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1002 A • ANALYTICAL CHEMISTRY, VOL. 53, NO. 8, JULY 1981

lism and excretion, (4) toxicity, (5) bi­ ological monitoring, (6) analytical methods, and (7) references. The liter­ ature coverage is not extensive, but the references cited are representative and recent. The methods discussed and recom­ mended are listed in outline form and, in some cases, alternative methods are given. While the selection of methods generally represents those most com­ monly used, some of the methods are dated and not considered rigorous. Most of the chapters are relatively complete and give the chemist or health professional a concise starting point for biological monitoring ap­ proaches. For a book of approximately 300 pages, a significant amount of fingertip information is readily avail­ able. One possible deficiency is that most of the chapters do not address speci­ men collection techniques, anticoagu­ lants, preservatives, or stability—all factors that are significant when a sample is analyzed at a remote loca­ tion. Also, there is generally a lack of information on when urine specimens should be collected for urinary metab­ olite evaluations, an important factor related to the pharmacokinetics of the parent compound. The selection of "normal" or "acceptable" values by the author should be verified with specimens collected from nonexposed workers since many of the values list­ ed are not well established. The au­ thor's mix of details overall is consis­ tent with his purpose of increasing awareness of biological monitoring. I have been associated with biologi­ cal monitoring for over 10 years, and I have found this book to be an excel­ lent reference source, which I use fre­ quently, especially when responding to questions of how to monitor an oc­ cupational exposure. Many of the methods listed have been successfully used in this laboratory; others still must undergo field evaluation. For in­ dividuals involved in biological moni­ toring or considering the use of this tool, the book is invaluable.

Books Received Proceedings of the Fifth International Conference on Zeolites. L. V. C Rees, Ed. xxxiii + 902 pages. Heyden & Sons, Inc., 247 South 41st St., Philadelphia, Pa. 19104. 1980. $81 Prudent Practices for Handling Haz­ ardous Chemicals in Laboratories. Na­ tional Research Council, Committee on Hazardous Substances in the Laborato­ ry, xiv + 291 pages. National Academy