Books
Neutron Activation Analysis: Thorough and Successful Discussion Activation Analysis with Neutron Generators. Sam S. Nargolwalla and Edwin P. Przybylowicz. xvii + 662 pages. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1973. $29.50 Reviewed by J. Hoste, Institute for Nuclear Science, University of Ghent, Ghent, Belgium Although a number of excellent books deal with neutron activation analysis, this one by Nargolwalla and Przybylowicz is most welcome, as it is the only one to deal so thoroughly with activation analysis by means of neutron generators and more particularly with 14-MeV neutrons. Even an
experienced activation analyst desiring to apply this technique is indeed confronted with many problems and options. He is, for instance, faced with the choice of "open" accelerators or sealed tubes. Each of these options again offers different alternatives as far as ion source, pumping system, target, high-voltage supply, transport system for the samples, neutron monitoring, etc., are concerned. The working principles of these alternatives are not only described in detail, but also advantages and disadvantages are discussed, so that the reader is able to choose the solution most satisfactory for his particular
problems. The fact that they also describe a great variety of complete existing systems, including the radioprotection arrangements, is of great help in planning an installation. As analysts are eventually mainly interested in accuracy and precision of the results, the chapter on sources of errors is particularly appreciated. More than half of the book finally deals with applications, element per element, for 14-MeV, 3-MeV, and thermal neutron activation, giving usually activation and decay curves, but not the gamma spectra of the isotopes produced which might have been more useful. As by far the most
SSIE Research Information Packages In a recent article, "Research in Progress," in our News and Views section (page 723 A of the July 1974 issue), the services of the Smithsonian Science Information Service (SSIE) were described. SSIE publishes the SSIE Science Ne wsletter which contains new listings of available research information packages. Some of the "packages" that may be of interest to analytical chemists were abstracted from a recent issue of the Newsletter.
sers for spectral analysis and remote monitoring of pollutants in the lower and upper atmosphere. $35 IR02S X-ray Fluorescence Analysis: Analysis of cements; rocks; minerals; rare earth compounds; super-conducting, ferromagnetic, and ferroelectric materials; archeological artifacts; plus trace element analysis of air and water pollutants, and the use of nuclear sources and semiconductor detectors. $35
To order the following, write to SSIE, Inc., Room 300, 1730 M IR03S Electron Spectroscopy: Photoelectron, Auger, and St., N.W., Washington, D.C. 20036. (Include code number and title. secondary electron spectroscopy, including the developAdd 10% postage and handling for orders outside the U.S., Cana- ment of spectroscopic techniques; analysis of material surda, or Mexico.) face structure, atomic and chemical structure, chemical and physical reactions. $45 IU10S Môssbauer Effect Spectroscopy: Structure of solids, organic and biological compounds; industrial and metallurgical applications. $45
FJ07S Neutron Activation Analysis. $35 IJ02S Dye Lasers: Dye laser tuning, broadband emission, mode loolocking, residual absorption, molecule-solvent interactions, picosecond pulse generation, dye laser spectroscopy, device developments. $35
IU16S Liquid Crystals: Studies on liquid crystals including formation, orientation, phase change, spectral analysis applications. $35
IJ04S Chemical Lasers: New types and materials, reaction kinetics, efficiencies, spectroscopic analysis, exothermic reactions, mode control, combustion lasers, reaction rates, molecular energy transfer. $25
IU04S Semiconductor Radiation Detection: Radiation detection in the optical (IR, visible, UV) and the nuclear (gamma, X-ray, etc.) range, plus crystal growth and development, material and device characteristics. $45
IJ09S Laser Nondestructive Testing: Applications of lasers and laser holography in the analysis of structures and materials such as solid propellents, tires, metals, etc. $35 IJ13S Laser Application in Chemical Analysis: Raman spectroscopy; laser emission spectroscopy; laser-stimulated fluorescent emission spectroscopy; photo fragment, matrix isolation, two photon, and molecular beam maser- and laser-enhanced absorption spectroscopy. $45
IZ04S Interferometers and Interferometry: Interferometry in the X-ray to radiofrequency range; long base interferometry; streak, laser, schlieren, scanning, Fourier transform, and shearing interferometry; interferometer development and applications; gratings. $45
IJ18S
IZ07S Optical Detectors: Microwave, infrared, visible, and ultraviolet detectors and detection systems; fundamental properties of detectors; performance analysis; development Laser Applications to Air Pollution: Utilization of la- and design criteria; plus associated research. $55
ANALYTICAL CHEMISTRY, VOL. 46, NO. 11, SEPTEMBER 1974 • 903 A
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frequent and successful application of 14-MeV neutrons deals with the oxy gen determination, a more detailed description, for instance, in metals would also have been welcome. As a whole one can feel that the book is written by analysts who have a great expertise in the field and have succeeded extremely well in making this knowledge available to potential users.
Organometallics from Li to Tl Chemical Analysis of Organometallic Compounds, Vol 1. T. R. Crompton. χ + 258 pages. Academic Press, Inc., (Lon don) Ltd., 24-28 Oval Rd., London, NW1 7DX, England. 1974. $16.25
Reviewed by E. C. Ashby, School of Chemistry, Georgia Institute of Tech nology, Atlanta, Ga. 30337 This book is concerned with the analysis of organometallic compounds containing metals of Groups I—III A and B: Li, Na, K, Cu, Ag, Au, Be, Mg, Ca, Cd, Hg, B, Ga, In, Tl. Analysis of aluminum and zinc compounds is not included, having been the subject of a previous book by Crompton entitled, "Analysis of Organoaluminum and Organozinc Compounds" (Pergamon Press, 1968). The chapters are ar ranged on the basis of the position of the metals in the Periodic Chart be ginning with lithium and ending with thallium. The most extensive coverage is for lithium, magnesium, mercury, and boron, consistent with the interest in and extent of analytical develop ment of these areas of organometallic chemistry. Each section is arranged according to the techniques of analy sis. For example, beginning with lithi um, the first section is concerned with methods of determination of the ele ments; the next section is concerned with titrametric methods involving coupling with alkyl halides, oxidation, cleavage with dialkyl or diaryl sul fides, thermometric titration, and lumometric titration; the next section deals with colorimetric methods (Watson-Eastham titration), and the fol lowing sections deal with NMR, UV, and GLC as methods of analysis. Throughout the book, details of spe cific analytical procedures are given so that the book itself can be used as a primary source. Since there is no other book that deals with analysis of main group or-
ganometallic compounds, the value of having most of the reported methods of analysis of these compounds at one's fingertips is of obvious merit. Close scrutiny of th sections on organolithium and organomagnesium compounds indicates that the author has an expert's appreciation for the compounds about which he writes, al though one of the simplest and best methods for analyzing organomag nesium compounds, namely, hydroly sis, followed by EDTA titration for magnesium seems to be missing. In addition, there seems to be no men tion of analysis of compounds such as PhMgBr or C 6 H 13 MgBr by GLC anal ysis of the benzene or hexane pro duced on hydrolysis of the Grignard reagent. Nevertheless, the book is well writ ten and complete enough to be a valu able addition to any laboratory con cerned with the preparation or utiliza tion of main group organometallic compounds.
Self-Study Review for Practicing Chemists The Interpretation of Proton Magnetic Resonance Spectra: A Programmed Introduction. E. J. Haws, R. R. Hill, and D. J. Mowthorpe. xii + 1 8 0 pages. Sadtler Research Laboratories, Inc., Book Division, 3316 Spring Garden St., Philadelphia, Pa. 19104. Paperbound. $6.90
Reviewed by David M. Grant, Depart ment of Chemistry, University of Utah, Salt Lake City, Utah 84112 This book provides a programmed learning introduction to the elementa ry principles of high-resolution proton magnetic resonance (PMR). It is ori ented toward the practicing chemist who wishes to use the PMR technique as a tool for compound identification and characterization, and probably would not meet the needs of more the oretically inclined workers. The ap proach does not presume any previous knowledge of the magnetic resonance field and begins with basic principles. While the level is mainly introductory, the program does develop concepts which are sufficiently sophisticated that the book should be useful as a self-study review for all but special ists. No attempt has been made to treat extensively the mathematical and physical foundations of the field, but the qualitative discussions of these more rigorous treatments are in the main satisfactory. The self-instructing program pro gresses smoothly from elementary concepts and definitions to a function al level where an individual should be able to handle readily the greater frac tion of PMR spectral information.
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The organization of concepts and the development of background informa tion are handled adroitly. Prom basic knowledge of chemical shifts and spinspin coupling, the authors introduce the problems encountered in complex spectra where overlapping of spectral lines and second-order effects of strongly coupled protons become im portant. The treatment of secondorder coupling effects is limited, for all intensive purposes, to the simplest possible case of two spins; therefore, most of the really challenging prob lems encountered in extracting infor mation from second-order splittings are not treated. On the other hand, the effects of temperature-dependent chemical exchange, of geminal nonequivalents owing to molecular sym metry, and of deuterium labeling are treated with some care. A good set of qualitative analysis problems accom panies the book, and these illustrate quite well the concepts developed in the book. The material is easy to read and fol low, since it is written in a typically clear and crisp British style. One minor criticism deals with the physical arrangement of questions and an swers. This could be improved, as one must frequently flip pages back and forth to proceed in the manner intend ed. The program should be suitable for undergraduate students involved in their first basic course in organic chemistry but would still be challeng ing to more advanced students.
Structural Studies of Organic Molecules Applications of Raman Spectroscopy. Stanley K. Freeman. Six cassettes + one course manual. Department of Edu cational Activities, American Chemical Society, 1155 16th St., N.W., Washing ton, D.C 20036. 1973. $85
Reviewed by William E. L. Grossman, Department of Chemistry, Hunter College of the City University of New York, New York, N.Y. 10021 "Applications of Raman Spectros copy" is a tape-recor.ded discussion by Dr. Freeman of certain aspects of Raman spectroscopy. A better title would be "Structural Studies of Or ganic Molecules by Raman Spectros copy." Apart from a brief introduction to the theory of the Raman effect, and some observations on suitable instru mentation, the work is devoted exclu sively to this subject. I found both advantages and disad vantages to the tape-recorded format. The author is a fluent speaker with a pleasant voice, and his enthusiasm for and obvious knowledge of Raman
spectroscopy are conveyed with an im mediacy which would be difficult to achieve in a conventional book. This is a major advantage of these recordings. On the debit side, the informality of the medium makes for a presentation which is perhaps slightly less careful than a written work would be. Two in stances may be noted: in the discus sion of depolarization ratio, it is de fined as IJly = I±/I{. Ix is stated to be the intensity of the depolarized radia tion scattered by the sample, and Iy that of the polarized radiation; in fact, it would be more exact to define them as the intensities of scattered light whose electric vectors are polarized parallel to the χ and y axes, respec tively. Similarly, IL and Γ\ are said in both the written and spoken text to be the transmitted intensities "when the analyzing polarizer is oriented perpen dicular and parallel with respect to the scattered . . . radiation," whereas, for the example used (plane polarized incident light), the reference direction is generally taken to be the electric vector of the incident radiation. It is likely that if the work had been pre sented in a more conventional format and had been easier to proofread and edit, the author would not have per mitted these statements to remain in their present form. The above points are not especially important when viewed in the context of the work as a hole, whose emphasis is on organic structural analysis. How ever, the cost of the set places it pretty well out of the reach of everyone but book reviewers and organizations like chemistry departments. The latter might be well advised to use it as an adjunct to the organic chemistry course, to offset the over-emphasis on infrared analysis found in most organ ic analysis courses. The prospective use of the tapes by undergraduates makes even minor errors more serious than they appear to more sophisticat ed users. The only other cavil is that Dr. Freeman, in his position of evangelist for Raman spectroscopy, at times un balances his presentation slightly too far in favor of Raman at the expense of infrared spectroscopy, which is, after all, still a useful technique. On the whole, though, the tapes are stim ulating and informative, and I would recommend them strongly as an edu cational tool.
How to Write a Technical Paper Practical Technical Writing. Jay R. Gould. Eight cassettes + one course manual. Department of Educational Ac tivities, American Chemical Society, 1155 16th St., N.W., Washington, D.C. 20036. 1973. $95
Books Reviewed by L. E. Erickson, Depart ment of Chemistry, Grinnell College, Grinnell, Iowa 50112 Jay Gould has put together an or derly and comprehensible guide to technical writing. The course empha sizes preparation of technical reports, including a general treatment of fun damental principles and separate sec tions dealing with the main text, pref atory and appendix material, internal structure, support material, mechanic (grammar, punctuation, etc.), and vi sual and graphic material. This is fol lowed by short sections on preparation of directions or instructions and prep aration of proposals. The final section discusses the technical paper, its char acteristics, format, and support mate rial. The need for the technical writer to inform, instruct, and persuade, with varying degrees of emphasis, provides the unifying theme for the course. The author makes no claim that the treatment of the various topics is uni formly thorough or complete. For ex ample, the section on the mechanics of technical writing is no substitute for a handbook of English usage. However, the material he does include in this section is well chosen and particularly pertinent to technical writing. Simi larly, the ACS "Handbook for Au thors" is a more complete and authori tative guide to manuscript prepara tion for an ACS journal than the rela tively brief treatment in this course. Appropriately, the importance of con sidering journal characteristics and re quirements is emphasized first in the section on the technical paper. The course is intended for practic ing scientists and engineers. Anyone who has faced the problem of writing technical material in his work or has recognized his need for some useful in structions on ways to improve his writing would find the material very useful. Although the course is de signed to permit either individual or group use, I suspect that it would have much greatr impact if a small group of persons in a lab or plant were to go through the material together. Inclu sion of sessions in which they criticize each others' reports, manuscripts, or responses to the exercises which follow each main section would help to over come one of the principal hazards of self-study courses, the lack of active participation and feedback. Overall, this course is no substitute for a full-semester course in technical writing, complete with regular criti cism from the instructor on specific assignments. However, it is probably
SURFACE AREA MICROMERITICS'proven analyzer accurately measures B.E.T. surface area and adsorption and desorptlon Isotherms. FEATURES • Classical, static, low-temp erature gas adsorption (B.E.T.) technique • Any non-corrosive gas for adsorbate • Requires no mixing of gases • No calibration required • Measures specific surface areas from 0.001 mVg up • Auto-ranging digital pres sure display, 0.0001 to 1000 mm Hg • Completely self-contained, built-in vacuum system • Proven system design . . . durable, all-metal construction • Outgases 4 samples to less than 0.001 mm Hg The most versatile, accurate manual analyzer on the market today, the Model 2100D measures specific sur face areas from 0.001 m7g up . . . no upper limit known . . . measures pore radii from about ten Angstroms up. Can also perform simple chemisorption studies. Utilizes the classical, ' static B E T . technique of adsorbing a gas at a temperature near its boil ing point . . . uses any non-corrosive gas as adsorbate . . . no calibration re quired . . . accurate, auto-ranging, di rect digital display of system pressure from 0.0001 to 1000 mm Hg. The Model 2100D is completely self-contained with all operations controlled and monitored from the front panel . . . built-in high vacuum system can outgas four samples to less than 0.001 mm Hg to prepare them for analysis . . . Dual adsorbate controls allow quick adsorbate changeover without line purging. Also Available: • DlgiSorb 2SQ0 - a computer controlled Instrument with capability exceeding the remarkable Model 2100D. « High Speed Surface Area Analyzers for B.E.T. surface areas In minutes.
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ANALYTICAL CHEMISTRY, VOL. 46, NO. 1 1 , SEPTEMBER 1974 • 907 A
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more accessible and directly pertinent to most practicing engineers and scientists. It is well worth the $95 cost for an organization and the 5-hour time investment for motivated students.
New Books instrumental Methods of Analysis. Fifth edition. Hobart H. Willard, Lynne L. Merritt, Jr., and John A. Dean, xix + 860 pages. D. Van Nostrand Co., 450 West 33rd St., New York, N.Y. 10001. 1974. $15.95
The fifth edition of this classic textbook continues to survey modern instrumental methods of chemical analysis. According to the authors, most of the chapters have been extensively revised, and some completely rewritten. Among the new topics covered in this edition are turbidimetry and nephelometry, the vacuum ultraviolet, reflectance measurements, Fourier transform IR, laser Raman spectroscopy, Mossbauer spectroscopy, GC/MS, and all classes of ion selective electrodes. AA has been expanded and integrated with emission. Classical polarography is treated in an enlarged chapter on voltammetry, polarography, and related techniques. Emphasis continues to be placed on structural identification of compounds through IR and Raman spectra, NMR, ESR, UV, and MS. Numerous examples are incorporated within the text. There are 390 numerical problems, many containing data that would be obtained in laboratory experiments. The experiments included have been selected to illustrate the principles discussed in the theoretical sections of each chapter. Some are described in great detail, and others are sketched outlines or suggestions for further work. Quantitative Analytical Chemistry. Third edition. James S. Fritz and George H. Schenk, Jr. xiv + 689 pages. Allyn & Bacon, Inc., 470 Atlantic Ave., Boston, Mass. 1974. $14.95
In the third edition of this text, a new chapter has been added to show by actual examples how an analytical chemist goes about solving problems and modifying analytical procedures to fit new situations. The authors have also tried to make the "relevance" of analytical chemistry more apparent while maintaining the emphasis on solid principles. Significant changes that have been made in this edition
include a much greater emphasis on chromatographic methods of separation and analysis, a section on how to handle and evaluate small sets of data, a section on enzymatic-kinetic methods of analysis, more theory and applications of ion-selective electrodes. Four new laboratory experiments have been added: statistical evaluation of weighing data; fluorometric procedure for the determination of vitamin D; a new GC experiment; and a TLC separation of nitroanilines. Reaction Mechanisms in Organic Analytical Chemistry. Kenneth A. Connors, xiii + 634 pages. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1973. $18.50
This book discusses organic analytical reactions on the basis of reaction type and mechanism, rather than by analytical method or technique or functional group. Attention is given to classical areas of analytical interest, such as acid-base reactions, metal-ligand coordination equilibria, and solubility phenomena. The text begins by establishing the physical-chemical basis of investigations into organic reaction mechanisms and describes the present state of knowledge of reaction mechanisms in the major classes of organic heterolytic reactions. This volume views analytical chemistry from the standpoint of physical organic chemistry. To illustrate mechanistic points and analytical applications, many examples have been selected from the biochemical literature. More than 100 problems have been included. The text is reproduced from typed copy. Process Synthesis. Dale F. Rudd, Gary J. Powers, and Jeffrey J. Siirola. xi + 320 pages. Prentice-Hall, Inc., Englewood Cliffs, N.J. 07632. 1973. $15.95
By integrating the concepts of synthesis and analysis in a parallel learning program, the aim of this book is to promote ease with the step-by-step utilization of analysis and synthesis in process development. The contents include chapters on the engineering of process systems, reaction-path synthesis, material balancing and species allocation, separation technology, separation task selection, task integration, and two on applications—fresh water by freezing and detergents from petroleum.
Continuing Series Ion Exchange and Solvent Extraction, Vol 6. Jacob A. Marinsky and Yizhak Marcus, Eds. xii + 301 pages. Marcel Dekker, Inc., 270 Madison Ave., New York, N.Y. 10016. 1974. $27.50
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The contents of this book are isolation of drugs and related organic compounds by ion-pair extraction, the dynamics of liquid-liquid extraction processes, application of the solubility concept in liquid-liquid extraction, and solvent extraction in the separation of rare earths and trivalent actinides. The text is reproduced from typed copy.
Investigation of Rates and Mechanisms of Reactions. Third edition. Gordon G. Hammes, Ed. xiii + 665 pages. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1974. $27.50
This book is Part Two of Vol 6 of "Techniques of Chemistry," edited by A. Weissberger. It brings together recent international advances in fast reaction techniques. The chapters discuss rapid flow methods, relaxation spectrometry, electrochemical methods, photostationary flash photolysis, nuclear magnetic resonance, and electron paramagnetic resonance. Principles and illustrative examples are given.
Applications of the Newer Techniques of Analysis. Ivor L. Simmons and Galen W. Ewing, Eds. viii + 383 pages. Plenum Publishing Corp., 227 West 17th St., New York, N.Y. 10011. 1973. $22.50
This book is volume six in the series "Progress in Analytical Chemistry." A group of selected papers given at the November 1972 meeting of the Eastern Analytical Symposium held in Atlantic City, N.J., is presented. Applications of Raman spectroscopy, X-ray diffraction, emission spectroscopy, nuclear magnetic resonance, liquid chromatography, thin-layer chromatography, pyrolysis chromatography, mass spectrometry, gas chromatography, and GC/MS are included. The text is reproduced from typed copy.
Separation and Purification Methods, Vol 2. Edmond S. Perry, Carel van Oss, and Eli Grushka, Eds. xi + 466 pages. Marcel Dekker, Inc., 305 East 45th St., New York, N.Y. 10017. 1974. $25.50
This volume contains discussions of applications of gas-solid chromatography, field flow fractionation, separation of latex particles according to size by continuous electrophoresis, affinity chromatography, gel chromatographic separation of oligosaccharides, free fluid particle electrophoresis on Apollo 16, methods of separation and purification using the molecular sieving properties of zeolites, and high-speed liquid chromatography. The text is reproduced from typed copy.
