A Useful Compendium of Methods - Analytical Chemistry (ACS

May 29, 2012 - A Useful Compendium of Methods. Anal. Chem. , 1983, 55 (6), pp 665A–666A. DOI: 10.1021/ac00257a778. Publication Date: May 1983...
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FOR FAST HPLC ANALYSIS... A Useful Compendium of Methods

Gas Chromatography of Organometal¬ lic Compounds. T. R. Crompton. χ + 589 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1982. $75

Reviewed by Peter Uden, Department of Chemistry, University of Massa­ chusetts, Amherst, Mass. 01003 This book provides the most com­ plete compendium available on gas chromatographic methods of analysis for organometallic compounds. The information is assembled as a detailed review and includes a substantial amount of experimental information. The author has used a group-by-group elemental survey of his subject. While the topic clearly is of interest to only some analytical chromatographers it nevertheless reflects well the extensive literature in this rather neglected field. Many will be surprised by the wealth of documented data and may be encouraged to apply it to their own analytical problems. In his introduction the author notes that there are more than 1000 papers in the organometallic gas chromato­ graphic literature. He includes discus­ sions of 528, usually with sufficient coverage to demonstrate their impor­ tance to the reader. Substantial por­ tions of key papers are quoted verba­ tim or with little condensation; thus while the information content is very high, there is little attempt at apprais­ al of advances in experimental gas chromatography. Information and procedures from the 1960s often are presented side by side with more re­ cent studies, and naturally much of the early work is outdated. This approach has the merit, how­ ever, of providing a good basis for reexamining many analytical GC problems in the light of current equip­

ment and methodology. Since such emphasis is placed on laboratory methods and results, the practical in­ formation should be of help to the ex­ perimental scientist—as long as it is viewed with an appropriately critical eye. The seven chapters are organized on a periodic basis. More than half of the book is dedicated to the group 4B ele­ ments, particularly silicon, reflecting the amount of work in this area. Organo-lead, tin, arsenic, mercury, and boron compounds are extensively treated, and there is coverage of com­ pounds of more than 15 other transi­ tion and main group metals. The only major omission is that of organophos­ phorous compounds; while this was dic­ tated by the definition of organometallics, their inclusion would have been useful. The author is usually careful to con­ fine coverage to definitive organome­ tallic compounds—those with sigma or pi carbon-metal bonds. However there are a few departures from this format—for example, the detailed in­ clusion of decomposition studies of zinc dialkyldithiophosphates, which is inappropriate—but since they are in­ cluded they should have been related to recent direct gas chromatographic studies of these chelates. The layout of the book makes it very easy for the reader to obtain in­ formation on the specific gas chro­ matographic behavior of compounds of particular elements, but a real defi­ ciency is the lack of introductory and background chapters relating to the overall field and its analytical and gas chromatographic problems. Correla­ tion of experimental approaches among different topics would be worthwhile as would introductory and

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ANALYTICAL CHEMISTRY, VOL. 55, NO. 6, MAY 1983 · 665 A

Books commentary material for each chapter. Despite some weaknesses and its high cost, the great amount of infor­ mation gathered here makes the book an essential acquisition for anyone in­ volved in the area of inorganic analyti­ cal chromatography; as a source text it is certainly invaluable. Ion Chromatography. J. S. Fritz, D. T. Gjerde, C. Pohlandt. χ + 203 pp. Dr. Al­ fred Huthig Verlag GmbH, Postfach 102869, 6900 Heidelberg 1, W. Ger­ many. 1982. $33

Reviewed by Roy Wetzel, Dionex Cor­ poration, 1228 Titan Way, Sunny­ vale, Calif. 94086 This is the first text that attempts to present all published methods be­ longing to the rapidly growing field of ion chromatography. Most methods found in the literature, along with those commercially available, are de­ scribed. The authors include a limited comparison of the two most prevalent methods, which they label "dual col­ umn" (including chemical reactions to reduce mobile phase background con­ ductivity) and "single column" (not including such reactions). IC methods using detectors other than conduc­ tance are described. The book is well organized and edit­ ed; it can be easily understood by the BS chemist. However, the synthesis of "single-column" ion chromatography column packings and their subsequent use, which are described in detail, may require more advanced training and skill. Over half of the text is dedicated to describing the dual-column and sin­ gle-column methods and applications available from Dionex Corporation and Wescan Inc., respectively. The dual-column discussion is more heavi­ ly weighted toward applications, while the single-column discussion empha­ sizes the synthesis of required chro­ matographic packings and the control of parameters affecting the chromato­ graphic analysis. Consequently, the useful knowledge for practicing ion chromatographers is limited to those who perform the single-column methods. Detailed description of instrumen­ tation is limited to the detectors com­ monly used for IC, including electro­ chemical (i.e., conductance, amperometric) and UV/VIS. Postcolumn derivatization is described as it applies to the detection of metals and phos­ phates. When comparing the sensitivities of the two prevalent methods, the au­ thors criticize an earlier publication

(Pohl, C ; Johnson, E. J. Chrom. Sci. 1980,18, 442) as being "erroneous and misleading." The discussion includes a systematic argument supporting their views, but fails to support the criti­ cism with specific evidence of errone­ ous or misleading data. It is unfortu­ nate that the first volume dedicated to such a valuable technique is colored by unsupported criticism of an excel­ lent publication. Certainly, the aca­ demic reader should scrutinize all per­ tinent literature before drawing con­ clusions regarding dual- and singlecolumn IC methods, and the practic­ ing analytical chemist should thor­ oughly evaluate existing methodolo­ gies before choosing one. In any case, the book is welcome be­ cause it is the first attempt to docu­ ment both the technique and applica­ tions of IC. Because IC methods are developed rapidly, several new meth­ ods are not included in this volume. Other useful publications include the IC chapter in "Trace Analysis," Vol. I; Lawrence, J.; Academic Press, 1982 and "Modern Inorganic Chromatogra­ phy"; Small, H.; Anal. Chem. 1983, 55, 235 A. A Textbook of Pharmaceutical Analy­ sis. 3rd. ed. Kenneth Connors, χ + 664 pp. John Wiley & Sons, Inc., 605 Third Ave., New York, N.Y. 10016. 1982. $55

Reviewed by Gary Christian, Depart­ ment of Chemistry BG-10, University of Washington, Seattle, Wash. 98195 This third edition of a successful textbook is very similar in organiza­ tion and content to the second edition, which was published in 1975. Most of the comments made by this reviewer previously (Anal. Chem. 1976, 48, 111 A) remain applicable. The text is ar­ ranged in six parts: titrimetric analy­ sis, physical and instrumental meth­ ods, separation techniques, elemental analysis, chemical reactions in analy­ sis (changed from functional group analysis), and some general topics. There are new chapters on immunoas­ say and derivative formation, and the statistics section has been expanded into a separate chapter with new ma­ terial on the correlation coefficient, least squares, detection limits, propa­ gation of errors, significant figures, and an expanded treatment of the t-test. The chromatography chapter has been reorganized with expanded discussion of detectors, column and solvent selection, and resolving power. While most original chapters re­ main largely unchanged, updated ref­ erences have been added, and there are 16 new problems, for a total of 252. New material presented includes oxi­

666 A · ANALYTICAL CHEMISTRY, VOL. 55, NO. 6, MAY 1983

dation-reduction of organic com­ pounds, pH standards for mixed or­ ganic-aqueous solvents, derivative spectroscopy, spectrophotofluorimetry and scatter interferences, fluorimetric drug analysis, ionization techniques, mixture analysis and double focusing in mass spectrometry, pH control in solvent extraction for group separa­ tions, and determination of thiol com­ pounds. There are five fewer experi­ ments for some saving of space, but two of the chromatographic experi­ ments are new. The analytical toxicol­ ogy chapter has been deleted, and the chapter on atomic absorption spec­ troscopy is a welcome addition. All in all, those who have found this text useful for their courses in the past will continue to do so with the new material. The length has been kept reasonable by carefully balancing new and old material.

Books Received Annual Reports on NMR Spectroscopy. Vol. 13. G. A. Webb, Ed. χ + 399 pp. Academic Press, 111 Fifth Ave., New York, N.Y. 10003. 1982. $99.50 The Polysaccharides. Vol. 1. Gerald Aspinall, Ed. xvi + 340 pp. Academic Press, 111 Fifth Ave., New York, N.Y. 10003. 1982. $47 Chromatography of Alkaloids. A. Baerheim Svendsen, R. Verpoorte. xv + 534 pp. Elsevier Scientific Pub­ lishing Co., 52 Vanderbilt Ave., New York, N.Y. 10017. 1983. $104.25 Safety and Accident Prevention in Chemical Operations. 2nd ed. Howard Fawcett, William Wood, xiv + 910 pp. John Wiley & Sons Inc., 605 Third Ave., New York, N.Y. 10016. 1982. $80 Thermal Analysis. Vols. 1 & 2, Bernard Miller, Ed. xxxii + 792 pp. and xxxii + 1530 pp. John Wiley & Sons Inc., 605 Third Ave., New York, N.Y. 10016. 1982. $90/2-vol. set Euroanalysis-IV. Reviews on Analyti­ cal Chemistry. L. Niinisto, Ed. 258 pp. Association of Finnish Chemical So­ cieties, Pohj. Hesperiankatu 3 Β 10, SF00260 Helsinki 26, Finland, 1982. 160 Finnish Markka Comprehensive Treatise of Electro­ chemistry. Vol. 6. Ernest Yeager et al., Eds. xxiii + 522 pp. Plenum Press, 233 Spring St., New York, N.Y. 10013. 1983. $67.50 Qualitative Inorganic Analysis. Theo­ dore Brown, H. Eugene LeMay. χ + 144 pp. Prentice-Hall, Inc., Englewood Cliffs, N.J. 07632.1983. $4.95