viron. Sci. Techno/., 7(11), Nov. 1973, (7Q) Gill, G. H., U.S. 3,720,093 (CI. 73/27R: G nol., 1974, 8(2) 149-52. 1056- 1059. Oln), 13 Mar. 1973; 5 pp. (2P) Bonczyk. P. A,, Ultee, C. J., Opt. Commun., 1972 6(2), 196-8. ( 1 3 ~ )Quinlan, C. W., Kittrell, J. R., J. Chromatogr. (8Q) King, W. H.. Ger. 1,598,401 (CI. G Oln) 05 Sci,, 10(11), 691-693. July 1973; U.S. Appl. 475,649; 29 July 1965; (3P) Breitenbach, L. P., Shelef, M., J. Air Poiiut. ControiAssoc., 23(2), Feb. 1973, 126-131. (14P) Sigsby, J. E., Jr., Black, F. M.. Bellar, T. A. 8 PP. (4P) Chand, R., U S . 3,763,025 (CI. 204/1T; G Klosterman, D L., Environ. Sci. Technoi., 7(1), (9‘3) Lauer, J. M., U.S. 3,767552 (Cl. 204/195P; G 51-54. Oln), 02 Oct. 1973; 7 pp. Olfl), 23 OCt. 1973: 5 DD. (5P) Dee, L. A., Martens, H. H.. Merrill, C. I., Naka- (15P) Wooten, G. W., Iltls, R., Johnson, V. L., U S . ( l o a ) Pebler, A,, Hickam.’ W. M., Ger. Offen. 3,749,929 (CI. 2501369; H Olj), 31 Jul 1973: 2,239,285 (CI. G Oln), 01 Mar. 1973; US. mura, J. T., Jaye, F. C., Anal. Chem., 45(8), Appl. 173,490; 20 Aug. 1971; 15 pp. July 1973, 1477-1481. 4 PP. (1lQ) Rosenthal, K., Bambeck, R . J., Anal. ln(6P) Diamond, P., U . S . Nat. Tech. Inform. Serv., strum., 1972, 10, 45-7. AD Rep., 1970, No. 752527; 13 pp; Avail. NTIS . (12Q) Ruch, W. E., “Quantitative Analysis of Gas(7P) Driscoll, J. N., Berger, A. W., Becker, J. H., Miscellaneous eous Pollutants,” Ann Arbor Sci. Publishers, Funkhouser, J. T., Valentine, J. R., J. Air Pol- ( l a ) Anonymous, Fed. Regist., 08 May 1973, Inc., P.O. Box 1425, Ann Arbor, MI 48106. /ut. Control Assoc., 22, 119-122, (Feb. 38(88),11458-63. (13Q) Senzel, A. J., “Instrumentation and Analytical 1972). (2Q) Armstrong, G. T., Domalski, E. S.,Minor, J. I., Chemistry,” ix -t 428 pp; Spec. Issues (8P) Kneebone. B. M., Freiser, H., Anal. Chem., Jr., Am. Gas Assoc., Oper. Sect., Proc., Sales, Am. Chem. SOC., 1155 16th St., N.W., 45(3), March 1973, 449-452. 1972. D74-D87. Washington, DC 20016; 1973. (9P) Kothny, E. L., Cook, W. A. Dimitriades, B., (30) Christian, J. D., Anal. Chem., 1973, 45(4), (l4Q) Wilhoit, R. C., Bell, M. E., Subach, D. J., Ferrand, E. F., Nifong, G. D., McDaniel, P. W., 698-702. Chen, C., J. Chem. Educ. 1973: 50(7), 486. Saltzman, B. E., Weiss, F. T., Health Lab. (4Q) Clingman, W. H., Jr., Amer. Gas Assoc., Oper. Sect., Proc., 1972, D64-D69. Sci., 1972, 9(4), 327-35. (1OP) Margolis, G., Driscoll, J. N., Environ. Sci. ( 5 0 ) Ferber, B. I., Wieser, A. H., U.S. Nat. Tech. inform. Serv., P 6 Rep., 1972, No. 210991, Standards Technoi,, 1972, 6(8). 727-31. (11P) Martens, H. H., Dee, L. A,. Nakamura, J. T., 21 pp: Avail. NTIS. (1R) ASTM Standards, Parts 18 and 19, Philadelphia, PA, 1972. Jaye, F. C., Environ. Sci. Technoi., 1973, (6Q) Fiais, L. R., Gentile, R. G., Ger. Offen. 7(13), 1152-4. 2,242,851 (CI. G Oln), 08 Mar. 1973; U S . (2R) ASTM Standards, Parts 18 and 19, PhiladelAppl. 176,804: 01 Sept. 1971; 24 pp, phia, PA, 1973. (12P) Merryman, E. L., Spicer, C. W.. Levy, A,. En-
Inorganic and Geological Materials Joseph 1. Dinnin U S .Geological Survey, National Center, MS 923,Reston, VA 22092
This review attempts to take an interdisciplinary look a t recently described methods for applied inorganic analysis. This section’s antecedents are the review of “Inorganic Microchemical and Trace Analysis” and “Inorganic Analysis” prepared for Fundamental Reviews for many years by P. W. and F. K. West (199) and the review entitled “Nonferrous Metallurgy. 11. Zr, Hf, V, Nb, T a , Cr, Mo, W”, most recently prepared by Butler and Kniseley (36). The title has been changed more nearly to reflect the nature of the content of the sections as they have evolved during recent years. The subject matter of the applied review has included not only nonferrous metallurgical analysis but the analysis of an increasingly wide range of inorganic materials. These areas of interest will be continued and extended to include other metallurgical, ceramic, or general inorganic material not elsewhere reviewed in this Journal. This chapter will also attempt to review major developments in the analysis of geological materials and, in general, to serve as a catchall for subject matter in inorganic analysis that may otherwise escape attention in the other fundamental or applied reviews. The area of interest includes classical and instrumental analysis. Abstracts and periodical literature up to November 1974 were included for consideration. In recent years, an average of approximately 200 abstracts have appeared biweekly in the “Inorganic Analytical Chemistry” section of Chemical Abstracts. Thus, a twoyear period normally covered in a review would represent a body of data that includes approximately 10,000 publicaAuthors have not been supplied with free reprints for dlstributlon. Extra coples’of the revlew Issue may be obtained from Speclal Issues Sales, ACS, 1155 18th St., N.W., Washington, DC 20038. Rernlt $4 for domestic U.S. orders; add $0.50 for addltlonal postage for foreign destinatlons.
tions. Fortunately, the biweekly subject index of Chemical Abstracts and the prompt yearly indexes of both Chemical Abstracts and Analytical Abstracts facilitate literature searches for individual subjects and obviate the need for the massive tables of reference data that would be required for a comprehensive review of inorganic analysis. This facilitates the dictum of the editor that reviews be critical and selective rather than all-inclusive. I t is as apparent in analytical chemistry as in other fields of science that “we are all laymen in each other’s specialties” (191).With this in mind, it is the general objective of this review to facilitate the task of the nonspecialist in keeping abreast of the recent developments in other analytical techniques and procedures. Attention will be directed primarily to work of a general nature that can serve as a starting point for more intensive literature searches or study and works that will help fully occupied analysts to keep abreast of developments in related fields. I have tried to approach this review from the viewpoint of a chemist whose job it is to analyze, advise, or direct the analysis of inorganic or geological materials and who would like to know some of the major advances that have been made in the last couple of years while he has been busy with a specialty or otherwise out of touch with the field. I shall try to call attention to major items in the literature including books, monographs, reviews, compendia, and major instruments, techniques, or trends and do what I can to help an interested analyst to uncover any generally useful papers that may be buried in the mass of literature. Applied inorganic analysis has in great part become the application of instrumental techniques to the analysis of inorganic materials. In many metallurgical, industrial, and commercial laboratories most analyses are performed by ANALYTICAL CHEMISTRY, VOL. 47, NO. 5, A P R I L 1 9 7 5
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emission spectrographic, flame spectrometric, X-ray fluorescence spectrometric, or other almost exclusively instrumental technique; it has been estimated that more than 75 percent of the analyses in the metals industry are performed by emission spectroscopy ( 0 - 1 7 ) .The wet chemical methods emphasized in this review represent merely the tip of the analytical iceberg. As noted by West (199), it should be understood that for a truer picture of recent advances in applied inorganic analysis, one must also refer to the other applicable sections of the Fundamental Reviews.
CLASSICAL ANALYSIS In a debate on the subject, “Is Classical Analysis Outmoded” sponsored by the Microchemical Methods Group of the Society for Analytical Chemistry ( 5 4 ) , A. G. Jones defended the term classical by quoting the Oxford English Dictionary definition as meaning “of the first rank or authority”. Classical analysis, he noted, is not the analytical technique of a particular period or particular group but comprises the best analytical technique available. I t is that technique requiring the most elegant of manipulative skills. He argued that as life progresses and as knowledge increases, so should classical analysis. I t does not necessarily require beakers, test tubes, Bunsen burners, or even H2S. Jones argued that analysts should take a balanced view of the tools of their profession, using those that did the job they had in hand, keeping the others available for use when necessary. There was, of course, confusion because of the number of tools available for the same job. But surely, he argued, this was where the professional expertise of analysts came in. He also warned that they should not become so enamored of the more glamorous, elaborately instrumented techniques that they lose sight of the simple, elegant techniques that were available.
GENERAL REVIEWS OF INORGANIC ANALYTICAL TECHNIQUES For many years the Fundamental and Applied Reviews in this Journal and the Annual Reports of the Chemical Society (London) were the two primary annual reviews, in English, of new developments in inorganic analysis. Fortunately, with the proliferation of the literature has come a proliferation of the periodic reviews that enable analysts to keep abreast of developments in their own and other specialties. The Fundamental Reviews in this Journal remain perhaps the single most useful recent reviews of methods of applied inorganic analysis. They include reviews of almost every major instrumental technique applicable to the analysis of inorganic or geological materials. In addition to general reviews of individual techniques, the sections on “Emission Spectrometry”, “Light Absorption Spectrometry’’, “Ion Exchange”, “Analytical Electrochemistry”, “Electroanalysis and Coulometric Analysis”, and “Fluorometric Analysis” have in recent years also included references to applications of the methods and useful tabulations of methods for determining the individual elements. In addition, various of the other sections have also contained useful discussions and tabulations of methods used for determining inorganic constituents. For instance, the section on “Organic Elemental Analysis” has contained a section on metallic elements; information in this section may be useful for analyzing mixtures of inorganic and organic constituents such as shales or clays. In addition, various other chapters of this Applications Review undoubtedly contain much material pertinent to inorganic analysis. For instance, the 1973 chapter on “Air Pollution” contains a large section devoted to “Inorganic 98R
Composition” reviewing recent advances in methods and procedures for inorganic constituents; much of the material discussed in “Nonferrous Metallurgy” is also applicable to general inorganic analysis; portions of the chapter on “Solid and Gaseous Fuels” and “Water” review methods for determining inorganic constituents. A similar comprehensive review is published in Japanese in J a p a n Analyst ( 3 4 ) and includes fundamental and applied subjects. The topics discussed in 1972 are very similar to those covered in the Fundamental Reviews, but include separate chapters on the following: analytical reagents; solvent extraction; ferrous analysis; analysis of nuclear fuels and reactor materials; analysis of ceramics (glass, cement, and refractory); forensic chemistry. A similar review of analytical techniques appears in Russian (119). The yearly review series (143-145) in Zavodskaya Laboratoria, published in Russian but available in English translation from Plenum Press, includes both a brief review of analytical techniques and tabular data on the determination of individual elements. The reviews, most recently prepared by Pilipenko and Volkova, are especially useful in that they include primarily material published in the USSR; the translations make this information readily available to English speaking analysts. Other reviews stress the general analytical techniques themselves and, in some instances include significant information on the determination of individual elements. The Selected Annual Reviexs published.by the Society for Analytical Chemistry ( 0 - 3 ,0 - 4 ) are a most useful continuing source of information on various specialties; several techniques have been comprehensively reviewed each year. The reviews, now in their third year, are similar in coverage to the Critical Reviews i n Analytical Chemistry ( 0 - 3 4 ) ,published by Chemical Rubber Company, now also in their third year of publication. Numerous other surveys and reviews of a less periodical nature have appeared in recent years and supplement the comprehensive treatments offered by the somewhat older, well-known treatises edited by Kolthoff and Elving ( 0 - 2 9 ) and Wilson and Wilson ( 0 - 6 4 ) . The works edited by Gouw ( 0 - 1 8 ) ,Kane ( 0 - 2 4 ) , Kirkendale ( 0 - 2 7 ) ,Richardson and Peterson ( 0 - 4 5 ) ,and Walsh (D-58) are among the most recent collected monographs presenting surveys of the various analytical techniques used for the analysis of inorganic materials. Similar works have been published in German ( 0 - 3 0 )and Italian ( 0 - 5 2 ) . A series published by the Medical and Technical Publishers (MTP) includes a two-part volume, edited by West, on analytical techniques ( 0 - 6 0 ) . In addition a number of textbooks ( 0 - 4 1 , 0 - 4 7 , 0-56, 0 - 6 3 ) ,primarily intended for the instruction of undergraduates, have also proved useful for the rejuvenation and modernization of obsolescent analysts.
ANALYTICAL TECHNIQUES This review is divided into 3 major sections which discuss respectively, developments in general analytical techniques, methods for the determination of the individual elements, and applications of the techniques to the analysis of various inorganic and geological materials, and related topics. Sample Decomposition Techniques. Sample decomposition techniques are still a subject of concern for those procedures, such as atomic absorption spectrometry, which are based upon aqueous solutions of samples. New metallurgical refractories and refractory minerals for which few suitable decomposition techniques are available, continue to keep the subject under active investigation.
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Joseph I. Dlnnln is a research chemist on the staff of the US. Geological Survey where, until recently, he directed the Analytical Services and Research Project in Washington. He has been employed in the Federal Service since graduation from Brooklyn College in 1942 and after Army service, and, with concomitant graduate study at the University of Maryland, has also been employed at the National Bureau of Standards and the U.S. Bureau of Mines. His interest in analytical geochemistry has included research studies in the analytical chemistry of niobium and tantalum, platinum metals, chromium minerals, and work in flame emission, absorption, and fluorescence spectrometry.
The Teflon lined bomb developed by Bernas (16) is commercially available (42, 138, 190) and is finding increasing application for decomposing materials such as uranium ores (137),coal ash ( 8 3 ) ,and high purity materials (184). A similar vessel manufactured in the USSR has been used for decomposing refractory silicates such as tourmaline, sapphirine, and staurolite (146). The device appears to be especially useful for decomposing refractories in which volatile trace constituents are to be determined. T h e generation-old sealed tube technique has been reviewed for the pressure dissolution of platiniferous materials (115). Although the work pre-dates the nominal time period of this review, a short book by Dolezal et al. ( 0 - 1 3 ) should be called to the attention of more inorganic analysts. The book did not fit under the subject headings of previous reviews. A number of laboratories find it a most useful source of information on the various techniques of decomposition that are available. Among developments in decomposition is the advocacy by Mulder (128) of the use of selenium dioxide as a solvent for the decomposition of refractory oxides. Tantalum and niobium pentoxides were found to be directly soluble while chromic oxide and alumina formed crystalline pyroselenites of low solubility; iron, indium, zinc, cadmium, lead, and silver oxides all formed extremely soluble pyroselenites. A Teflon apparatus, designed by Mitchell and Nash (123) should be useful for the contamination-free vapor phase destruction of silicate materials. Separation, Extraction, and Concentration. With continued need for methods for trace and ultra-trace analysis, there has been a continued interest in methods of separation and preconcentration. Interest has been sufficient to stimulate the publication of a journal devoted t o separation science. A critical overview by Irving (89) of many of the methods of separation includes a number of lesser known techniques such as froth flotation, reverse osmosis, resolidified solvents, liquified gases, the use of substances such as diantipyrylmethane to give two organic phases, and novel packings for gas chromatographic separations. An impressively sized book by Korkisch ( 0 - 2 8 ) presents a great deal of information on the separation of a number of the rare elements. The methods of separation discussed for each element include cation and anion exchange, various chromatographic methods, solvent extraction, coprecipitation and, where applicable, distillation; references are grouped a t the end of each separation technique. The elements discussed are the following: actinides; rare earths; lithium, rubidium, cesium, francium; beryllium; gallium, indium, thallium; germanium; selenium, tellurium, and polonium; silver; gold; titanium; zirconium and hafnium; va-
nadium; niobium and tantalum; molybdenum and tungsten; technetium and rhenium; and the platinum metals. Among the more unusual separation schemes that have been proposed is that of solid extraction employing molten organic compounds. Flaschka and coworkers (60) have described a variation called homogeneous extraction in which an organic complex that is miscible with aqueous solutions a t higher temperature is immiscible a t lower temperatures. G a s Chromatography. The applications of gas chromatography in inorganic analysis are as yet rather limited. However, the potential for high selectivity and sensitivity are sufficiently high for a number of determined investigators to continue study of the method. Inorganic gas chromatography is included in the general review of GC by Juvet and Cram in the 1974 Fundamental Review (98) and a review by Rodriguez-Vazquez includes 190 references to recent work in the subject (155).Two reviews in Russian have provided 300 references to work done in the period 1963 to 1970 ( 7 ) and 238 references to work on organometallic compounds during the period 1960-1972 (39). More recent developments are discussed by Barratt (12).A book by Guichon and Pommier ( 0 - 2 0 ) has been translated from the French and gives a comprehensive survey of the technique. Among the chromatographic techniques, gel chromatographic separations of inorganic compounds have been surveyed in a review with 120 references (206) and extraction chromatography of inorganic compounds has been reviewed in a Japanese publication (102). Among recent interesting applications of gas chromatography is its use for the analysis of the gaseous components in mineral occlusions (121). The inclusions provide valuable information on the conditions under which the mineral was formed. The technique might also find use for similar applications in metallurgical analysis. Ion Exchange. Inorganic applications of ion exchange have been reviewed by Walton in the 1974 Fundamental Reviews (195). A most useful table lists the element of interest, the elements or compounds from which it is separated, the exchanger, eluant, elution order, and reference. Liquid ion exchangers are considered to be solvent extraction and are but briefly mentioned. The Society for Analytical Chemistry’s Selected Annual Reviews of Analytical Science, also contains a useful chapter by Vernon on developments in ion exchange ( 0 - 3 ) . Reviews in Russian (174), and German (88) have also been published. Among interesting applications are the separation of iron(I1) from iron(111) in the presence of various complexing agents (208). The uses of liquid ion exchangers in inorganic analysis have been reviewed by Green (77) and includes more than 100 references to material published since his prior review in 1964. Applications of liquid ion exchangers include their use in the determination of trace elements in soils and 5 standard rocks (157). Solvent Extraction. Solvent extraction was last reviewed in Analytical Chemistry in the Fundamental Review of 1968 (69). Although numerous other reviews and books have appeared in the literature since that time, the most useful tables provided by Freiser are sorely missed. Among the more recent reviews is that by Stary (172) in the M T P Reviews of Physical Chemistry. A book by Zolotov on the extraction of chelate compounds ( 0 - 7 2 ) is now available in a most useful English edition. Among reviews of selected subjects, there have appeared a study on the extraction of iodide complexes (148) and a review of the extraction of transition metals with mesityloxide (165). A book by Blyum ( 0 - 7 ) on extraction photoA N A L Y T I C A L CHEMISTRY, VOL. 47, NO. 5, APRIL 1975
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metric methods using basic dyes summarizes progress in these combined fields. Organic Reagents. Current interest in high purity materials and trace contaminants has stimulated the search for new organic reagents and their use for the separation and determination of inorganic constituents. A number of reviews and books have comprehensively surveyed recent progress. Ueno (189) in a review with 271 references has surveyed the literature from 1968 to 1971. In addition to developments in new reagents, he summarizes progress in the use of combined reagents and provides a number of useful tables that facilitate the search for specific reagents or combinations for determining individual elements. A book by Burger ( D - 8 ) includes theoretical considerations of selectivity and detailed discussion of the application of selective reagents to the various analytical techniques., Approximately 100 pages of summarizing tables ease the search for information on specific reagents or information on reagents available for the various elements. Approximately 500 references are provided. Other reviews have been made by Belcher ( 1 8 ) and Pilipenko and Volkova (143, 144). Pilipenko and Tananaiko (142) have surveyed the literature from 1966 to 1970 on ternary or mixed complexes. Numerous convenient tables are provided. A new series of monographs on analytical reagents is being prepared by staff members of the Vernadskii Institute and published by the Science Council on Analytical Chemistry of the USSR. The first monograph, by Nazarenko and Antonovich, is on trihydoxyfluorones (132). The publication of a continuing series of collected monographs, edited by Flaschka and Barnard ( D - 1 6 ) summarizes information on a variety of chelate related topics including 2-pyridylazo compounds, applications of chelates to flame spectrometry, extractive titrations, and amperometric titrations involving chelates. A review of the use of masking agents, both organic and inorganic, was prepared by Yurist (207) and provides 278 references that cover the period from 1950 to 1970. Electrochemical Analysis. A recent review of instrumentation in analytical chemistry speaks of “The Renaissance in Polarographic and Voltammetric Analysis” ( 6 1 ) and indeed there appears to be a revival of interest in the application of techniques such as differential pulse polarography and anodic stripping voltammetry to inorganic analysis. The revival appears to be concurrent with the availability of several sophisticated commercial instruments which, it is claimed, can perform a t least 15 electrometric analytical techniques. In addition to the Fundamental Reviews in this journal and the aforementioned article. a number of reviews summarize progress in this field. In the M T P Reviews, Hulanicki ( 8 7 ) has reviewed general electrochemical methods and presented several useful tables on applications of stripping voltammetry, and 411 references to recent work in the field. Pyatnitskii (149) has reviewed progress in polarographic analysis from 1968 to 1972 and has included 9 pages of tabular information and 212 references. Copeland and Skogerboe ( 4 3 )have reviewed anodic stripping voltammetry as have Fleet and Jee ( 5 9 ) . A discussion of ASV by Ellis ( 5 3 ) includes a survey of available commercial instrumentation. A collection of monographs ( A - 2 ) summarizes much of the recent knowledge on the electrochemistry of the individual elements. Ion Selective Electrodes. Ion selective electrodes (ISE) are assuming an increasing role in inorganic analysis as the l00R
number of commercially available electrodes increases. More than 20 electrodes or electrode types are available and they appear to be enjoying widespread use. The fluoride electrode has proved to be especially valuable in geochemical analysis for the determination of fluoride as it has been found possible completely to eliminate the need for laborious distillations. Ion selective electrodes are included in the review of potentiometry, in the Fundamental Reviews ( 3 3 ) . Additional reviews have been prepared by Tengyl (181) who cites 316 references, Wilson (201),Durst ( 5 1 ) ,Clerc ( 4 1 )and Staroscik (171). Among the more unusual electrodes is a perrhenate selective electrode based upon a liquid ion exchanger and aqueous layers separated by a cellophane film ( 7 6 ) . The electrode has a linear response to 10-6M Re 04-and no interference was noted by excess C1-, S042-, MOO^^-, NOS-, VOa-, clod-. Light Absorption Spectrometry. Inorganic applications of light absorption spectrometric methods through November 1973 have been reviewed by Boltz and Mellon in the 1974 Fundamental Reviews ( 2 9 ) .Elements are tabulated alphabetically with the material analyzed, the method, reagent, wavelength, molar absorptivity, and reference. Kinetic spectrophotometric methods are also reviewed. Similar tabulations of spectrophotometric methods in the previously cited reviews of Pilipenko and Tananaiko (142)and Pilipenko and Volkova (143, 144) increase the chances that significant and useful procedures will come to the attention of more analysts. Far ultraviolet solution spectrophotometry has been reviewed recently by Fox ( 6 6 ) . Fluorescence a n d Chemiluminescence. Interest in fluorometric methods of analysis has continued to increase although organic applications appear to be increasing faster than inorganic. From the relative volumes of papers on the subject, interest in the USSR appears to be greater than that in other countries. A number of useful books are now available on the subject possibly indicating a general maturation of the field. Among recent books are those by Parker ( 0 - 4 0 ) and Winefordner et al. ( D - 6 5 )which primarily deal with theoretical considerations and books by Guilbault (D-19) and White and Argauer ( 0 - 6 2 )on practical aspects. In addition to the comprehensive review by Weissler (197) in the 1974 Fundamental Reviews, photoluminescence and chemiluminescence have been reviewed by Bark and Wood ( 8 ) ,chemiluminescence and bioluminescence by Seitz and Neary (163),practical application of chemiluminescence by Isaacson and Wettermark ( g o ) , and general molecular fluorescence spectroscopy by Guilbault ( 7 9 ) . A Polish review surveys both spectrofluorimetric and spectrophotometric methods used in trace analysis ( 9 9 ) . There are now more than 30 organic reagents that can be used to produce fluorescent species useful for analysis and the number is gradually increasing. The search for new reagents and the attempt to increase the sensitivity of known reactions appears to have stimulated interest in the study of low temperature reactions. Much of this work was reviewed by Solov’ev and Bozhevol’nov (168). Among other interesting developments in this field have been the interest in solid state luminescence whereby many elements which do not form luminescent chelates in solution can be made to form luminescent phosphors when incorporated into the crystal lattice (156). In another unusual application, titration, extraction, and fluorometry have been combined into a procedure more
ANALYTICAL CHEMISTRY, VOL. 47, NO. 5 , APRIL 1975
sensitive than the individual methods for the determination of trace amounts of certain metals ( 1 5 4 ) . Activation Analysis. Neutron activation appears to have matured as an analytical technique and has become especially useful in applications where sample or reagent contamination is t o be minimized. The high sensitivity and specificity of the technique have made it most useful for trace analyses and recent advances in instrumentation have made possible the simultaneous determination of numerous elements with a minimum of sample processing. Major recent advances and publications have been presented in the Fundamental Reviews (114);Lyon (113) has also critically and amusingly reviewed three meetings a t which were presented numerous applications of activation analysis. A book by DeSoete, Gijbels, and Hoste ( 0 - 1 2 ) in addition to basic principles, presents an extensive bibliographic survey of the field and extensive referenced tables of applications. Additional reviews have been prepared by Pierce (1411. Radioactive tracers (186, 209), radiometric titrations (1861, and general radiochemical methods (50, 131) have also been reviewed. Isotope Dilution Analysis. Isotope dilution analysis using radioactive tracers has continued to be useful for reactions in which complete isotopic exchange can be established. Numerous procedures are tabulated by element in a recent monograph (0-50) by Tolgyessy and others. Information on the matrix, tracer, amount determined, separation process, yield determination, and reagent are conveniently available. Isotope dilution techniques using substoichiometric analysis have been reviewed by Stary and Ruzicka (173)as have the use of chelates as reagents in substoichiometric separations ( 2 5 ) . A review by Tolgyessy (186) contains almost 500 references to recent work. Kinetic and Catalytic Methods. Although they do not find widespread use, kinetic methods serve a special need in inorganic analysis where alternative methods are inapplicable or unavailable. For instance, they are especially valuable for the determination of osmium and ruthenium. Inorganic application of kinetic analysis are included in the Fundamental Review by Greinke and Mark ( 7 4 ) ; a comprehensive survey of the field has been presented by Guilbault ( 7 8 ) as part of the M T P Reviews; catalytic methods are treated separately by Yatsimirskii in the same publication (205), and by Svehla (176). Mark has reviewed many of the factors affecting the accuracy and precision of kinetic-based analytical methods (117). Thermal. Thermal methods of analysis have continued to play an important role in the characterization of minerals and studies of inorganic compounds. Although not directly used for elemental analysis, thermal methods have played an important role in determining the purity of reagents, precipitates, and numerous other uses. A book by Daniels ( 0 - 1 0 ) discusses most of the thermoanalytical techniques including thermogravimetry, differential thermal analysis, differential scanning calorimetry, dilatometry, mechanical, electrical, and magnetic methods in thermal analysis, evolved gas detection analysis, and combinations of various techniques. Reviews of various techniques in thermal analysis have been prepared by Murphy in the 1974 Fundamental Reviews (130), and by Wendlandt (198);reviews of thermometric and enthalpimetric titrations have been prepared by Bark ( 9 ) , Bark et al. (IO),Beezer ( 1 4 ) , and Hansen et al. (82).
Titrimetric Methods. Practicing wet analytical chemists will be grateful t o the Society for Analytical Chemistry for publication of the first in their series of Analytical Sci-
ences Monographs which is a booklet by Woodward and Redman ( 0 - 6 8 )entitled “High-Precision Titrimetry”. The monograph gathers in one convenient place information on many of the techniques required for performing titrations with a precision better than 0.1 percent relative. Although visual titrations are stressed, guidance is also provided for performing titrations by photometric or electrometric methods. In a period when recent graduate chemists are fortunate to have been introduced to a buret, it is reassuring to have a booklet such as this available for instruction and as a refresher. This monograph supplements the monograph of Wagner and Hull ( 0 - 5 7 ) in presenting a contemporaneous view of inorganic titrimetry. Some unusual end-point detection methods are discussed by Curran in a monograph on new developments in titrimetry ( 4 6 ) . Among the novel methods discussed are pressuremetric, cryoscopic, phase, and flame photometric titrations. Among other significant publications on titrimetry were a discussion by Johansson ( 9 7 ) of the choice of indicators in photometric titrations and a discussion by Berka and others ( 1 5 ) of the various factors that influence the usefulness of titrimetric methods. Among major publications related t o titrimetry is the latest in the series of monographs on Analytical Chemistry edited by Belcher and Freiser. The book, edited by Bishop ( 0 - 6 ) ,is itself a collection of monographs and in more than 700 pages appears to tell the analyst everything that he had ever wanted to know about indicators. Along with elaboration of the history and principles of visual indicators, are discussions of the various types of acid-base indicators, including organic dyes, nonaqueous acid-base titrations, titrations with non-chelating liquids, metallochromic, metal, adsorption, and oxidation-reduction indicators, including those with high formal potential, and fluorescent and chemiluminescent indicators, Photochemical Techniques. Various applications of photochemical techniques to analytical chemistry are reviewed in a collection of monographs edited by Fitzgerald (63); the techniques include photochemical titrations in which photochemical reactions are used for titrant generation ( 6 4 ) ,photochemical pretreatment (151), and the use of lasers in analytical chemistry ( 7 0 ) . A general survey by Peter and Csanyi (140) includes a discussion of photocatalytic methods, photochemical indicator reactions, photogravimetric and photodissociation methods. Flame Spectrometry. If volume of literature can be used as a measure of popularity, flame spectrometric methods, and especially atomic absorption techniques, are the current most used methods in inorganic analysis. Winefordner and Vickers (202) have culled more than 800 references from a total of more than 2000 articles published in a 2-year period and cite almost 100 reviews, books, and bibliographies published during that time. If it is assumed that 10,000 articles on inorganic analysis are published per 2-year period, the literature devoted to flame spectrometry represents approximately 20 percent of the total. Developments in flame spectrometry thus play a major role in documenting progress that has been made in inorganic analysis. For a review of recent developments in this major aspect of analytical technology, a reader is advised to begin by referring to the comprehensive 1974 Fundamental Review by Winefordner and Vickers in which literature through 1973 is critically documented, classified, and tabulated. There are presented a number of useful tables listing the elements by order in the periodic table, the matrix in which the elements exist, the flame where applicable, and refer-
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ence. Included are tables of applications of flame atomic emission, flame molecular emission, indirect methods using flame emission, flame atomic absorption, indirect methods using atomic absorption, applications of microsampling techniques, applications and flame atomic fluorescence, and flameless atomic fluorescence. The tables greatly facilitate the search for individual topics in flame spectrometry. The Society for Analytical Chemistry’s Annual Reports on Analytical Atomic Spectroscopy, ( 0 - 2 2 , 0 - 6 7 ) are another extremely useful and continuing source of information on inorganic applications of flame spectrometry. The latest volume contains almost 1700 references to work received during calendar 1973. The reports include numerous tables listing the elements in alphabetical order and giving information on the material analyzed, concentration range, the technique, the form of the sample, a brief indication of the sample pretreatment, atomization process, and reference. Separate tables list the procedures for the analysis of metals; chemicals; oxides, ceramics, slags, and cement; minerals; soils, plants, and agricultural products; environmental studies and other fields. The Atomic Absorption Newsletter (167) is a continuing source of new and useful information on AAS and provides a convenient semi-annual bibliographic summary; their most recent total for such entries is 4091. Publications are cross-indexed by area of application and elements determined. In metallurgical analysis, a Soviet review, available in translation, conveniently summarizes papers published between 1966 and 1971 on the AAS analysis of steels and alloys (101). Among more recent reviews is that of Massmann (118) which includes a survey of furnace methods in AAS, as does a recent review by Woodriff (203). The Third Theophilus Redwood Lecture, delivered by West ( 2 0 0 ) ,includes a survey of new developments in atomic fluorescence spectrometry; a review by Browner ( 3 1 ) contains more than 200 references to work in AFS. Among interesting developments in atomic fluorescence spectrometry are the first reported applications of non-dispersive AFS by Norris and West (135) for the determination of Zn in soils and alloys and by Tsujii and Kuga (188) for the determination of arsenic. The prolific school of analytical chemistry a t the University in Birmingham has in recent years devised a new flame analytical technique which they have named Molecular Emission Cavity Analysis (MECA) and which appears to be extremely useful for determining trace amounts of many metals and nonmetals. The technique employs a small cavity a t the end of a rod into which samples are deposited. The cavity is introduced into a flame in line with a detector and the resulting emission is recorded. The technique has thus far been applied to the determination of sulfur (221, selenium and tellurium ( 2 4 ) , boron ( 2 3 ) , and arsenic and antimony ( 2 1 ) .A review has also been published ( 2 0 ) . Possibly the most exciting development in applied flame spectrometry in recent years has been the development and subsequent commercial availability of graphite furnaces and the possibilities they hold for the trace analysis of many materials. Numerous reviews and critical studies have appeared on the use of the graphite furnace for nonflame atomization ( 4 , 45) and the technique is enjoying ever wider use. The furnace is being used for direct atomization of rock samples for the determination of numerous elements (E-26-E-28), for the determination of antimony in steel ( 6 7 ) ,determination of trace elements in high purity glasses and their raw materials (71), combined with electrodeposition for the determination of a number of elements 102R
in salt solutions (96, 201), and numerous other applications. Among other exciting developments in flame spectrometry is the use of the videcon tube as a detector and the possibility this holds for the simultaneous determination of numerous elements. Mitchell, Jackson, and Aldous (122) have described some of their work with a silicon-target tube for multielement atomic absorption spectrometry and Busch, Howell, and Morrison ( 3 5 ) have described a flame emission instrument. Among other developments in AAS have been the use of hollow cathode emission for the determination of sulfur, iodine, arsenic, selenium, mecury (101) and boron ( 4 7 ) ;improvements in the determination of the noble metals (193) and the rare earths (182). X-Ray Spectrometry. New developments in X-ray absorption and emission have been reviewed by Birks and Gilfrich ( 2 6 ) in the 1974 Fundamental Reviews; recent books and reviews are listed in an appendix to their references. A review by Jenkins ( 9 5 ) in the M T P Reviews, lists 460 references to recent literature. X-Ray techniques are among the methods outlined in a recent survey of modern methods of geochemical analysis (B-15). X-Ray fluorescence (XRF) analysis is becoming increasingly useful for the almost complete analysis of metallurgical products, rocks, and minerals and as a supplemental technique for determining elements not readily amenable to wet chemical analysis. The comparative results obtained by Fabbi (E-11) indicate that silicate rocks can be quantitatively analyzed by XRF spectrometric methods with a precision comparable to that achieved by routine wet chemical techniques. With the use of multiple detectors, automatic sample changers, and computer assisted read-outs, the dream of push-button rock analysis is rapidly approaching reality. In the analysis of lunar materials, XRF, emission spectrometry, and wet chemical techniques have been combined into analytical systems of high accuracy (E-15, E 16).
Emission Spectrometry. Barnes comprehensive review of emission spectrometry (ES), through 1973 ( 1 1 ), includes a survey of trace element analysis, rare earth and actinide determinations, isotope analysis, and analysis of metals, nonmetals, and geological materials. Included are several tables listing alphabetically the materials or matrix analyzed, elements sought, and references. Emission spectrometry is now used for the computer spectrographic analysis of rocks, including both major and minor elements (E-IO, E-23, E-51). As adjunct to wet chemical methods, ES is still most valuable for a rapid semiquantitative survey of the elements present in material prior to quantitative determination of the individual elements. It is especially useful where only small amounts of material are available. Recent developments in emission spectrometry have been discussed in several books ( 0 - 3 6 , 0 - 4 8 ) and monograph collections ( 0 - 2 7 ) . Mass Spectrometry. Where the highest accuracy in trace analysis is required, analysts are increasingly turning to mass spectrometric-isotope dilution techniques. This is evidenced by the use of the techniques in geochronology, determination of trace constituents of lunar samples, and characterization of trace constituents of standard samples. Although inorganic applications of mass spectrometry are not included in the 1974 Fundamental Reviews, a survey of current progress in the field has been made by Robertson (152) and is included in the M T P Review of Science. A review by Weber and Deines (196) is included in a discussion of modern methods of geochemical analysis. Morri-
ANALYTICAL CHEMISTRY, VOL. 47, NO. 5, APRIL 1975
Table I. Selected Books, Monographs, and Review Articles on the Analytical Chemistry of the Elements References
References Element
Actinium Actinides Aluminum Americium Antimony Arsenic Astatine Berkelium Beryllium Bismuth Boron Bromine Cadmium Californium Cerium Cesium Chlorine Cobalt Curium Einsteinium Fluorine Francium Ga 11ium Germanium Gold Hafnium Indium Iodine Iridium Lanthanum Lithium Magnesium Mer cur y Molybdenum
Books or chapters
Articles
( A-26) (159) (A-24, 4 6 ) ( A-26) ( A-5)
( A-5) ( A-20) ( A-26) (A-8, 33) ( A- 8 ) ( A-31) ( A- 5 ) ( A-42)
( A-26) ( A - 8 , 40) ( A-8) ( A-5) ( A-38) ( A-26) ( A-26) ( A - 5 , .32) ( A-20) ( A - 8 , 10) ( A - 8 , ,301 (A-3, 6 ) ( A - 8 , 22, 27) ( A-8) ( A-5) ( A- 3 )
(160) (91)
( 178)
( A-8) ( A- 8 ) ( A-45) (94, 150, 161)
Element
Books or chapters
Neptunium Nickel Niobium Osmium Oxygen Palladium Phosphorus Platinum and platinum metals Plutonium Potassium Protactinium Rare earths Rhenium Rhodium Ruthenium Scandium Selenium Si1icon Silver Sulfur Tantalum Technetium Tellurium Thallium Thorium Titanium Tungsten Uranium Vanadium Yttrium Zirconium
( A-22) (A-21, 36) (A-8, 11, 1 6 , 25) ( A-3)
Articles
(13, 48, 56, 78, 139, 179, 183) ( A - 2 3 , 26) ( A-18) ( A-35) (A-8, 40) (A-8, 9 ) ( A-3) (A-1, 3 ) ( A-8) ( A - 8 , 29) ( A-28)
( A-5) (A-8, 11, 16, 25) ( A-20) ( A - 8 , 10, 29) ( A - 8 , 19) (A-8, 39) ( A-8) ( A - 8 , 13) ( A - 8 , 34) (A- 8 ) ( A - 8 , 40) ( A - 8 , 12, 27)
( A - 7 , 8 , 13)
son and Roth (127) have included a review of the mass spectrometric analysis of inorganic and geological materials in a collection of monographs on mass spectrometry. Among recent interesting articles on mass spectrometry is a review by Fenselau ( 5 7 ) of the current state of development of combination gas chromatograph-mass spectrometers. In a review of the applications of spark-source mass spectrometry to the steel industry, Wrigley (204) discussed some of the advantages and problems of the techniques. Mass spectrometry was particularly useful for the determination of the individual rare earths in steel intended for oil and natural gas pipelines.
ANALYSIS OF THE INDIVIDUAL ELEMENTS Only in recent years have there been available a number of monographs and major chapters of compendia summarizing much of the existing knowledge of the analytical chemistry of the individual elements. Until about 20 years ago, analysts resorted to a handful of books such as the well known works of Hillebrand, Lundell, Bright, and Hoffman (EM),Lundell, Hoffman, and Bright ( B - 9 ) ,Groves ( B - 5 ) , and Sandell ( B - 1 3 ) . In more recent years, the individual chapters in the compendia edited by Kolthoff and Elving ( A - 1 7 ) summarized the literature up to approximately 1965 on the determination of the individual elements. This work was supplement-
ed by the book by Pinta ( A - 3 7 )on metals and by Boltz ( A 5 ) on non-metals. As the present time, there are available a number of monographs summarizing current knowledge of the analytical chemistry of the elements, many prepared by analysts a t the Vernadskii Institute of Geochemistry and Analytical Chemistry, USSR Academy of Sciences. The original works were published in Russian in the later 1960’s; English translations were made by the Israel Program for Scientific Translations, Jerusalem, and beginning in 1971 were published by Ann Arbor-Humphrey Publishers, Michigan. They are presently distributed by the Halsted Press Division of John Wiley and Sons, Inc. These works appear to be expansions by many of the same authors of a rather comprehensive work on the analytical chemistry of the rarer elements, published in 1962 ( A - 4 8 ) .The English translation was also published by the Israel Program on Scientific Translations, Inc. for the National Science Foundation and is available from the Office of Technical Services, U.S. Dept. of Commerce. At the present time, there are available 26 volumes representing a majority of the elements including the rare earths, and actinides. Inasmuch as most newly published work is merely an elaboration or modification of previously existing procedures, the Vernadskii monographs, although originally published 6 to 8 years ago, are still close to the state of the art. However, where major instrumental or
A N A L Y T I C A L CHEMISTRY, VOL. 47, NO. 5, APRIL 1975
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other advances have been made in recent years, the monographs are seriously out of date and are of only historical interest. For instance the monograph on fluorine, ( A - 3 2 ) , although originally published in 1970 and translated in 1973, makes no mention of ion selective electrodes and neglects some of the most popular current spectrophotometric procedures. Table I lists alphabetically by element many of the recent books, chapters in compendia, and review articles that have been published on the analytical chemistry of the individual elements. The monographs and major chapters are assembled in Appendix A to the references. In addition to the works cited in Table I, several other useful encyclopedic works provide useful summaries or descriptions of methods used for each of the elements. Although primarily directed to the analysis of soil ( A - 4 ) , (A44), or other fields, the procedures can readily be adapted for use for the analysis of numerous materials. Snell and Ettre’s Encyclopedia of Industrial Chemical Analysis (A-43) contains much information on the determination of the elements as well as the analysis of industrial and commercial materials and should update the invaluable Standard Methods of Chemical Analysis, edited by Furman and Welcher (A-15,B-20). The Fundamental Reviews are also a major source of useful information on recent advances in the analytical chemistry of the individual elements. The sections on the individual techniques contain numerous tables of references, arranged by elements, to the determination of the elements. For instance, Winefordner and Vickers’ section on Flame Spectrometry (202) contains more than 250 tabular references to flame spectrometric methods; Boltz and Mellon’s section on light absorption spectrometry (29) contains more than 600 references to individual procedures. Among other useful reviews is a survey by Lisk (110) of procedures used for the determination of toxic elements. A convenient table provides references to numerous methods recently published for the determination of each of more than 20 elements. Anions. Although primarily directed to the analysis of water, a paper by Boltz (28) presents a useful review of methods available for the determination of anions. The review is a report of part of a symposium on the subject presented a t the 1971 Eastern Analytical Symposium. Another review appears in the Critical Reviews of Analytical Chemistry (27). The use of indirect methods in atomic absorption spectrometry has been reviewed by Kirkbright and Johnson (103). Although also applicable to cations, the techniques are primary useful for anions and non-metals. The use of basic dyes for the determination of anions was reviewed by Fogg and coworkers (65). The dyes were particularly useful for the determination of antimony, thallium, and gallium. Purification methods and other uses of the dyes were also discussed. AREAS OF APPLICATION Analysis of Metallurgical a n d Industrial Products. Table I1 lists the subject and reference number of selected recent books and articles that review methods used for the analysis of various metallurgical and industrial products. The books are listed alphabetically by author in Appendix C to the reference. Other review articles and books describing specific techniques or applications can be found in the respective sections of the Fundamental or Applied Reviews; an attempt was made to avoid duplication with items to be found there. Numerous recent specific applications to inorganic anal104R
ANALYTICAL CHEMISTRY, VOL. 47,
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Table 11.Books and Review Articles on the Analvsis of Metallurgical a n d Other Industrial Products
-
BCOh Subject
References
Barium and sulfite salts ASTM; Chemical analysis of metals Phosphorus, phosphoric, acid and fertilizers Structural composites Construction materials; spectro graphic analysis Ferrous metals, alloys and steel Nonferrous metals and alloys Refractory compounds Treatise on analytical chemistry, Part I11 (analytical chemistry in industry)
(C - 1 ) (C-2, 1 5 )
(C-3, 10, 1 3 ) (C-11, 14) (C -12) ( C -7)
Review Artlcles
General manufactured products, methods Blast furnace slag; rapid wet met hods Iron ore; official Romanian methods Foundries; annual review of methods Metallurgy; chemical and phys ical methods Coal mine dust Phosphoric acid; raw materials and intermediates Portland cement Ferrovanadium; AAS Metallurgical analysis; AAS, SiOz Steel and alloys; AAS Ferrous alloys; XRF Ferrous metals; emission spec trometry
(93)
( 158)
(38, 44)
ysis are listed conveniently in the many tables in the Fundamental and Applied Reviews. Analyses are arranged by elements determined and material analyzed. Comprehensive information on specific applications is readily available from the biweekly and yearly indexes of Chemical A b stracts and yearly abstracts of Analytical Abstracts. This past year has marked the near completion of publication of Snell and Ettre’s 20-volume encyclopedia of industrial chemical analysis (A-43). Beginning in 1966, the individual volumes have been published intermittently and now provide an excellent source of information on the analytical chemistry of specific elements, specific techniques, or the analysis of specific materials. Part I11 of Kolthoff and Elving’s “Treatise on Analytical Chemistry” ( A - 1 7 ) is to be directed to the analysis of industrial materials as is Volume IV of Wilson and Wilson’s “Comprehensive Analytical Chemistry” ( 0 - 6 4 ) . Unfortunately, except for an introductory volume on general considerations, neither treatise has as yet published volumes in this phase of applied analysis. Geological Materials. Developments in the analysis of geological materials have paralleled progress in the analysis of inorganic materials in general. The instrumental invasion has so engulfed this area of analysis that it is becoming rare to find evidence of recent new work on new gravimetric procedures.
APRIL 1975
Table 111. Selected Recent Books a n d Monographs
on Analytical Techniques Subject or title
Atomic absorption spectrometry in geology Annual reports on analytical atomic spectroscopy Ion selective electrodes Indicators Organic reagents in inorganic analysis Photometric analysis Extraction photometric methods using basic dyes Extraction of chelate compounds Activation analysis with neutron generators Neutron activation analysis Nuclear physics methods for analysis of mineral raw mate rials Thermal analysis Decomposition techniques in inorganic analysis Separation of r a r e r elements Trace analysis: methods for separation and concentration Ascorbinometric titrations Trichromatic colorimetry Chelates in analytical chemistry Thin layer chromatography Gas chromatography i n inorganic chemistr y Soil science: principles and practice New developments in titrimetry Introduction to separation science High precision titrimetry Modern methods for the s e p a r a tion of r a r e r metal ions Accuracy in spectrophotometry and luminescence Ion exchange and solvent extrac tion Determination of gaseous ele ments in metals Radiochemistry Analytical applications of EDTA Isotope dilution analysis Fluorescence analysis: a practical approach Luminescence Emission spectroscopy
Reference
(D-1)
(0-72) (0-38) (0-51) (0-70)
(D-10, 59) (0-13)
(D-28) (0-37, 49) (0-14) (D-15) ( D - 1 6 , 72) (0-55) ( D -20) (0-21)
(D-23, 2 6 ) (D-25) (0-68) ( D -28)
( D -32) (0-31) (0-35)
( D -39) (D-43) (D-50, 51) ( D - 1 9 , 62) ( 0 - 4 0 , 65) ( D -1 7 , 36, 4 8 )
As this is the first of the Applied Reviews t o include specific discussion of the analysis of geological materials, an attempt has been made to include significant older publications which may have escaped citation in previous applied reviews (Table 111). Many of the current, most used, books on rock and mineral analysis are included in the list of recent books appended to the references. Several older works are included because they still describe the current state of the art and no newer replacements or additions have as yet appeared. Mineral Analysis. The history and current state of min-
eral analysis has been delightfully and comprehensively reviewed by Hey (86) who traces the art from its origin in the 1770’s t o recent years. He discusses the evolution of the analytical techniques applied to mineral analysis and puts a stamp of approval on the use of the newer instrumental techniques, judiciously applied, for the determination of many elements in minerals. Table IV lists a number of the more general papers on geochemical analysis that have appeared in recent years. The publications are grouped by analytical specialty. Although the relative number of publications in each group may merely reflect the prejudice of the compiler, it is striking to note the overwhelming use of instrumental methods in a discipline nurtured in classical gravimetric techniques. L u n a r Materials. The analyses of the returned lunar samples have been termed the “greatest coordinated analytical effort in history” (0-71, p. 208) and probably represent the most extensive and intensive application, yet known, of current inorganic analytical techniques. The techniques vary from conventional gravimetric rock analysis methods to the most sophisticated instrumental techniques developed to this time. Descriptions of the methods probably represent the best overall view of applied inorganic analysis as it is practiced today. Detailed descriptions of the analytical techniques used on the returned lunar samples have been published in the Proceedings of the Lunar Conferences (E-15, E-16). The analyses include the following: major, minor, and trace elements including volatile light elements; various isotopic studies for age determination; rare gas analyses; and radionuclide determinations. A recent ASTM symposium attempted to provide an opportunity for those outside the lunar program to learn of some of the advances in methods and instrumentation resulting from the program. The resulting proceedings ( E - 5 ) describe some of the procedures used for sampling, contamination monitoring, mass spectrometric determination of volatiles, techniques for analysis of gases, infrared techniques, and determination of oxygen and rhenium. Prior to the availability of the Apollo samples, Mapper and Smales (116) reviewed many of the analytical techniques that would be useful for the analysis of recovered extraterrestrial materials. Hopefully, more such useful reviews will be available on the actual techniques used on the returned lunar samples. The Apollo program should receive this year’s medal for long distance X-ray spectrometric analysis. In an experiment devised by Adler, Trombka, and Gorenstein ( 3 ) , an X-ray fluorescence analysis was performed of approximately 20 percent of the moon’s surface using solar X-rays as an excitation source. Magnesium, aluminum, and silicon were determined by XRF; potassium, uranium, and thorium by gamma-ray spectrometry; radon and thoron were determined using an alpha particle spectrometer. Trace Analysis. Concern with environmental contamination and the characterization of highly pure materials has continued to foster interest in trace determinations and the special problems of sensitivity, selectivity, and contamination associated with such work. A recent book, entitled “Ultrapurity” ( D - 7 1 ) has conveniently gathered together much of the existing information on the special problems involved in trace analysis and is a most useful reference to have handy. In addition to individual chapters on the various analytical techniques, cited elsewhere, the book contains individual chapters on the purification of solvents, reagents, preparation of ultrapure water, contamination, airborne contamination, and glass, vitreous silica and ceramic containers used in analysis. A
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Table IV. Selected References on the Analysis of Geological Materials General method used
Material elements determineh, comment
Flame Rocks and minerals, alspectrometry kali and alkaline earths,part of complete scheme of analysis Rocks and minerals; lithium fluoborate fusion, complete scheme of analysis Silicate and carbonate rocks; trace elements General geologic; Na, K, Rb, Cs, Mn, Li, Ca, Eu, Sr, Ba, Al, Yb, Y, La, Gd, Sc; ovenflame atomizer Silicates; Si, Al, Fe, Mg, Ca, K, Na, Mn, C r , Ti, Cu, Zn; lithium metaborate fusion; lanthanum releaser Rocks and soils; Ag, Cr, Cu, Pb, Zn; thermal atomization; tantalum crucible, 2750 "C Silicate rocks; Be, V, Ba, Rb, Be; N , H , H , flame Silicates and sulfides; Si silicates; N 2 H , H , flame Fluorspar; Pb, Zn, Cu, Ca, Mg, Na, K Silicate rocks; Cd, Pb, Ag, T1, Zn; direct atomization Direct atomization; Rb, Cs, Ga, In Minerals and rocks; sodium peroxide sintering Silicate rocks; lithium metaborate fusion; fluoboric acid dissolution Silicate rocks; trace elements; graphite furnace; decomp. in Teflon-lined A1 bomb Rocks and minerals; trace elements Sulfide and silicate minerals; Si; Teflonlined bomb o r Na,O, fusion in Zn crucible Rocks and minerals; 14 elements; lithium fluoborate fusion Bastnasite, Monazite, adolinite; lanthanides and yttrium; AAS; nitrous oxideacetylene
lO6R
Reference
(E-1)
(E-2)
(E-22) (E-30)
(E-33)
(E-38)
(E-48)
(E-19, 47)
(E-9) (E-26)
(E-27, 28) (E-8)
(E-40)
(E-22)
(E-39) (E-19)
(E-2)
(E-36)
General method used
Material elements determineh, comment
X-Ray fluores - Aluminosilicate; Si, Al, cence specFe, Ca, K, P, Ti, Fe; Li,B,O, fusion trometry Rocks; As, Sb, Ni, Rb, Sc, V, Zn; chromatographic cellulose pellet Rocks; K, F1, Ti, Si, Ca, Al, Mg, P, Mn Rocks; Fe, Mn, Ti, K, P , Si, Al, Mg, Na, Li,B,0,-LiF fusion; double concentration method Rock forming minerals; Na, Mg, Al, Si, K, Ca, Ti, C r , Mn, Fe; electron probe Rocks and mineral analysis; application of mass absorption coefficients Rocks, soils, clay minerals Nondispersive Rocks and minerals; major elements; soft X-ray fluores lithium drifted silicon detector; multicence specchannel analyzer trometry Rock;, major elements; Electron milithium tetraboratecroprobe lanthanum oxide fusion Emission spec - Silicate rocks; Ba, Co, Cr, Cu, Ga, Mn, Ni, trometry Pb, Sc, Sr, V, Y, Zn Silicate rocks and minerals; effect of matrix elements on determination of C r , Mn, V, Ti, Cu, Ni, Co, Pb, Sr Silicates; Si by AAS; Na, K by flame emission; Al, Fe, Mg, Ca, Mn Ti, Ba, Co, Sr, C r , Cu, N i , V, Li Silicate rocks; major elements computer spectrochemical analysis; excitation and plate preparation, instrumentation, program description Combination Magnesites and doloscheme of mites; complete analanalysis ysis Tantalum and niobium minerals; Sr, Ti, Al, Fe, Mn, Ca, Mg, Na, K, Nb, Ta, Z r , Th, U , REE, F ; flame emission, spect r o phot., complexometric titration
ANALYTICAL CHEMISTRY, VOL. 47, NO. 5, APRIL 1975
Reference
(E-3)
(E-11)
(E-20) (E-49)
(E-29)
(E-32)
(E-18) (E-21)
(E-52)
(E-34)
(E-4)
(E-17)
(E-IO, 23, 51)
(E-7)
(E-31)
~~
Table IV. (Continued) General method used
Combination scheme of analysis
Material elements determineh, comment
Apatites; K, Na, Fe, Mn, Mg, Sr by AAS; Si and P by spectrophot. Micas; AAS, gran., t i t r . , plot, and thermal methods; complete scheme Ilmenite; A1 by complex. titr.; part of complete scheme Silicates; Fe, Al, Ti, Mn, Mg, Fe(I1) by spectrophot. ; Ca by complex. titr.; Na and K by flame emiss. Tourmalines; Ca, Mg, Fe, Mn, K, Na, Li, Rb, and Cs by AAS; Si, Al, Ti by spectrophot. Clay standards; complete and detailed procedures Magnesites, dolomites; major elements; gran. Silicate, carbonate, and phosphate rocks; complete rock analysis Lunar rocks and soils; major and trace elements; isotopes
General method used
Reference
Chemical and spectrophotometric
(E-35)
(E-14)
(E-25)
Miscellaneous
(E-46)
(E-45)
(E-42)
(E-7)
(E-44)
(E-14 24)
chapter by Robertson on contamination problems (153) contains numerous tables of information otherwise difficult to find; included is information on the trace element concentrations in various types of polyethylene; contamination after storage of water, sea water, and other solutions in various containers; contamination after evaporation of various acids in Teflon, platinum, and quartz dishes; trace-element concentrations in filter materials and papers; trace element concentrations in a variety of chemical reagents, acids, and chelating compounds; metal content of rubber and organic coatings. A chapter by Adams on glass containers contains much useful information that should be brought to the attention of anyone performing trace analysis in such containers. A comprehensive discussion of methods and problems of separation and preconcentration techniques in trace analysis has been presented by Tolg (184, 185). Included are a discussion of errors and their minimization, sources of contamination in the laboratory, contamination by reagents; a comprehensive tabulation and discussion of methods for decomposing inorganic materials for the determination of volatile and non-volatile constituents is also presented. Among the separation methods discussed are volatilization, precipitation, liquid-liquid extraction, ion exchange, and specialized procedures such as thin-layer chromatography, and gas chromatography. In discussing special problems in the analysis of high purity materials, Tolg describes various combinations of decomposition-determination procedures and reviews a number of novel apparatuses developed by him and his associates for special problems. Among other recent reviews of the determination of trace elements are discussions by Belcher (17-19) of new
Material, elements determined, comment
Rocks and soil; Si, Fe, A1 and Ti by spectrophot. Sedimentary rocks; W, Mo, Pb, Cu, Zn by extraction-spectrophot, Silicate rocks; major elements; gravimetric and titrimetric methods Basanite, anhydrate, and gypsum; quantitative analysis of mixture by infra-red absorption spec. Teflon apparatus for vapor phase destruction of silicates Rocks; La, Nd, Lu, Rb, Sb, Yb, Sc, C r , Co, Cs, Ce, Eu, Tb, Hf, Ta, Th; neutron activation analysis Comparison of AAS and conventional rapid methods of analysis of rocks Manganese nodules; r a r e earth elements; sparksource mass spectrometry
Reference
(E-41)
(E-50)
(E-37)
(E-12)
(123)
(E-43)
(E-6)
(E-13)
methods in which attention is directed to a revival of a technique called candoluminescence which may be useful for determining ppb concentrations of bismuth, manganese, antimony, lead, lanthanides, and other elements (187).Molecular emission spectroscopy in flames is recommended for highly sensitive determinations of arsenic, antimony, halogens, phosphorus, selenium, tellurium, sulfur, and nitrogen. Several highly selective new reagents are recommended for palladium and cobalt. Attention is redirected to 4-chloro-4-aminodiphenyland 2-aminoperimidine for determining extremely low concentrations of sulfate. Some of the basic definitions and considerations in trace analysis have been discussed by Egan ( 5 2 ) . Numerous other related reviews discuss some sources of contamination (162), adsorption characteristics of borosilicate glass, polyethylene, and polypropylene ( 17 5 ) , reduction of contaminants (124), use of Teflon and vitreous silica for concentration ( 3 0 ) . Various analytical techniques useful for the analysis of environmentally important materials are reviewed by Greifer and Taylor ( 7 3 ) and others (108). Other reviews discuss the determination of trace elements in high purity metals (92, 111) and trace techniques that do not require dissolution of the sample (100). Problems associated with the use of mass spectrography and flameless atomic absorption spectrometry for the determination of trace elements are discussed by Fuller ( 7 2 ) ;ideas on minimization are expressed by Griepink and Krijgsman (75).
Automated Analysis. The pace of automation of analyses has apparently attempted to keep up with the widespread increase in demand for analyses. This is reflected in
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the increase in the number of reports on the application of automation to various fields of analyses. A recent review by Van Gemert (192) of automated wet chemical methods describes their application to the analysis of fertilizers and other agricultural products, environmental analysis, corrosion studies, geological materials, metals and alloys, and numerous other inorganic materials. Standard Samples. As analytical techniques have continued to depart from the classical gravimetric methods based upon the absolute weights of separated constituents, they have become more dependent upon the use of standard samples for testing, calibrating, and controlling anaLITERATURE CITED
Brusdeyiins, A,,
lytical processes. This dependence has become more pronounced as interest has focused upon trace constituents. A number of organizations have attempted to keep pace with the demand for new standards and an increasing number of reference materials are rapidly becoming available. A wide variety of new inorganic reference materials for the metallurgical and other industries have been included in the current catalogue of the National Bureau of Standards (170). Flanagan (58) and Abbey (2) have provided recently revised compilations of the reference samples available for the earth sciences, including environmental analysis. Chem.-Zfg., 97, 543-47
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(209) Zmijewska, W., Chemia Anal., (Warsaw), 17, 1970, 281 pp. 179-215 (1972). (A-28) Myshlyaeva, L. V., Krasnoshchekov. V. V., "Analytical Chemistry of Silicon", Wiley (Halsted). New Vork, NV, 1974; Chem. Appendix A. Selected Books and Monographs on Abstr., 80, 152518q (1974). the Determination of the Elements (A-29) Nazarenko, I. I., Ermakov, A. N., "Analytical (A-1) Avtokratova, T. D., "Analytical Chemistry of Chemistry of Selenium and Tellurium", Wiley Ruthenium", Wiiey (Halsted), New Vork, NV. (Halsted), New Vork, NV, 1973, 280 pp. 1971, 250 pp. (A-30) Nazarenko, V. A,, "Analytical Chemistry of (A-2) Bard, A. J., Ed., "Encyclopedia of ElectroGermanium", Wiley (Halsted), New Vork. chemistry of the Elements", Vol. 1,2, DekNV, 1974. ker, New Vork, NV, 1974. (A-31) Nemodruk, A. A,, Karalova, 2. K., "Anaiyti(A-3) Beamlsh. F. E., Van Loon, J. C., "Recent cai Chemistry of Boron", Wlley (Halsted), Advances in the Analytical Chemistry of the New Vork, NV, 1971, 267 pp. Noble Metals", Pergamon. Oxford, 1972, (A-32) Nikolaev, N. S., Suvorova, S. N., Gurovich, 511 pp. E. I., Peka. I., Korchemnaya, E. K., "Analyti(A-4) Black, C. A,, Editor-in-Chief, "Methods of cai Chemistry of Fluorine", Wiley (Haisted), Soil Analysis". Part 2, American Society of New Vork. NY, 1973, 222 pp. Agronomy, Madison, WI, 1965, pp 771- (A-33) Novoselova, A. V.. Batsanova, L. R., "Ana1572. lytlcai Chemistry of Beryllium", Wiley (Halst(A-5) Boltz, D. F., "Colorimetric Determination of ed), New Vork, NV, 1971, 225 pp. Nonmetals", Wiiey, New Vork. NV, 1958. (A-34) Palei, P. N., "Analytical Chemistry of Urani(A-6) Busev, A. I., Ivanov, V. M., "Analytical um", Wiley (Halsted), New Vork, NY, 1971, Chemistry of the Elements: Analytical 421 pp. Chemistry of Gold", Nauka, Moscow, 1973, (A-35) Pal'shin, E. S.,Myasoedov, B. F.. Davydov, 263 pp, Chem. Abstr., 81, 335981 (1974). A. V., "Analytical Chemistry of Protactin(A-7) Busev. A. I., "Analytical Chemistry of Moiybium", Wiley (Halsted), New Vork, NV, 1971, denum", Wiley (Halsted). New Vork, NV, 233 pp. 1971, 283 pp. (A-36) Peshkova, V. M., Savostina, V. M.. "Analyti(A-8) Busev, A. I., Tiptsova, V. G., ivanov, V. M., cai Chemistry of Nickel", Wiley (Halsted), "Handbook of the Analytical Chemistry of New Vork, NV, 1971, 207 pp. Rare Elements", Wiley (Haisted), New Vork, (A-37) Pinta, M.. "Detection and Determination of NY, 1971,402 pp. Trace Elements", Ann Arbor Science Pub(A-9) Colton. R., "The Chemistry of Rhenium and lishers, Ann Arbor, MI 1966 (French original, Tellurium", Wiley-lnterscience, New York, 1962). NY, 1965. (A-38) Pyatnitskii, I. V., "Analyticai Chemistry of (A-10) Dymov, A. M., Savostin, A. P., "Analytical Cobalt", Wlley (Haisted), New York, NV, Chemistry of Gallium", Wilev (Halsted), New 1971, 253 pp. Vork, NV; 1971. (A-39) Ryabchikov, R. i, Gol'braikh, E. K., "Analyti(A-11) Elinson, S. V., "Spectrophotometry of Niocal Chemistry of Thorium", Wiley (Halsted), bium and Tantalum", Atomizdat, Moscow, New York, NV, 1971, 289 pp, 1973, 288 pp. (A-40) Ryabchikov, D. I., Ryabukhin, V. A,, "Analyt(A-12) Eiinson, S. V., Petrov, K. I., "Analytical ical Chemistry of Yttrium and the Lanthanide Chemistry of Zirconium and Hafnium", Wiley Elements". Wiley (Halsted), New Vork. NY, (Halsted), New York, NY, 1971, 243 pp. 1971,365 pp. (A-13) Eiwell, W. T., Wood, D. F., "Analytical (A-41) Sharipova, N., "Qualitative Analysis of Rare Chemistry of Molybdenum and Tungsten", Elements", Kazakhstan, Alma-Ata, USSR, Pergamon, Oxford, 197 1, 288 pp. 1973, 142 pp; Chem. Abstr., 10067t (1974). (A-14) Feigl, F., Vinzenz, A,, "Spot Tests in inor- (A-42) Scherbov. D. P., Matveets. M. A.. "Analytiganic Analysis", translated by R. E. Oesper, cal Chemistry of the Elements: Analytical Elsevier, New York, NY, 6th ed., 1972, 670 Chemistry of Cadmium", Nauka, Moscow, 1973, 254 pp. PP. ' (A-15) Furman, N. H., Ed., "Standard Methods of (A-43) Snell, F. D., Ettre. L. S., Ed., "Encyclopedia Chemical Analysis", 6th ed., Vol. 1, Van of Industrial Chemical Analysis", Wiley (inNostrand-Reinhoid, New York, NV, 1962. terscience), New Vork, NY. Voi. 1, 1966; (A-16) Gibalo, I. M., "Analytical Chemistry of NioVol. 2, 1966; Vol. 3, 1966; Vol. 4, 1967; bium and Tantalum", Wiley (Halsted), New Vol. 5 , 1967; Vol. 6, 1968; Vol. 7, 1968; Voi. 8, 1969: Voi. 9, 1970; Vol. 10, 1970; Vork, NY. 1971, 346 pp. Vol. 11, 1971; Voi. 12, 1971; Voi. 13, 1971; (A-17) Koithoff. I. M., Elving, P. J., Ed., "Treatise on Analytical Chemistry", Part 2, Wiley, New Voi. 14, 1971; Vol. 15, 1972; Vol. 16, 1972; Vork, NY, Vol. 1, 1961; Vol. 2, 1962; Vol. 3, Vol. 17, 1973; Vol. 18, 1973; Vol. 19. 1974; 1962; Vol. 4, 1966; Vol. 6, 1964. Voi. 20, 1974. (A-18) Korenman, i. M., "Analytical Chemistry of (A-44) Taras, M. J., Chairman, Editorial Board, "Standard Methods for the Examination of Potassium", Wiiey (Haisted), New Vork, NY, Water and Wastewater, Thirteenth Edition", 1971, 267 pp. (A-19) Korenman, I. M., "Analytical Chemistry of American Public Health Association, AmeriThallium", Wiley (Halsted), New York, NY, can Water Works Association, Water Pollu1971. 166 00, tion Control Federation, APHA, Washington, (A-20) Lavru'khinari. K.. Pozdnyakov, A. A,. "AnaDC, 1971, 874 pp. ivtical Chemistrv of Technetium, Prometh- (A-45) . . Tikhonov. V. N.. "Analvtical Chemistrv Of ibm. Astatine and Francium", Wiley (HalstMagnesium", Nauka, M~oscow, 1973, .254 ed), New Vork, NY, 1971, 307 pp. pp.. Chem. Abstr., 81, 72270h (1974). (A-21) Lewis, C. L.. Ott, W. L., "Analytical Chemis- (A-46) Tikhonov, V. N., "Analytical Chemistry of Aluminum", Wiley (Halsted), New York, NV, try of Nickel", Pergamon, Oxford, 1970, 232 1973, 250 pp. PP. (A-22) Mikhaiiov, V. A,, "Analytical Chemistry of (A-47) Vasii'ev, V. V., "Practical Manual on Chemical Detection of Anions". izd. Leninarad Neptunium", Wiiey (Halsted), New York, NV, Univ., Leningrad, 1973, 190 pp; &em. 1973, 250 pp. Abstr., 81, 10066s (1974). (A-23) Miiyukova, M. S.,"Analytical Chemistry of Plutonium", Wiley (Haisted), New Vork, NY, '(A-48) Vinogradov, A. P.. Ryabchikov. D. I., "Detection and Analysis of Rare Elements", 1971,440 pp. Published for the National Science Founda(A-24) Molot, L. A,, "Analytical Chemistry of Alumition by the Israel Program for scientific num", Part I, Izd. Saratovskovo Um-ta, Translations, Jerusalem, 1962. 1971, 135 pp. (A-25) Moshier. R. W., "Analytical Chemistry of Niobium and Tantalum", Pergamon, Oxford, Appendix 6. Selected Books on the Analysis of 1964, 278 pp. Rocks and Minerals (A-26) Mayasoedov, B. F., Guseva, L. i., Lebedev, I. (B-1) Basargin, N. N., "Chemical and PhysiochemA,. Miiyukova, M. S., Chmutova. M. K., "Anical Methods for the Analysis of Ores, Rocks alytical Chemistry of Transpiutonium Eleand Minerals", Nauka, Moscow, 1974, 94 ments", Wiley (Halsted). New York, NY, pp.; Chem. Abstr., 81, 1 3 0 5 8 0 ~(1974). 1974, 404 pp.; Chem. Abstr., 81, 114207a (8-2) Belopo'skii, M. P., Bunakova, N. Vu., Mikhaii(1974). ova, N. A,. et ai., "Chemical Analysis of (A-27) Mukherji. A. K., "Analytical Chemistry of ZirRocks and Minerals", (Manual), Nedra, Mosconium and Hafnium", Pergamon, Oxford,
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A N A L Y T I C A L CHEMISTRY, VOL. 47, NO. 5 , APRIL 1975
cow, 1974, 248 pp. (8-3) Bennett, H., Reed, R. A,, "Chemical Methods of Silicate Analysis", Academic Press, New Vork, NV, 1971, 272 pp. (8-4) Easton, A. J., "Chemical Analysis of Silicate Rocks", Elsevier, New Vork, NV, 1972, 258 PP. (8-5) Groves, A. W., "Silicate Analysis", 2nd ed.. George Allen and Unwin, Ltd., London, 1951, 336 pp. (B-6) Hillebrand, W. F., Lundeil. G. E. F., Bright, H. A,, Hoffmann, J. I., "Applied Inorganic Analysis", 2nd ed., Wiley, New Vork, NV, 1953, 1034 pp. (8-7) Jeffery, P. G., "Chemical Methods of Rock Analysis", Pergamon, London, 1970, 507 PP. (B-8) Levinson, A. A,, "Introduction to Exploration Geochemistry", Applied Publishing, Ltd., Calgary, 1974. (B-9) Lundell, G. E. F.. Hoffman, J. I., Bright, H. A,. "Chemical Analysis of iron and Steel". Wiiey, New York, NY, 1931. (B-10) Maxwell, J. A,, "Rock and Mineral Analysis", Wiley (interscience), New Vork, NV, 1968, 584 pp. (B-11) Moskalyuk, A. A,, "Determination of the Composition of Mineral-Forming Solutions by a Method of Aqueous Extracts from Inciusions. Procedural instructions", Leningrad: Vses. Nauch.-issled. Geol. Inst., 1973, 80 pp.; Chem. Abstr., 81, 90891v (1974). (8-12) Popov, N. P., Stolyarova, I. A,, Ed., "Chemical Analysis of Rocks and Minerals", Moscow: Nedra, 1974, 248 pp.; Chem. Abstr., 1 3 0 5 7 8 ~(1974). (8-13) Sandell, E. B., "Colorimetric Determination of Traces of Metals", 3rd ed., Wiiey (Interscience), New York, NY, 1959, 1032 pp. (8-14) Schroll, E., "Introduction to Analytical Geochemistry", Ferdinand Enke, Stuttgart, Germany, 1974, 260 pp. (6-15) Smales, A. A,, Wager, L. R., "Methods in Geochemistry", Wiley (interscience), New York, NY, 1960, 464 pp. (B-16) Shultz, J. I., Beii, R. K., Rains, T. X., Menls, O., "Methods of Analysis of NBS Clay Standards", National Bureau of Standards, NBS Spec. Pub/., NO.280-37, 1972. (8-17) Soil Conservation Service, "Soil Survey: Laboratory Methods and Procedures for Coilecting Soil Samples", Soil Survey Investlgations Report No. 1, revised April 1972, Soil Conservation Service, 63 pp. (B-18) Voinovitch, I. A,, Debras-Guedon, J., Lovrier, J., "The Analysis of Silicates", orig. French ed., Herman, Paris, 1962; English translation, israel Program for Scientific Translation, Ltd.. Jerusalem, Israel. 1966. (B-19) Wainerdi, R. E., Uken, E. A,, Ed., "Modern Methods of Geochemical Analysis", Plenum, New York, NV, 1971, 398 pp. (8-20) Welcher, F. J., Ed., "Standard Methods of Chemical Analysis", Vol. 2, Part A; Vol. 3, Part A and B. Van Nostrand-Reinhold, New York, NY, 1963.
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Appendlx C. Selected Books and Review Articles on the Analvsls of Metallurolcai and Other ~Industrial Products ~
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(C-1) Akhmetov, T. G., Lisina. N. V., "Analytical Methods for Monitoring the Production of Barium and Sulfite Salts", Khimiya, Moscow, 1974, 199 pp., Chem. Absfr., 9451c (1974). (C-2) Annual Book of ASTM Standards, Pt. 12, "Chemical Analysis of Metals, Sampling and Analysis of Metal Bearing Ores", ASTM, Philadelphia, PA, 1974, 833 pp. (C-3) Bunshah, R. F., "Modern Analytical Techniques for Metals and Alloys", Vol. 3, Pt. 1, Wiley (Interscience). New Vork, NY, 1970. (C-4) Ershov, V. A,, Moizhes, I. B., iodaova, E. S., et ai., "Manual for Analysis in the Production of Phosphorus, Phosphoric Acid, and Fertilizers", Khimiya, Leningrad, Otd. Leningrad, 1973, 212 pp.; Chem. Abstr., 81, 33597e (1974). (C-5) Garg. S. K., Svalbonas, V., Gurtman, G. A., "Monographs and Textbooks in Material Science, Vol. 6: Analysis of Structural Composite Materials", Dekker, New York, NY, 1973, 473 pp. (C-6) Haimann, M., Ed., "Analytical Chemistry of
Phosphorus Compounds", Wiley (InterYork, NY, Vol. 1. 1967; Vol. 2, 1969; Vol. 3, "Systematic Materials Analysis", Academic, New York, NY, Vol. 1, 2, 3, 4, 1974. 1972; Vol. 4, 1972. science), New York. NY, 1974, 850 pp. (C-7) Kolthoff. I. M.. Elvino. P. J., Stross. F. H., (D-17) Grove, E. L.. Ed., "Analytical SDectroscoDy (D-46) Simmons, I. L., Ewing, G. W., Ed., "Applications of the Newer Techniques of Analysis", Series", Vol. 1. Analytical Emksion Spec"Treatise on Analytical chemistry", Part ill, Plenum, New York, NY, 1973, 384 pp. troscopy, Part 1, 1971; Part 2, 1972. Vol. 2, Wiley, New York, NY, 1971. (C-8) Kurbatova, I. I., Abramkina, V. G., Averbukh, (D-18) Gouw, T. H., Ed., "Guide to Modern Methods (D-47) Skoog, D. A., West, D. M., "Principles of Instrumental Analysis", Holt, Rinehart and of Instrumental Analysis", Wiley (InterM. A,, "Handbook On Spectroscopic AnalyWinston, New York, NY, 1971, 170 pp. science), New York. NY, 1972, 512 pp. sis of Construction' Materials". Stroilzdat, Moscow, 1972; Chem. Abstr., 78, 66635c (D-19) Guilbault, G. G., "Practical Fluorescence, (D-48) Slavin. M., "Emission Spectrochemical Analysis", Wiley, New York, NY, 1971, 254 (1972). Theory, Methods, and Techniques", Dekker, New York, NY, 1973, 664 pp. PP. (C-9) Melnick. L. M.. Lewis, L. L., Holt, B. D., Ed., "Determination of Gaseous Elements in Met- (D-20) Guichon. G , Pommier. C., "Gas Chromatog- (D-49) Tolg, G., "Ultramicro Elemental Analysis", Wiley (interscience), New York. NY, 1970, raphy in Inorganic Analysis", Wiley, New als", Wiley (Interscience), New York, NY, 200 pp. York, NY. 1972, 360 pp. 1974, 744 pp. (D-50) Tolgyessy, J.. Brau, T., Kyrs, M., "Isotope (D-21) Hausenbuilier, P. L., "Soil Science; Princi(C-lo) Stepin. V. V., Silaeva, E. V., Kurbatova, V. Dilution Analysis", Pergamon. New York. ples and Practice", Wm. C. Brown Co.. DuI., Federova, N. D.. Ponorov, V. I., "The NY. 1972. buoue. IA. 1972 Analysis of Ferrous Metals, Alloys, and Manganese Ores", Moscow, Izd. Metallurgiya. (D-22) Huibard, D. P., Ed., "Annual Reports on An- (D-51) Tolgyessy, J., Varga. S.,Krivan, V., "Nuclealytical Atomic Spectroscopy", 1972, Vol. ar Analytical Chemistry. 1. Introduction to 1971,392 pp. 2, Society for Analytical Chemistry, London, Nuclear Analytical Chemistry", University (C-11) Stepin, V. V., Silaeva, E. V., Kurbatova, V. I. 1973. Park Press, Baltimore, MD. 1971; VoI. 11, et al., "Analysis of Nonferrous Metals and (D-23) Jordan, J., Ed., "New Development in Titri1972; Vol. 111, 1974. Alloys", 2nd ed., Metailurgiya, Moscow, metry. Vol. 2", Dekker, New York, NY, (D-52) Ugo, R., "Instrumental Chemical Analysis". 1974, 207 pp.; Chem. Abstr., 81, 329484 L. G. Guadagni, Milan, 1972, 688 pp. 1974, 200 pp. (1974). (C-12) Samsonov, G. V., Frantsevich, I. N., Ed., (D-24) Kane, P. F.. "Characterization of Solid Sur- (D-53) Vaughan, G. A,, "Thermometric and Enthalfaces", Plenum, New York, NY, 1974. pimetric Titrimetry". Van Nostrand-Reinhold, "Chemical Properties and Analysis of ReLondon, 1973,255 pp. fractory Compounds", Plenum, New York, (0-25) Karger. 6.L., Ed., "An Introduction to Separation Science", Wiiey (Interscience), New (D-54) Vinogradov, A. P., Ryabchikov, D. I., Ed., NY. 1972, 127 pp. "Detection and Analysis of Rare Elements", York, NY, 1973, 586 pp. (C- 13) Steels (Alloyed and Highly Alloyed). Methods Israel Program for Scientific Translations, of Chemical Analysis. State Standards (D-26) Kazakov, A. V., Kantere, V. M., Galkin, L. G., "Titrimeters. (Titrimetry)", Mashinostoen1962, 744 pp: Office of Technical Services GOST 12344-66-GOST 12365-66 and GOST NOOTS-62-11021. ie. Moscow, 1973, 223 pp.; Chem. Abstr., 17051-7 1. Gosudarstvennyi Komitet (D-55) Volynets, M. P., "Thin-Layer Chromatogra81, 10069v (1974). Standartov, Izd. Standartov, Moscow, 1973, (D-27) Kirkendaie, G. A., Ed., "Analytical Methods phy in Inorganic Analysis", Nauka, Moscow, 271 pp,; Chem. Abstr., 81, 127864r (1974). for Material investigation", Gordon and 1974, 151 pp.; CA-1B0585C (1974). (C-14) Westwood, W., Cooper, B. S., "Analytical Breach, New York, NY, 1971. (D-56) Walton, H. F., Reyes, J., "Modern Chemical Methods in Use in Non-Ferrous Mining and (0-28) Korkisch, J., "Modern Methods for the SepAnalysis and instrumentation', Dekker, New Metallurgy. A Selective Review", The Instituaration of Rarer Metal ions", Pergamon. York, NY, 1973, 440 pp. tion of Miing and Metallurgy, London, 1973, (D-57) Wagner, W., Hull, C. J., "Inorganic TitrimetLondon, 1969,620 pp. 54 PP. ric Analysis, Vol. l " , Dekker, New York, NY, (C-15) Wilson, M. L., "Nondestructive Rapid Identifi- (D-29) Kolthoff, I. M., Elving, P. J., "Treatise on Analytical Chemistry, Part 1, Theory and Prac1971, 225 p. cation of Metals and Alloys by Spot Test", ASTM Spec. Tech. Pub/., 550, ASTM, Philatice", Wiiey, New York, NY. 1959. (D-58) Waish, L. M., Ed., "Instrumental Methods for (D-30) Korte, F., "Chemical Methods, Vol. 1, AnalyAnalysis of Soils and Plant Tissue", Soil delphia, PA, 1974, 54 pp. sis, Pts. 1 and 2", Thieme, Stuttgart, GermaScience Society of America, Inc., Madison, WI. 1971. ny, 1973, 1342 pp.; Chem. Abstr., 80, Appendix D. Selected Books and Monographs on 10071q (1974). (D-59) Wendlandt, W. W.. Thermal Methods of General Analytical Techniques (D-31) Marinsky, J. A,, Marcus, Y., "Ion Exchange Analysis", 2nd ed., Wiley (Interscience), (D-1) Angino, E. A,, Billings, G. K., "Atomic AbNew York. NY, 1974, 528 pp. and Solvent Extraction", Vol. 4, Voi. 5 , Deksorption Spectrometry in Geology", 2nd ed., (D-60) West, T. S., Ed., "MTP International Review ker, New York, NY. 1973. Elsevier, New York, NY, 1972, 160 pp. of Science. Physical Chemistry, Series 1, (D-32) Mavrodineanu, R., Shultz, J. I., Menis, D., (0-2) Babko, A. K., Pilipenko, A. T., "photometric Voi. 12, Analytical Chemistry, Pt. 1 and 2". Ed., "Accuracy in Spectrophotometry and Analysis. Methods for Determining NonmeButterworth, London, 1972. Luminescence Measurements", U.S. Govtals", Khimiya, Moscow, 1974, 360 pp.; ernment Printing Office, Washington, DC. (D-61) Westwood, W., Cooper, B. S., "Analytical Chem. Abstr., 81, 130579d (1974). Methods in Use in Non-Ferrous Mining and 1972. (D-3) Bark, L. S., Ed., "Selected Annual Reviews (D-33) Meinke, W., "Characterization of Solids. Metallurgy, A Selective Review", The Instituof the Analytical Sciences", Vol. 1, Society Chemical Composition" in "Treatise, Solid tion of Mining and Metallurgy, London, 1973, for Analytical Chemistry, London, 1971. State Chem.", 387-434, N. B. Hannay, Ed., 54 PP. (D-4) Bark, L. S.,Ed., "Selected Annual Reviews (D-62) White, C. E., Argauer, R. J., "Fluorescence Plenum, New York, NY, 1973. of the Analytical Sciences", Vol. 2, Society (D-34) Meites, L., Ed.. "Critical Reviews in AnaiytiAnalysis: A Practical Approach", Dekker, for Analytical Chemistry, London, 1972. New York, NY, 1970, 389 pp. cal Chemistry", Chemical Rubber Co.. (D-5) Betteridge, D.. Hallam. H. E., "Modern Ana(D-63) Willard, H. H., Merritt, L. L.. Jr., Dean, J. A., Cleveland, OH. lytical Methods", Chemical Society, London, (D-35) Melnick, L. M., Lewis, L. L., Hoit, 8. D., Ed., "instrumentai Methods of Analysis", 5th ed., 1972, 228 pp. Van Nostrand, New York, NY, 1974, 860 pp, "Determination of Gaseous Elements in Met(D-6) Bishop, E.. Ed., "Indicators", Pergamon (D-64) Wilson, C. L., Wilson, D. W., Ed., "Compreals", Wiley, New York, NY, 744 pp. Press, New York, NY, 1972, 746 pp. hensive Analytical Chemistry", Elsevier. (D-36) Mika, J., Torok, T., "Analytical Emission (D-7) Biyum, I. A,, "Extraction Photometric MethNew York. NY, Vol. 1, 1960; Vol. IIA, 1964; Spectroscopy", Crane Russak and Co.. Lonods of Analysis by Means of Basic Dyes", don, 1974, 576 pp. Vol. IlB. 1968; Vol. IC. 1971. Nauka, Moscow, 1970, 219 pp. (D-37) Minczewski, J., Chwastowska, J., Dybezyn- (D-65) Winefordner, J. D., Shulman, S. G., O'Haver, (D-8) Burger, K., "Organic Reagents in Metal T. C.. "Luminescence Spectrometry in Anaski, R., "Trace Analysis: Methods for SepaAnalysis", Pergamon. Oxford, 1973, 266 pp. lytical Chemistry", Wiley (Interscience), New ration and Concentration", Wyd. Nauk(D-9) Camman, K., "Guide for Chemical LaboratoYork, NY, 1972, 354 pp, Tech., Warsaw, 1973, 566 pp.; Chem. ry Practices, Vol. 13: Use of Ion-Selective Abstr., 81, 57940h (1974). (D-66) Winefordner, J. D., Ed., "Spectrochemical Electrodes: an Introduction". Springer, Ber- (D-38) Nargolwalla, S. S . , Przybylowicz. E. P., Methods of Analysis", Wiiey (Interscience), lin, 1972, 226 pp.: Chem. Abstr., 81, "Chemical Analysis, Vol. 39: Activation New York, NY, 1974, 530 pp. 83379p (1974). Analysis with Neutron Generators", Wiley, (D-67) Woodward, C., Ed., "Annual Reports on An(D-10) Daniels, T., "Thermal Analysis", Kogan New York, NY, 1973, 662 pp. alytical Atomic Absorption, 1973", Vol. 3, Page Ltd., London, 1973, 272 pp. (D-39) Newton, G. W. A., Senior Reporter, "RadioSociety for Analytical Chemistry, 1974. (D-1 1) Dean, J. A,, Rains, T. C., "Flame Emission chemistry", Vol. 1, Chemical Society, Lon- (D-68) Woodward, C., Redman, H. N., "Analytical and Atomic Absorption Spectrometry", Vol. don. Sciences Monograph No. 1: High Precision 1 and 2, Dekker, New York, NY, 1971. (D-40) Parker, C. A., "Photoluminescence of SoluTitrimetry", SOC. Anal. Chem., London, (D-12) De Soete. D., Gijbels, R., Hoste. J.. "Neutron 1973, 63 pp. tions", Elsevier, New York, NY. 1968, 544 Activation Analysis", Wiley (Interscience), (D-69) Wu. Chen-Ch'eng. "Industrial Analysis", San PP. New York, NY, 1972. (D-41) Pickering, W. F., "Modern Analytical ChemMin Shu Chu, Paipei, Taiwan, 1972, 188 pp; (D-13) Dolezal, J., Povondra, P., Sulcek. Z.,"Deistry", Dekker, New York, NY, 1971, 622 Chem. Abstr., 81, 1 2 7 8 6 7 ~(1974). composition Techniques in Inorganic Analy(D-70) Yakubovich, A. L., Zaitsev, E . I., PrzhiyalPP. sis", Elsevier, New York, NY, 1968, 224 pp. (D-42) Pilipenko, A. T., "Organic Reagents in Inorgovskii, S. M., "Nuclear-Physics Methods for (D-14) Erdey, L., Svehla, G., "Ascorbinometric Tiganic Analysis", Vishcha Shkola, Kiev, Analysis of Mineral Raw Materials", 2nd ad., trations", Akad. Kiado: Budapest, 1973, 183 1972, 216 pp, Atomizdat, Moscow, 1973, 391 pp; Chem. pp.; Chem. Abstr., 81, 152511 (1974). (D-43) Pribil, R., "Analytical Applications of EDTA Abstr., 80, 55559w, (1974). (D-15) Felhorski. W., Stanioch, W., "Trichromatic and Related Compounds", Pergamon, Ox- (D-71) Zief, M.. Speights, R., Ed.. "Ultrapurity: Colorimetry", Wyd. Nauk.-Tech, Warsaw, ford, 1972, 368 pp, Methods and Techniques", Dekker, New 1973, 317 pp.; Chem. Abstr., 81, 90894y (D-44) Price, W. J., "Analytical Atomic Absorption York, NY, 1972, 699 pp. (1974). Spectrometry". Heyden & Son, London, (D-72) Zolotov. Yu. A., "Extraction of Chelate Com(D-16) Flaschka, H. A,, Barnard, A. J.. Jr., "Che1972,239 pp. pounds", Wiley, New York, NY, 1970, 310 lates in Analytical Chemistry", Dekker, New (D-45) Richardson, J. H., Peterson, R. V., Ed., PP. A N A L Y T I C A L CHEMISTRY, VOL. 47, NO. 5, APRIL 1975
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Appendlx E. Selected References on the Analysis of Geologlcal Materlals
(E-1) Abbey, S.."Analysis of Rocks and Minerals by Atomic Absorption and Flame Emission Spectroscopy. IV. Composite Scheme for Less-Common Alkali and Alkaline-Earth Eiements", Geol. Survey Canada, Paper No. 71-50, 1972, 18 DD. (E-2) Abbey, S., Lee, N. J., Bouvier, J. L.. "Analysis of Rocks and Minerals Using an Atomic Absorption Spectrophotometer. Part 5. An improved lithium-fluoborate scheme for 14 elements", Canada. Geol. Survey Paper 7419, 1972,26 pp. 6 3 ) Ashley, D. G., Andrews. K. W., Analyst, 97, 841-7 (1972). (E-4) Avni, R., Harel, A,, Brenner, I. B., Appl. Spectrosc., 28, 641-5 (1972). 6 5 ) ASTM Special Technical Publication 539, Analytical Methods Developed for Application to Lunar samples Analyses, American Society for Testing Materials, 1973, 156 pp. (E-6) Atherton, M. P., Brotherton. M. S., Raiswell, R., Chem. Geol., 7, 285-93 (1971). (E-7) Bennett, H., Reed, R. A,, Anahst (London), 96, 640-55 (1971). 6 8 ) Corbett, J. A., Godbeer, W. C., Watson, N. C., Proc. Australas. lnst. Min. Metall., No. 250, 1974, pp 51-4. 6 9 ) Davey, J., Nicholson, N. M., "Determination of Trace Elements in Fluorspar Mining Survey Samples", British Steel Corp. Report, GS/EX/14/72/C, 1972, 8 pp. (E- 10) Dorrzapf, A. F., Jr., J. Res. U.S. Geol. Survey, 1, 559-62 (1973). (E-11) Fabbi, B. P., Espos, L. F.. U.S. Geol. Survey Prof. Pap. 800-6, 8147-50 (1972). (E-12) Gallus-Olender, J., Chem. Anal. (Warsaw), 17, 139-45 (1972). (E-13) Glasby, G. P., Mar. Chem., 1, 105-25 (1972). (E-14) Gormasheva, G. S., Bakaieinikova, T. K., Novikov, V. M., Ezheg.. lnst. Geokhlm., Sib., Otd., Akad. Nauk SSSR 1972, 466-70, 1973; Chem. Abstr., 81, 1 3 0 4 7 7 ~(1974). (E-15) Gose, W., Ed., Proceedings of the Fourth Lunar Science Conference, Vol. II, Geochim. Cosmochim. Acta, Suppl. 4, 1973. (E-16) Gose, W., Ed., Proceedings of the Fifth Lunar Science Conference, Vol. 11, Geochlm. Cosmochim. Acta, Suppl. 5 , 1974.
(E-17) Govindaraju, K., Analusis, 2, 367-76 (1973). (E-18) Gribble, G. W.. Total Chemical Analysis of Rocks, Soils, and Clay Minerals by X-ray Fluorescence Quantometer, Hawaii Institute of Geophysics, No. H1G-74-2, 1974, 81 pp. (E-19) Guest, R. J., Macpherson, D. R.. Anal. Chim. Acta, 71; 233-53 (1974). (E-20) Harvey, P. K., Taylor, D. M., Hendry, R. D., Bancroft, F., X-Ray Spectrom., 2, 33-44 119731. (E-21) Hebeit, A. J., Street, K., Jr., Anal. Chem., 46, 203-7 (1974). (E-22) Heinrichs, H., Lange, J., Fresenius' Z. Anal. Chem., 285, 256-60 (1973). (E-23) Helz, A , J. Res., U.S. Geol. Survey, 1, 475-82 (1973). (E-24) Heymann, D., Ed., Proceedings of the Third Lunar Science Conference, Vol. 11, Chemical and Isotope Analysis/Organic Chemistry, Geochim. Cosmochlm. Acta, Suppl. 3, 1972. [E-25) Hitchen. A,. "Determination of Titanium in Lead Zirconate-Load Titanate Electronic Ceramics, Comparison of Titrimetric Methods with Polarographic and Differential Spectrophotometric Methods", Can. Mines, Br., Tech. Bull. TB 153, 1972, 35 pp. (E-26) Langmyhr, F. J., Stubergh, J. R., Thomassen, Y . , Hanssen, J. E., Dolezal, J., Anal. Chim. Acta, 71, 35-42 (1974). (E-27) Langmyhr, F. J., Thomassen, Y.. Fresenius' 2.Anal. Chem., 264, 122-7 (1973). (E-28) Langmyhr, F. J., Rasmussen, S.,Anal. Chim. Acta, 72, 79-84 (1974). (E-29) Lavrent'ev, Yu. G., Pospelova, L. N., Soboiev, N. V., Malikov, Y . I., Zavod. Lab., 40, 657-61 (1974); Chem. Abstr., 81, 130536n (1974). (E-30) Lischenko. Ya. P., L'vov, B. V., Oriova, N. A,, Probl. Izuch. Osvoeniyz Prir. Resur. Sev., 184-8, T. N. Ivanova, Ed., Akad. Nauk SSR, Kol'sk. Filial: Apatity, USSR, 1973; Chem. Abstr., 81, 9379k. (E-31) Lyubomiiova, G. V., issled. Ob/. Rud. Mineral, 203-8, M. S. Bezsmertnaya, Ed., "Nauka": Moscow, USSR, 1973; Chem. Abstr., 81, 1 0 0 2 0 (1974). ~ (E-32) Mastins, H., Jones, J. B., Nesbitt, R. W., J. Geol. SOC.Australia, 19, 217-24 (1972). (E-33) Medlin, J. H., Suhr, N. H., Bodkin, J. B., Kim. Sanayi, 21, 21-34 (1973). (E-34) Medved, J., Plsko, E., Cubinek, J., Acta Geol. Georg. Univ. Comenianae, Geol., 27, 18394 (1974); Chem. Abstr., 81, 1304242 ,
I
(1974). (E-35) Novikov, V. M., Shiryaeva, V. A,, Khaltueva, V. K., Ezheg., lnst. Geokhim., Sib. Old., Akad. Nauk SSSR 1972, 476-80 (1973); Chem. Abstr., 81, 13048% (1974). (E-36) Ooghe, W., Verbeek, Anal. Chim. Acta, 73, 87-95 (1974). (E-37) Peck, L. C., "Systematic Analysis of Silicates", U.S. Geol. Surv. Bull., 1170, 1964, 89 PP. (E-38) Riandey, C., Pinta, M., Analusis, 2, 179-85 (1973). (E-39) Rubeska. I., Kem. Kozlem, 41, 195-203 (1974); Chem. Abstr., 81, 85450s (1974). (E-40) Saavedra, J., Garcia Sanchez, A,, Rodriguez Perez, S..Chem. Geol., 13, 135-39 (1974). (E-41) Sass, A,, lnfs. Chim., 227-35 (1972). (E-42) Schultz, J. I., Bell, R . K., Rains, T. C.. Menis, O., Methods of Analysis of NBS Clay Standards, Nat. Bur. Stand. Spec. Publ., 260-37, 1972, 86 pp. (E-43) Shock, H. H., Fresenius' Z. Anal. Chem., 263, 100-7 (1973). (E-44) Shapiro. L., "Rapid Analysis of Silicate, Phosphate, and Carbonate Rocks", rev. ed., U.S. Geol. Survey Bull., 1401, 1975. (E-45) Shiryaeva, V. A,, Novikov, V. M., Grigor'eva, V. A., Ezheg., lnst. Geokhim., Sib. Otd., Akad. Nauk SSSR 1972, 471-5, 1973; Chem. Abstr., 81, 1 3 0 4 7 8 ~(1974). (E-46) Shuvalova, N. I., Stoiyarova, I. A,, Shcherbovich, G. V., Anal. Metody Geokhlm. Issled., Mater. Geokhim. Conf., 4th 1970, 45-9, E. M. Kvyatkovakii, Ed., Leningrad. Gorn. Inst., Leningrad, USSR, 1972: Chem. Abstr., 81, 32811d (1974). (E-47) Terashima, S., Bull. Geol. Survey, Japan, 23, 287-304 (1972). (E-48) Terashima. S., Chishitsu Chosajo Geppo, 24, 469-85 (1973): Chem. Abstr.;81, 32921q (1974). (E-49) Tertian, R., Geninasca. R.. X-Ray Spectrom., 1, 83-92 (1972). (E-50) Vas'kova, A. G., Avilov, V. B., Vop. Litol. Geokhim. Vulkanogenno-Osad. Obrazov. Yuga Dal'nego Vostoka 1971,248-51, E. A. Kireeva, Ed., Akad. Nauk SSSR, Dal'nevost. Geol. Inst.; Chem. Abstr., 81, 1304361 (1974). (E-51) Walthall. F. G., J. Res. U.S. Geol. Survey, 2, 61-71 (1974). (E-52) Wittkopp, R., O'Day, M.. Anal. Lett., 6, 1021-28 (1973).
Ferrous Metallurgy W. A. Straub and J. K. Hurwitz U . S . Steel Corporation, Research Laboratory, 125 Jamison Lane, Monroeville, PA 75 146
This review covers the period from November 1972 through October 1974, and is a continuation of previous reviews:The search of Chemical Abstracts was aided by the Knowledge Availability Service Center a t the University of Pittsburgh. The other source used was Analytical Abstracts. Following each citation in the Literature Cited, either the Chemical Abstract ( C A ) volume and abstract numbers or the corresponding Analytical Abstract ( A A )numbers are given. Because of the increased emphasis on the analysis and use of prereduced ores, iron has been added to the elements surveyed for this review. Authors have not been supplied wlth free reprlnts for distribution. Extra coples of the revlew Issue may be obtalned from Special Issues Sales, ACS, 1155 18th St., N.W., Washlngton, DC 20036. Remlt $4 for domestic U.S. orders; add $0.50 for addltbnal postage for foreign destlnatlons.
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CONFERENCE PROCEEDINGS, BOOKS, AND REVIEWS In the past few years, several symposia, colloquia, and conferences have been held with part or all of the proceedings being devoted to analytical problems in ferrous metallurgy (2, 18, 81, 244). Several general books and reviews on the analysis of ferrous alloys and ores have also been published (19, 242, 261, 492, 493), with particular emphasis on the analysis of raw materials, ores, slags, and metal powders by X-ray, emission, and nuclear methods (72, 151, 162, 163, 190, 489, 543). The analysis of steels and ferroalloys for trace elements has been reviewed (282,291,562).A new book on the determination of gases in metals (352) and an extensive review on the determination of nonmetallic incluin have appeared ( I 5 ) . Atomic absorption spectrometry has continued attract-
ANALYTICAL CHEMISTRY, VOL. 47, NO. 5, A P R I L 1975
