Anal. Chem. 1980, 52. 53R-69R (9) DeBeer, R.; Merks, R. P. J. Delft frogr. Rep. 1979, 4 , 63-6. (10) Wosik, J.; Nesteruk, K.; Zbieranowski. W.; Sienkiewicz, A. J. fhys. E . 1978, 7 1 , 1200-1209. (11) Chamberlin, R. V.; Moberly, L. A.: Symko, 0. G. J. fhys. Colloq. (Orsay, Fr.) 1978,2(6), 1217-18. (12) Balia, J.; EroGecs, M.; Janossy, A. Hung. Acad. Scl., Cent. Res. Inst. fhys.. KFKI (1978). KFKI-1978-251, 6 pp.; C . A . 1978, 89, 171707C. (13) Eaton, S. S.; Eaton, G. R. Anal. Chem. 1977, 49, 1277-8. (14) Chiu, V. J. H.; Griller, D.; Ingold, K. U.;Knittei, P. J . fhys. Ed. 1979, 12, 274-5. (15) Fouse. G. W.; Bernhard, W. A. J . Magn. Reson.. 1978, 32, 191-8. (16) Mialhe. P. Phys. Status Solidi B . 1979,93, 189-95. (17) Dalgaar, E. R o c . R . SOC. London, Ser. A 1978. 367, 487-512. (18) Eaton, S. S.;DuBois, D. L.; G. R . J . Magn. Res. 1978, 32, 251-63. (19) Istomin, V. E.; Shcherbakova, M. Ya. Zh. Strukt. Khim. 1977, 18, 824-34. (20) Bikchantaev, I.G.; Ovchinnikov, I.V. Zh. Strukt. Khim. 1977, 78, 956-8. (21) Baranowski, J.; Cukiorda, T.; Jezowska-Trzebiatowska, 6.; Kozlowski, H. J . Magn. Reson. 1979,33, 585-93. (22) Markham, G. D.; Rao. B. D. N.; Reed, G. H. J . Magn. Reson. 1979,33, 595-602. (23) Eidels-Dubovoi, S.;Beltran-Lopez, V. J. Magn. Reson. 1978,32,441-9. (24) Ovchinnikov, I. V.; Konstantinov, V. N. J . Magn. Reson. 1978, 32, 179-90. (25) Balasubramanian, K.; Dalton, L. R. J. Magn. Reson. 1979,33,245-60. (26) Mailer, C.; Miller, D. M. J . Magn. Reson. 1978,32,289-92. (27) Wessel, R.; Schwarz, D. Exp. Tech. fhys. 1978,26(2), 195-202. (28) Lowe, D. J. Biochem. J . 1978, 177(3), 649-51. (29) Lowe, D. J. Biochem. J . 1978, 777,649-51. (30) Goldberg, I. J . Magn. Reson. 1978,32,233-42. (31) Sharrock, P. J . Magn. Reson. 1979, 33, 465-7. (32) Petrakis. L.; Grandy, D. W. Anal. Chem. 1978, 5 0 , 303-8. (33) Solozhenkin, P. M.; Sidorenko. G. G.; Larin, G. M.; et ai. Zh. Anal. Khim. 1979,34, 808-11; C . A . 1979,91,8 2 4 6 6 ~ . (34) Chang, Te-Tse; Foster, D.; Kahn, A. H. J . Res. Natl. Bur. Stand. U . S 1978,83, 133-64. (35) Modine, F. A.; Sonder. E.; Weeks, R. A. J . Appl. fhys. 1977, 48, 3514- 18. (36) Kashiwagi, 0.; Nakamura, H.; Isobe, T., Tarutani, T. Mem. Fac. Sci., Kyushu Univ. Ser. C 1959, 7 7 , 257-60; C . A . 1979,90, 132289~. (37) Stegmann, H. B.; Uber, W.; Scheffer, K. Fresenius' 2.Anal. Chem. 1977, 286,59-64. (38) Janzen, E. G.; Burns, S. P. Anal. Left. 1977, 10, 1009-17. (39) Proskuryarov, I.I.; Prokhorenko, I.R.; Vosnyak, V. M.; Erokin, Y. E. Bioflsika 1978,23(5),916-18. (40) Schmidt, J. J . Lumin. 1979, 78- 79 (Pt.I), 183-6. (41) Nuzuma, S.; Hirotu, N. J . fhys. Chem. 1978,82, 453-9. (42) Conners, R. E.; Comer, J. C.; Durand. R. R., Jr. Chem. Phys. Left. 1979, 67,270-4. (43) Schweiger, A.; Joerin, E.; Guenthard, H. H. Chem. fhys. Lett. 1979,61, 223-7. (44) Scandola, M.; Reed, P. E. J . Mater. Scl. 1978, 14,541-8. (45) Jackson, S. E.; Smith, E. A,; Symons, M. C. R. Faraday Discuss. Chem. SOC. 1978,64, 173-87. (46) Ishizu, K.; Kohama. H.; Mukai, K. Chem. Left. 1978,227-30. (47) Flesia, E.; Surzur, J. M.; Tordo, P. Org. Magn. Res. 1978, 1 7 , 123-6. (48) Cannistraro. S . ; Van de Vorst, A.; Jori, G. fhotochem. fhotobiol. 1978, 28,257-9. (49) McBride, M. 8. Soil Sci. 1978, 126, 200-209. (50) McBride, M. B. Clay Miner. 1977, 72(3), 273-7. (51) McBride. M. B. Clavs Clav Miner. 1979. 27. 97-104 (52j McBride, M. B. Cliys Cb> Miner. 1979, 27, 91-6. (53) Byberg, J. R . Chem. fhys. Left. 1978, 56, 563-7. (54) Raynor, J. B.; Robson, M. J . Chem. Res. Synop. 1979, 105. ( 5 5 ) Tanaka, T.; Matsuda. T.; Okuzumi, I.J . Polym. Scl., foiym. Chem. Ed. 1979, 77,917-18. (56) Mialhe, P.; Kassis, H.; Quedec, P. J . fhys. C. 1977, 70, 1381-4. (57) Vorob'ev, L. N.; Talipov, G. Zh. Fir. Chim. 1978, 52(2), 361-5. (58) Lossee, D. B. J . Catal. 1977,5 0 , 545-8. (59) Gutowski, M. fhys. Rev. B.: Condens. Matter 1978, 78,5984-9. (60) McPherson, G. L.; Ndine, M. H.; Devaney. K. 0. fhys. Rev. B: Condens. Matter 1978, 78, 601 1-13. (61) Stach. J.; Kirmse. R.; Hoyer, E., Wartewg, S. J. Inorg. Nucl. Chem. 1978, 40, 1529-32. (62) Knight, L. B., Jr.; Mouchet, A.; Besudry, W. T.; Duncan, M. J. Magn. Reson. 1978,32. 383-90.
(63) Symons, M. C. R.; Brown, D. R.; Eastland. G. W. Chem. Phys. Left, 1979, 61, 92-5. (64) Benson, W. R.; Yang, G. C.; Heitzmann, M W.; Ford, L. A. J . Labelled Compd. Radiopharm. 1978, 15, (suppl. vol.), 343-52. (65) Kirmse, R.; Dietzsch, W.; Solovev, B. V. J . Inorg. Nucl. Chem. 1977, 39, 1157-60. (66) White, L. K.; Chasteen. N. D. J . fhys. Chem. 1979,83,279-84. 167) Seiter. C. H. A.: Anaelos. S. C.: Perreault. R. A . Biochem. Bloohvs. . _ Res. Commun. 1977, 78(3),761-5. (68) Cannistraro, S.;Indovina, P. L. fhys. Med. Biol. 1979, 24(1), 197-8. LITERATURE FOR TABLE 1
(1) Edmondson, D. E. "Biological Magnetic Resonance", Berliner, L. J., Reuben, J., Eds.; Plenum: New York, 1978; Vol. 1. (2) Warden, J. T. Ref. 1. (3) Boas, J. F.; Pilbrow, J. R.; Smith, T. D. Ref. 1, pp 277-342. (4) Eaton, S. S.; Eaton, G. R. Coord. Chem. Revs. 1978,26, 207. (5) Owens, F. J. "Magnetic Resonance of Phase Transitions", Owens, F. J., Pooie. C. P., Jr., Farach, H., Eds.; Academic Press: New York, 1979; Chapter 6. (6) Ingram, D. "Experimental Magnetism", Kalvius, G. M., Tebble. R. S.,Eds.; Wiley: New York, 1979; Voi. 1 (7) Dorio, M. M. Magn. Reson. Rev. 1977,4 , 105-36. (8) Garrett, W. L.; Marinkas, P. L.; Owens, F. J.; Wiegand, D. A. Energ. Mater. 1977, 1 , 285-382. (9) Bullock, A. T. Annu. Rep. Prow. Chem. Sect. B . 7977 1978,90-104; 1976, 73,71-83. (10) Engleman, R.; Halperin. B. Ann. fhys. (faris) 1978, 3 ,453-78. (11) Cavenett, 8. C. J . Lumin. 1979, 18-19; Pt. 2, 846-52. (12) Huettermann, J., JerusalemSymp. Quantum. Chem. Biochem. 1977, 70. 85-98. (13) Weaver, E. C.; Corker, G. A. Encycl. Plant Physiol., New Ser. 1977,5 , 168-1 78. (14) Symons, M. C. R., Annu. Rep. Prog. Chem., Sect. A : Phys. Inorg. Chem. 1977, 73,91-112; Pure Appl. Chem. 1977,49, 13-26. (15) Geist, D. "Boron and Refractory Borides", Matkovich. V. I . , Ed.; Springer: Berlin, 1977; pp 65-77. (16) DeBoer, E., Klaassen. A. A. K.; Mooii, J. J.: Noordik, J. H. Pure A.m. / . Chem. I979?5 1 , 73-83. (17) Tormaia, P. J. Macromol. Sci., Rev. Macromol. Chem. 1979, C17, 297-357. (18j~RoilHnce,D. K. ~ p p l Poiym. . Spectrosc. 1978,207-19. (19) Meybeck, A.; Meybeck, J. Appl. Fibre Sci. 1978, 1, 505-56. (20) Ursu, I.; Lupei, V.; Lupei, A,; Voicu. I.Rev. Roum. Phys. 1979, 24, 229-34. (21) Morton, J. R . ; Preston, K. F. A . C . S . Symp. Ser. 1978,6 8 , 386-409. (22) Kayushin, L. P. Acta Biochim. Biophys. Acta Sci. Hung. 1977, 72, 187-90. (23) Wan, J. K. S.;Wong, S. K. Rev. React. Species Chem. React. 1976, 1, 227-61. (24) Parmon. V. N.; Kokorin, A. I.; Zhidomirov. G. M. Zh. Strukt. Khim. 1977, 18, 132-77. (25) Kispert, L. D. ACS Symp. Ser. 1978, 6 6 , 349-85. (26) Sevilia, M. D. Jerusalem Symp. Quantum Chem. Biochem. 1977, 10, 15-25. (27) Keana, J. F. W. Chem. Rev. 1978, 78, 37-64. (28) Evans, M. C. W. Top. fhotosynth. 1977,2,433-64. (29) Peisach, J. Dev. Blochem. 1978, 7 , 285-306. (30) King, T. E.; Ohnishi, T.; Winter, D. B.; Wu, J. T. Adv. Exp. Bo/.1976, 74, 182-227. (31) Evans, M. C. W. Biochem. SOC. Trans. 1978, 6 , 906-8. (32) Russell, G. A. Aspects Mech. Organomet. Chem. ( f r o c . Symp.) 1978, 59-108; Brewster, J. H., Ed.; Plenum: New York. (33) Beveridge. D. L. Mod. Theor. Chem. 1977,(Semiempirical Methods Electronic Structure Calc., Part B.) 163-214. (34) Wasson. J. R., "Instrumental Analysis", Bauer, H. H.. Christian, G. D., O'Reilly, J. E., Eds.; Allyn and Bacon: Boston, 1978; Chapter 13. (35) Boatmer, L. A.; Abraham, M. M. Rep. frog. fhys. 1978, 4 . 87-155. (36) Dengan. S. K.; Venkataramen, B. R o c . Nucl. Phys. Solidstate fhys. Symp. 1975, 78C,571-5. (37) Gaffney. B. J.; Lin, D. C. Clin. Exp. Ammuno-reprod. 1977,4 , 31-50. (38) Knoles, P. F.: Peake. B. Electron Spin Reson. 1977, 4 . 212-86. (39) Gilbert, B. C. Electron Spin Reson. 1977,4, 11 1-43. (40) Symons, M. C. R . Electron Spin Reson. 1977, 4 , 84-110.
Emission Spectrometry Walter J. Boyko, Peter N. Keliher," and James M. Malloy Chemistry Department, Villanova University, Villanova, Pennsylvania 19085
This is the 17th article in the series of biennial reviews in the field of emission spectrometry/spectroscopy and is the first written by the present authors. This review article will 0003-2700/80/0352-53R$05.00/0
survey selectiuely the emission spectrochemical literature of 1978 and 1979. By agreement, however, flume emission publications are reviewed in the section of this issue entitled 1980 American Chemical Society
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“Flame Emission, Atomic Absorption, and Atomic Fluorescence Spectrometry’’ authored by Gary Horlick. This follows previous custom ( I I A , 51A). Because of the late arrival of some publications appearing in December 1979, we may have missed some references of importance and it is hoped that these will be discussed in the next biennial review. In general, we are following the format used by Barnes (8A-l1A) in previous reviews of the subject. Because of space constraints in this review issue, however, ANALYTICAL CHEMISTRY has asked us to cover the field in a critical selective manner and not to attempt to provide an all-inclusive bibliography. In this fundamental review, the emphasis will be on developments in theory, methodology, and instrumentation. Applications will be cited only insofar as they advance the state of the art or have particular current relevance. References will be cited only if they are of particular importance to analytical chemists and s ectroscopists; articles of primary interest to astronomers an$’or physicists are not, in general (with some exceptions in Section B), cited. Readers should note that detailed and specific application information is available from Analytical Abstracts, Chemical Abstracts, and also the more specific Atomic Absorption and Emission Spectrometry Abstracts published by the PRM Science and Technology Agency (7A). In addition, the latest Application (6A)contains many Reviews issue of ANALYTICAL CHEMISTRY recent spectrochemical application references. Readers should also note the excellent annual series Annual Reports on Analytical Atomic Spectroscopy (32A,33A) published by The Chemical Society, Burlington House, London W1V OBN, United Kingdom. These annual reports provide detailed information on emission spectrometry and are highly recommended to those with an interest in the field. Volume 8, reviewing 1978, has just appeared (33A)and the Editors, J. B. Dawson and B. L. Sham, - . are to be commended for their outstanding effort. In going through the 1978-79 literature. we have selected the fd1ow’;lng puElications as being most relevant, and most emission spectrometry papers published in these journals are cited in this review: Analyst (London),Analytica Chimica Acta, ANALYTICAL CHEMISTRY, Analytical Letters, Applied Optics, Applied Spectroscopy, Applied Spectroscopy Reviews, Canadian Journal of Spectroscopy, CRC Critical Reviews in Analytical Chemistry, Environmental Science and Technology, Fresenius’ Zeitschrift fur Analytische Chemie, ICP Information Newsletter, International Journal of Environmental Anal tical Chemistry, Journal of Chemical Education, Journarof the Optical Society of America, Journal of Quantitative Spectroscopy and Radiative Transfer, Microchemical Journal, Optica Acta, Progress in Analytical Atomic Spectroscopy, Review of Scientific Instruments, Science, Spectrochimica Acta, Part B, Spectroscopy Letters, Talanta, and Water Research. Papers published in unreviewed magazines such as American Laboratory, Industrial Research and Development, Laboratory Practice, etc. are not generally cited. However, where we feel a publication is of fundamental importance, it is reviewed whatever the source. Readers should note that Progress in Analytical Atomic Spectroscopy is a new publication (29A) specializing in interdisciplinary reviews in atomic spectrometry. The first issues have appeared and have set a high standard; the Editor (C. L. Chakrabarti) is commended for his work. Another new plasma newsletter, PlasmaLine, edited by A. T. Zander appeared in late 1979; copies may be obtained by writing to the Editor (97A).
BOOKS AND REVIEWS Several important books and chapters in books have appeared during the past two years. Torok, Mika, and Gegus (88A) have written “Emission Spectrochemical Analysis”; Pinta’s book (71A) “Modern Methods for Trace Element Analysis” has been published as has Hanle and Kleinpoppen’s edited book “Pro ress in Atomic Spectroscopy, Parts A and B” (48A, 49A). rove has edited two volumes of “Applied Atomic Spectroscopy” (45A, 46A). Volume 1 contains five chapters on photographic photometry, volatilization of samples by laser beams, properties of carbon electrodes, behavior of refractory samples, and preparation of standards and samples. Volume 2 contains five chapters on the application of emission techniques to ocean0 raphy, precious metal analysis, petroleum analysis, biome8ca1, and toxicological analysis. Barnes has edited a book (14A)describing various aspects of induc-
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tively coupled plasmas (ICP) to emission spectrometry. In the eight chapters, Barnes reviews the ICP (15A),Browner discusses sampling approaches (%A), Watters and Norris comment on factors influencing precision and accuracy of analysis (92A),Jones and Boyer review food analysis using ICPs (54A), Golightly reviews geochemical applications of ICPs (42A), Abercrombie et al. describe a multielement technique for the collection and analysis of airborne particulates in air quality surveys ( I A ) ,Jones uses an ICP for soil and plant tissue analysis (53A),and Zamechek et al. use an ICP for trace metal analysis in silicon and aluminum (96A). Keliher has written a chapter “Flame and Plasma Emission Analysis” in Volume 1 of “Physical Methods in Modern Chemical Analysis” (56A). The development of direct current plasma (DCP), ICPs, and microwave induced plasmas (MIP) is reviewed. Butler has edited a book (28A) on the analysis of biological materials. This is the proceedings of a conference held in South Africa in 1977 on spectrometry in biological analysis. Risby has edited a book (74A) “Ultratrace Metal Analysis in Biological Sciences and Environment” based on a symposium held a t the 174th meeting of the American Chemical Society in Chicago, Ill., August 29-30,1977, Reeves and Brooks (73A)have published a book covering the sequence of processes necessary in the analysis of geological materials for trace elements. Schuetzle has edited a book (79A)based on a symposium on monitoring toxic substances held during the 174th ACS meeting in Chicago, August 31,1977. The 59th edition of the “CRC Handbook of Chemistry and Physics” has been published (93A)providing much useful spectral data. Two ASTM publications on standards (4A, 5 A ) will also be of interest to emission spectroscopists. Several books largely dealing with atomic absorption spectrometry are also of related interest in emission spectrometry. These include books by Alkemade and Herrmann (2A),Price (72A),and Thompson and Reynolds (85A). Cresser has published a particularly interesting book on solvent extraction in flame spectroscopic analysis (30A). Malissa and Robinson (62A)have edited a book on the analysis of airborne particles by physical methods, and Meek and Craggs (65A) have published the long awaited second edition of “Electrical Breakdown of Gases”. It had been 25 years since the first edition had been published. The book’s 11 chapters are written largely independently by nine physicists and electrical engineers. Despite the diverse authorship, style is maintained consistently throughout and chapter bibliographies only minimally overlap. O’Haver’s chapter on “Wavelength Modulation Spectroscopy” is the definitive work on the subject (67A) and recommended reading. O’Haver has also recently reviewed (68A). Horlick and the subject in ANALYTICAL CHEMISTRY Hieftje have written a chapter on correlation methods in chemical data measurements (52A) emphasizing spectrochemical analysis. The Optical Society of America’s “Handbook of Optics” has recently been published (36A). Several analytical chemistry textbooks have been published during the past two years. Barnes has a particularly wellwritten chapter on “Emission Spectroscopy” ( l 2 A ) in Bauer et al.’s text “Instrumental Analysis”. Kenner and Busch‘s book on “Quantitative Analysis” (57A) has a useful section on emission spectrometry. The 4th Edition (revised by others) of Vogel’s classic book on quantitative inorganic analysis has been published (17A) and contains a section on emission spectrometry. “Wilson and Wilson’s Comprehensive Analytical Chemistry, Volume IX” (84A) has also recently been published and contains a lengthy chapter by Tschopel entitled “Plasma Excitation in Spectrochemical Analysis” (89A). Several significant review articles have appeared during the past two years. Alkemade and co-workers (3A)have reviewed noise and signal ratios in anal tical spectrometry. In a follow-up paper, Boutilier et al. &3A) consider signal-to-noise ratios in more detail. Fundamental reviews in atomic spectrometry have also been published by Kaiser (55A),Goykhman and Gol’dfarb (43A,44A), and Mandelshtam (63A). Morrison’s article on element trace analysis of biological materials (66A) contains a useful section on emission spectrometric techniques. Hydride generation methods for atomic spectroscopic analysis (75A) and rapid scanning in atomic spectroscopic analysis (77A) have also been reviewed.
EMISSION SPECTROMETRY
Bates et al. (18A)have compiled a useful bibliography listing just about every analytical plasma emission publication from 1959 through 1977. This bibliography clearly indicates the explosive owth of plasma emission during the past 20 years. On the suGect of historical perspective, Willis (94A) has reviewed activities in analytical atomic spectroscopy at the CSIRO Division of Chemical Physics where so many important advances were made and Sir Alan Walsh (91A) has published an interesting speculative article entitled “Atomic Spectroscopy-What Next”. The review with the most intriguing title is most definitely “Demand-Pull and SciencePush in Multielement Analysis” by Marvin Margoshes (64A). Margoshes makes several interesting comments on the processes of innovation in the field of multielement analysis.
SPECTRAL DESCRIPTIONS AND CLASSIFICATIONS Walter J. Boyko (left) is a graduate student in the Chemistry Department at Vilhnova University. He received his B.A. degree (1970) from LaSalle College, Philadelphia. After several years industrialand teaching experience, he began graduate studies at Villanova in the autumn of 1978. Mr. Boyko is working toward the Ph.D. degree and is currently studying fundamental processes in direct current and microwave plasmas. Peter N. Keliher (center) is Professor of Analytical Chemistry at Villanova University. He received his A.B. degree (1962) from St. Michael’s College and M S c . (1967) and Ph.D. (1969) degrees from the University of London. Dr. Keliher also holds the Diploma of Membership (D.I.C.) of Imperial College, London. Dr. Keliher has published approximately 35 papers in various areas of analytical chemistry and Is presently Treasurer of the Division of Analytical Chemistry, ACS. Dr. Keliher was 1979 Chairman of the Federation of Anaiytical Chemistry and Spectroscopy Societies (FACSS) Governing Board. James M. Malloy (right) is also a graduate student in the Chemistry Department at Villanova University. He received his B.S.degree (1976) from the University of Scranton. After two years industrial experience, he began graduate studies at Villanova in the autumn of 1978 and is presentiy finishing his M.S. thesis work involving a comparison of continuous (conventional) and discrete nebulization into chemical combustion flames and into direct current plasmas.
The ICP in atomic spectrometry has been reviewed by Fassel (37A, 38A), deGalan (34A, 35A), Barnes (13A, 15A, 16A), Robin (76A), Boumans and co-workers (24A, 25A), Burman and Bostrom (27A),Fischer (39A),Shan (80A),Liang and Zhang (61A),Bogdain (ZIA,22A), and Kornblum (58A). Gast (40A)has compared the ICP and X-ray fluorescence for the determination of trace metals in iron foundry materials. Skogerboe (BIA,82A) has reviewed various multielement techniques for the determination of inorganics in water; Belcher has surveyed various atomic spectrometric methods for the analysis of ferrous material (19A) and metallurgical materials (20A);and Crow and Connolly (31A)have reviewed the analysis of portland cement by spectrometric techniques. Kossowsky has compared various analytical techniques for the analysis of electronic materials (59A),and Topping’s review of various analytical methods for the determination of tungsten includes a section on emission spectroscopic techniques (87A). Gladney et al. have reviewed (41A) element concentrations in U S . Geological Survey Experimental References Samples. Lasers continue to be important in emission spectrometry and analytical chemistry as discussed in a recent ANALYTICAL CHEMISTRY report (60A) on the 32nd Annual Summer Symposium on Analytical Chemistry called “Lasers and Analytical Chemistry” held a t Purdue University, June 27-29th, 1979. Omenetto has edited “Analytical Laser Spectroscopy” (69A), a collection of papers examining the techniques, applications, and future developments of analytical laser spectroscopy. This interesting book examines the physics underlying analytical implementation of lasers in atomic spectroscopy. Hieftje has edited (50A) an ACS symposium series book on new applications of lasers in chemistry; this is based on an ACS Symposium held at the 175th ACS meeting in Anaheim, Calif., March 14-15, 1978. Of related interest, Steinfeld has edited a book “Laser Coherence and Spectroscopy” (83A). The 1978 instrument issue of Science contains three interesting laser articles (47A, 70A, 78A). Topp has recently reviewed pulsed laser spectroscopy (86A), and Wyant has commented on precision optical testing (95A).
The theory of the hyperfine structure of heavy atoms was examined by Sushkov et al. (IIOB).Atomic structure theory was reviewed by Hibbert (56B);and a book on the physics of atoms in atomic spectroscopy, previously mentioned, was published by Hanle and Kleinpoppen (48A, 49A). Sobelman (106B)published “Atomic Spectra and Radiative Transitions”, and Bashkin and Stoner (12%) published the second volume of their atomic energy levels and Grotian diagrams. Wyart (121B)reviewed the present state and trends in the analysis of lanthanide spectra, and Martin et al. (81B) published a volume on the atomic energy levels of the lanthanides. Worden et al. (120B) determined the ionization potentials of the lanthanides by laser spectroscopy. The ionization ener ies for the ytterbium(I1) isoelectronic series were examine2 by Sugar and Kaufman (109B) while Fischer and Hansen (42B) calculated oscillator strengths for the zinc isoelectronic series. Wavelength standards were reviewed by Baird (IOB),and Beck et al. (15B)published a second volume of “Table of Laser Lines in Gases and Vapors”. Outred (92B) compiled a table of over 8000 atomic spectral lines in the near infrared. Fassel and co-workers (119B) presented wavelengths for prominent lines of 70 elements in the ICP. “Tables of Spectral Lines of Neutral and Ionized Uranium Atoms” was published by Korostyleva and Dontsov (68B). Estimates of the wavelengths of two resonance lines in the francium spectrum were calculated by Lundberg and Rosen (75B). Liberman et al. (73B) found first evidence of an optical transition in francium using an atomic beam excited by a tunable laser. Table I presents selective references to atomic spectra including lifetimes, oscillator strengths, transition probabilities, and hyperfine splittings. As in past years (8A-11A), values for molecular and hi hly ionized atomic species are excluded. Oscillator strengtghs for alkali metal atoms were reviewed by Devdariani and Klyucharev, (33B) whereas Newel1 (88B) reviewed the determination of oscillator strengths by electron impact spectroscopy. Brown and Parsons (25B)examined the use of a flame for determining relative atomic transition probabilities; and Fuhr, Miller, and Martin (45B) published a bibliography on transition probabilities. Atomic transition probabilities and lifetimes were reviewed by Wiese ( I 17B). Measurements of lifetimes in a flame were made by Ham and Hannaford (54B),while Martinson (82B),and Curtis (32B) reviewed lifetime measurements. Line shapes in laser-produced plasmas were examined by Jamelot et al. (61B). Behmenburg (17B) and Fuhr, Miller, and Martin (44B) reviewed line shapes. Line broadenings were examined by Birnbaum (19B),Dimitriijevic and Grujic (34B),Lee (72B), Rozshyanai (98B),and Smith (105B). The use of lasers and beam-foil techniques continues to be an active area of interest. Beam-foil techniques were reviewed by Andrae (8B),Bashkin ( I I B ) ,Sellin (100B),and Veje (116B); while lasers were reviewed by Schawlow (78A), Scott and Strasheim (99B), Tayuki and Ohtsu (111B), and Toschek (113B). Finally, Peterson, Anderson, and Parsons (93B) applied the techniques of pattern recognition in spectral classification of the energy levels of curium.
INSTRUMENTATION Optics. In the general category of optics, Busch, Malloy, and Talmi (17C) have investigated multiple entrance slits for simultaneous multielement analysis. Allemand ( I C ) has ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
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Table I. Selected References t o Atomic Spectra Wavelengths ( A ) , Energy Levels (E), Ionization Energy ( I ) , Lifetimes (T), Oscillator Strengths ( f ) , Hyperfine Splittings (hfs), and Transition Probabilities ( A ) ionization ionization ref. element level element level ref. type Sr I 55B, 63B, 77B Li 1-111 h 62B 7 ,f 6.7Li I1 39B, 4OB 69B I1 hfs 7 2 6B 'lZr hfs 41B I Be f 77B 11, I11 Zr 47 B 11, I11 f f Mo I 14B B 89B I E 7 I lOlB 7 41B I Ag 113,115 hfs, isotope shift 122B In 47 B I11 Sn I 87 B C 41 B I f, hfs 84B I, I1 A N 2B I I, I1 112B Sb 7 I 41B I isotope shift Xe 115B I1 46B f I1 97B I 0 41 B 7 f I 74B I A , isotope shift cs 79B, 118B Ne E,I I 90B, 104B 18B. 50B I 7 , hfs hfs Na I1 hfs 5B hfs, isotope shift 53B; 60B I Mg 133,135 ,131CS hfs I1 hfs, isotope shift 49 B 7B 138-142 Cs A1 I 101B, 114B hfs, isotope shift 2 3B f, 7 6B, 57B, 69B Ba 11 7 , hfs, isotope I-XI1 BOB E, I 64B shift , 11-VI1 7 S 27 B A I 4B I La 7 24B, 70B, 78B 111-VI I 7 ,hfs, isotope Sm 36B 7 shift 48B VI1 7 c1 T I1 21B I1 7 65B Ar I 7 Eu 7 I 52B 37B I1 21B 7 7 95B 11, I11 Tb I 13B, 29B Ca hfs 108B I-xx E, I I hfs, isotope shift 58B I1 7 59B DY I1 9B isotope shift cr 1B A 11-VI Mn Er I 35B 1B 111-VI A f I, I1 22B 7 Fe Tm 20B I f I 8 3B h 94B Yb I1 f I 86B 1B 111-VI A Hg f 102B I1 A 107B I, I1 co 7 51B, 96B Bi I 6'Ni E , A , hfs, T hfs 16B 73B, 75B Ni 111-VI I h 1B A Fr isotope shift 66B, 67B I I cu 7 6B U T 235U 91B, 103B hfs 30B I, I1 Zn 7 235 ,233U isotope shift 85B 59B I1 7 Kr I h 3BB, 43B 71B I Cm A, 7 studied the effect of unwanted light in a spectrometer, and Brown and Tarrant (14C) and also Sharpe and Irish (93C) have commented on scattered light in monochromators. Fassel and co-workers (31C) have examined the effectiveness of interference filters for the reduction of stray light effects in atomic emission spectrometry and Boumans (11C) has examined instrumental requirements for ICP spectrometry. Oscillating slit mechanisms were studied by Schwarz et al. (91C), and Leshanskii and Rudnev (60C) used fiber light for lighting the inlet slit of a spectrometer. Scheeline et al. (88C) experimentally characterized straight spectrometer slits and, in related work, Scheeline et al. (87C) investigated the use of a versatile mirror mount for stable optical instruments. Satu et al. (85C) used an umbrella-type dynamic focusing mirror system, and Brown, Jacobs, and Nee (13C) studied parasitic oscillation, absorption stored energy density, and heat density in active mirror and disk am lifiers. Coleman and Walters (228), in a significant paper, designed a large modular optical bed for versatile optical and spectroscopic ex erimentation. Kurochkina and Rubinovich (59C) developeta cathode layer line amplification effect to improve the detection limits for precious metals. In plasma focusing, a method involving beam deviation as a diagnostic tool was developed by Schmidt and Ruckle (89C). Smith et al. (96C) studied integrated bi-stable optical devices while Cann and co-workers (19C) reported on a new multichannel spectrographic attachment. Salmon and Holcombe (83C, 84C) studied an optical system used for gathering simultaneous time and spatial data from transient events and Whitten and Ross (114C) examined fiber optic waveguides for time of flight optical spectrometry. Slodzian (95C) studied transfer optics for microanalysis by secondary ion emission. Mitev et al. (65C) made a study of current signals in the vacuum ultraviolet region, and 56R
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Hjortsberg, Chen, and Burnstein (47C) used a resonant internal-reflection prism with surface guided and Fabry-Perot electromagnetic waves in spectrometry. Glassner et al. (40C) examined a new interactive method of Abel inversion applied to plasma spectrometry. Zembutsu and Fukunishi ( 1 1 8 0 commented on wavelength properties of selenium and sulfur based glass films and their application to optical wavelength devices. Pollard's thesis (782) describes the design, automation, and optimization of a wavelength modulated multielement AE/AF spectrometer system. Dupoisot and Prat (30C) have constructed a high resolution interference spectrometer while corrections of optical distortion have been studied by Hemela (45C) and automatic compensation of spectral interference developed by Prudnikoiv and Shapkinzi (76C). Palmer et al. (74C) have developed a system for the automatic measurement of spectrograms. Chapman and Gordon (21C) developed a procedure to correct drift in a photoelectric spectrometer. Holcombe (51C) has described an inexpensive reflective image rotator, and Horlick and Yuen (52C) have constructed a modular Michelson interferometer for Fourier transform spectrochemical measurement. Tarrant (104C) has developed an interesting optical technique for studying stray light in spectrometers. Verrill (113C) has also measured stray light in spectrometers. Moos et al. (66C) have reported on the construction, calibration, and ap lication of a compact spectrometer for plasma diagnostics; anfRose, Caruso, and co-workers (77A,81C, 82C) have applied an oscillating mirror rapid scanning system for multielement atomic spectrometry. Their source was a MIP. Wolcott (115C) has devised an entrance slit mask for use with a step filter or sector. The mask allows exposure of a preselected portion of the eight steps which reduces the height of each spectrogram and permits more exposures per plate.
EMISSION SPECTROMETRY
Gratings. Instruments based on echelle gratings are being used more frequently in analytical atomic spectrometry. A typical echelle grating monochromator will have approximately an order of magnitude greater resolving power than a conventional monochromator of comparable focal length (56A). Zander and Keliher (117C) have recently examined the spectral efficiency of a commercially available echelle grating monochromator. Skogerboe and Urasa (94C, 112C) have studied, in some detail, the analytical capabilities of a DCPechelle spectrometer system. Felkel and Pardue (32C)have interfaced an echelle spectrometer with an image detector and silicon vidicon tubes for simultaneous multielement determinations. Felkel (33C)evaluated various detectors coupled to an echelle grating spectrometer, and McKeith et al. (64C) have developed a new Cassegranian echelle spectrograph. Gustavsson and Ingman (44C) have performed atomic fluorescence and atomic emission measurements with an image dissector echelle spectrometer. Ostrowski and Chashchin (73C) studied and evaluated a holographic Fourier spectrometer. The effects of the relative phase relationships of gratings on diffractions from thick holograms were examined by Tsukada et al. (107C). The effects of scattered light and holographic interferences were studied by Ng et al. (69C) and also by Francis et al. (34C). Grating incidences have been examined by various workers in some detail, e.g., Soerensen (98C),Arakawa et al. (3C), Garifo and co-workers (38C), Malvezzi and Tondello (63C), and Brauninger and co-workers (12C). Basu (5‘2) studied rating filters in thick film optical waves and Basu and ballantyne (4C) examined random fluctuations in first-order wavelength grating filters. Knop (58C) studied diffraction gratings for color filtering in the zero diffraction order and Namba and Aoyagi (68C) developed an ion beam method for producing echelette gratings. Seligson and Baumeister (92C) developed a phenomenological theory of a buried diffraction grating, and Derrick et al. (28C) studied the theory and application of crossed gratings. Loewen and Neviere (62‘2) commented on simple selection rules for VUX and XUV diffraction gratings, and Bykouski et al. (18C) developed three-dimensional diffraction ratings with oblique layers in thin-film optical waveguides. ivakhin et al. (102C) studied the process of diffraction grating formation a t the optical waveguide surface. Johnson (55C) studied the evolution of spectral profiles under ion beam erosion, and Carius e t al. (20C) performed spectral analysis with a JENA 1000 double grating monochromator. Several new types of spectrometers were produced revolvin around grating technology. Gerasimova and Bogdanov (39C7 developed a vacuum high intensity spectrograph with a flat diffraction lattice for the 120-700 nm spectral region. Klueppel et al. (57C) developed a spectrometer for time-gated spatially resolved study of repetitive electrical discharges. Titus (1062) developed a rapid scanning spectrometer for chemical investigations. Strojek and Uziel (100C) constructed a rapid scanning mirror spectrometer, and Henry (46C) designed a variable resolution spectrometer for a multichannel system. As noted earlier, Rose and co-workers (77A, 81C, 82C) have also constructed rapid scanning systems. Detectors. Recent work has focused on photodiode as well as on vidicon type detectors. Snow (97C) has developed self-scanning photodiode arrays, and Bubert et al. (15C,16C) have studied a linear silicon photodiode array consisting of five photodiodes each having a separate output. The signal-to-noise ratios of systems using the photodiode array and of a photomultiplier (EM1 9789 QB) were compared. Rapid scanning photodiode arrays for nickel and cobalt were examined by Anderson et al. (2C). Betty and Horlick (9C)produced a correlation readout system for a photodiode array spectrometer. Gorbachev and co-workers (41C) examined a spectrometer with a vidicon for investigation of the contour of spectral lines. Hoffman and Pardue (48C, 49C) used vidicon detectors for improvement of a stacked spectral display and characterizing performances of the vidicon spectrometer with autoranging amplifiers. Darland et al. (25C, 26C) described a high-speed, direct current-coupled pulse counter that could be constructed with readily available integrated circuits for less then $150. Boedeker (10C) also developed a detector for multiple collection. Hofman and Emers (50C) have used differential light detec-
tors, and Muller and co-workers (67C) have published an interesting paper on a method (the evaporation of liquid Freon) to simultaneously cool light detectors and light sources. Robinson et al. (80C) have used a sensitive streak camera as an emission detector, and Corrons and Zalewski (23C) have studied the response of detectors a t low (350-1200 nm) wavelengths. Talmi (103C)has reported on recent applications of optical multichannel spectrometric systems. Betteridge et al. (7C)have used a gallium phosphide light-emitting diode and a silicon phototransistor as a light sources and sensor, respectively. The output current from the phototransistor is converted into voltage by a novel current-to-voltage converter. Using the term “detector” in a slightly different sense, emission spectrometric systems are becoming increasingly popular as detectors in chromatography (56A, 90A). Uden, Barnes, and co-workers (61C, 77C, 78C, 110C, 1 l l C ) have several significant papers in this area. They have used both direct current plasmas (DCP) and microwave induced plasmas (MIP) in their work, and both plasmas may be used with gas chromatographic systems. Because of solvent effects, however, the MIP cannot be used with HPLC systems but the DCP has been successfully interfaced (111C). Reamer, Zoller, and O’Haver (79‘2) have used a MIP as a detector for the gas chromatographic determination of tetraalkyllead species in the atmosphere. The lead 405.78-nm line was monitored. Schwarz (9OC) used a MIP for the quantitative determination of various organic materials monitoring the hydrogen line a t 656.28 nm. Sommer and Oh19 (99C) have used an ICP as a chromatographic detector. In somewhat related work, Belcher and co-workers ( 6 C ) have used Molecular Emission Cavity Analysis (MECA) as a chromatography detector. Sample Introduction. Methods for reproducibly introducing samples into “atom reservoirs” continue to be of interest, and the most significant papers are discussed here. Nebulizers for sample introduction into ICPs have been described by Donohue and Carter (29C),Uchida and co-workers (108C,109C), Wolcott and Sobel (116C),and Suddendorf and Boyer (101C). Savage and Hieftje (86C) have reported enhanced nebulization effects through the application of an electric field. Gustavsson (43C)has commented on aspects of nebulizer characteristics in ICPs. Denton and his colleagues a t the University of Arizona (35C-37C) have three particularly interesting papers on various aspects of sample introduction. In one publication, they describe a new microsampling cone (37C)for capillary pneumatic nebulization. Although their system is used with a premixed (flame) burner, it could be useful in plasma emission spectrometry. In another paper, Fry and Denton (35C)describe a high solids nebulizer that is actually able to accommodate tomato sauce without clogging. A third paper (36‘2) describes an improved hydride preconcentration system for ICP spectrometry. Cresser (24C)has described an interesting impact cup used in conjunction with a pneumatic nebulizer that increases the useful working range (in flame spectrometry) by a factor of twelve. The “Cresser Cup” should find some uses in plasma emission spectrometry in cases where workers are dealing with high analyte concentrations. Computer Interfacing. The effect of computers in emission spectrometry is increasing every year. In an important paper, Defreese and co-workers (27C)have described a relatively inexpensive microcomputer-controlled monochromator accessory which provides split beam, dual wavelength capability as well as radiometric compensation for source fluctuation at a single wavelength. The microcomputer controls the selection of both wavelengths and also performs other control and computation functions for the spectrometer system. Kawaguchi (56C) has developed a programmable monochromator for the simultaneous determination of several elements. Jackson and Priest (54C) have discussed general applications of computers in optical spectrometry, and Granrath and Hunt (42C) have commented on signal detection using Fourier transform techniques. Niemczyk and Ettinger (70C)have described a computercontrolled photon counting spectrometer used for rapidly scanning low light level spectra. Hornshuh (53C) has used microprocessor control to optimize a silicon vidicon detector system. Nomura and co-workers (71C)have developed a new computational method of spectral line shape analysis. The ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
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parameters of object functions were found to fit the experimental values on the basis of a nonlinear least squares method. A computer-based microdensitometry system has been used by Bettison and Bundy (8C),and Ostertag (72C) has developed a microprocessor-based spectroscopic picture processing system. Thomas (105C) has used a minicomputer for spectrographic analysis.
STANDARDS, SAMPLES, NOMENCLATURE, CALIBRATION, CALCULATIONS The June 1978 (Volume 33, Number 6) issue of Spectrochimica Acta, Part B contains three important IUPAC documents reprinted from past issues of Pure and Applied Chemistry. These were reprinted with the permission of the IUPAC Secretariat and after consultation with V. A. Fassel, Chairman of the Commission on Spectrochemical and Other Optical Procedures for Analysis, the person responsible for the formulation of these IUPAC rules. “Nomenclature, Symbols, Units and Their Usage in Spectrochemical Analysis” is broken down into three sections on “General Atomic Emission Spectroscopy” (210),“Data Interpretation” ( 2 2 0 ) , and “Analytical Flame Spectroscopy and Associated NonFlame Procedures” (230). These should be read by all workers in the field of emission spectrometry. Hirsch’s book on “Statistics” ( 1 2 0 ) offers guidance to chemists in the application of experimental design and statistical methods. Ratzlaff and co-workers (260-280) have discussed optimization of accuracy and precision, and Thorburn Burns ( 3 4 0 ) has provided a general guide to sources of information on the nomenclature and evaluation of analytical methods. Goode and Northington ( 1 1 0 ) have studied systematic errors in flame atomic emission spectrometry and Delaney et al. ( 5 0 ) have compared several signal-to-noise enhancement techniques. Dybczynski and co-workers ( 7 0 ) have commented on accuracy and precision in the determination of trace elements in water, and Balslev et al. ( I D ) reported on noise amplification and resolution improvement in deconvolution of experimental spectra. Meites ( 1 9 0 ) has reviewed new techniques for the analysis and interpretation of chemical data, and Falk and co-workers ( 8 0 ) have presented some theoretical considerations on trace analysis by atomic emission spectrometry. Olscheske and Walters ( 2 4 0 ) have studied the capabilities of a disk based microcomputer system and adapted a sophisticated modeling program for emitting and absorbing plasma discharges into it. McQuaker et al. ( 1 8 0 )have calibrated an ICP system for the analysis of environmental materials, and Prudnikov (250) has made some general comments on the choice of the spectral instrument in plasma and flame emission spectrometry. In order to avoid any ossible confusion regarding American (lo9) and European (107 2 ) usage of the term “billion”, Koch ( 1 6 0 ) has proposed a new unit for trace analysis, pp lox. Johnson ( 1 3 0 ) describes a method for the rapid calculation of vacuum wave numbers, and Florian and Matherny ( 9 0 ) have used a computer in the determination of transformation parameters. The book “Evaluation and Optimization of Laboratory Methods and Analytical Procedures: A Survey of Statistical and Mathematical Techniques” (17 0 ) was published in 1978 and is recommended reading. The 1979 edition of the “Standard Reference Material Catalog” (320) contains useful information on the topic. Tuell et al. ( 3 6 0 )have compared standards for the determination of trace wear metals in jet engine oils and Stoeppler et al. (330) have reviewed standards for trace and ultratrace metal and metalloid analysis. Tolg (350)has commented on some new methods for the analytical characterization of high-purity materials. In the field of water analysis, growing importance is being attached to the ability to compare, with confidence, the results from different laboratories. Wilson ( 3 7 0 ) has described an approach for achieving comparable analytical results from a number of laboratories, and Neider ( 2 0 0 ) has reviewed international cooperation in the field of reference materials. Cali ( 3 0 ) has discussed the role of reference materials in the laboratory, and Christie ( 4 0 ) has evaluated several reference materials. Boumans ( 2 0 ) has reviewed some elementary concepts in the statistical evaluation of trace element measurement, and DeVilliers ( 6 0 )has prepared small quantities of copper standards for emission spectrographic analysis. Knott et al. ( 1 5 0 ) have compared synthetic calibration 58R
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standards for OES and XRF. Ryan and Holzbecher ( 3 0 0 ) have prepared filter paper standards for trace analysis. Staats ( 3 1 0 ) has commented on calibration and calibration control in an iron works laboratory. Woodyard and co-workers ( 3 8 0 ) at the Federal Bureau of Mines have developed a mathematical expression for the emulsion calibration curve used in optical emission spectrometry. In a related paper, Zimmer and Heltai ( 3 9 0 ) have studied the effect of properties of microdensitometers on the shape of the characteristic curve of the photographic emulsion. Klockenkamper and Beuck ( 1 4 0 ) have studied grain sensitivity for photographic emulsions. Gardner (100) discusses requirements for clean rooms for trace metal analysis and, in a paper with the fascinating title “On the Care and Feeding of Analytical Chemists”, Rose (290) makes interesting comments on the choice of number of samples for analysis, blind samples, and general data reporting. This is a very well written “fun” paper.
EXCITATION SOURCES Arc Discharges. A number of interesting papers have appeared during the past two years. Rautschke et al. (139E) have studied vaporization processes in a DC arc. Decker and Kobus (38E, 39E) have shown that the temperature of the anode s ot of a DC arc is, under given conditions, determined largely y! two factors: the temperature at which the metal of the buffer compound volatilizes and enters the arc plasma and the energy required to effect this volatilization. Vukanovic and co-workers (179E) have used a high speed camera to observe the process of plasma formation and rotation in a graphite tube and Ikonomov et al. (75E) have used mass spectrometry to investigate the plasma composition in a DC arc. Fakhry et al. (53E) have studied the effect of an external magnetic field on the volatilization of elements in the DC arc, and Krasnobaeva et al. (92E) studied the axial distributions o the effective temperature and electron pressure in the presence of various additives in air and argon with barium nitrate as the additive in a DC arc. Heinrich and co-workers (68E) have performed plasma spectroscopic studies on alternating current arc discharges in methane. Operating parameters such as current intensity, electrode gap, and methane filler gas pressure were varied. Petrakiev and Oreshkov (136E) have studied the influence of lithium on the axial distribution of thallium in an arc discharge, and Lowry and Strube (105E) have determined carbon by DC arc spectrometry using copper electrodes. Kuzyakov et al. (94E) have calculated the degree of dissociation of monoxides and fractions of free zirconium and hafnium atoms in an arc plasma, and Hogrefe and Lowry (69E) have used an arc technique for the quantitative analysis of thin films. Dittrich and Vogel (41E) compared DC arc excitation, flameless AAS, and flameless AFS for the determination of trace tellurium in small semiconductor samples. Flameless AAS was the preferred method owing to lower detection limits. Sugimae and Skogerboe (161E) determined fluoride in geological materials by formation and excitation of calcium fluoride in a DC arc, and Apsher ( 5 E ) developed a DC arcpowder technique for the determination of several metals in magnesium alloys. Murty and Kaimal (123E)used a similar technique for the determination of trace impurities in high purity cadmium, and Eskenazy and Mincheva (51E) used arc emission for the determination of trace amounts of indium in minerals and rocks. KO (88E) developed a single-carrier method for the emission spectrometric analysis of uraniumplutonium oxides. Direct Current Plasmas (DCP). Skogerboe and his research associates at Colorado State University have published several significant papers in this area during the past two years. As mentioned previously, Skogerboe and Urasa (94C) have evaluated the analytical capabilities of a two-electrode inverted “V” type DCP used in conjunction with an echelle spectrometer. Detection limits were reported to be equivalent or superior to those characteristic of flame AAS and often competitive with those obtained with ICP systems. Johnson, Taylor, and Skogerboe (79E) characterized spectral interferences associated with a DCP-20-channel direct reading echelle spectrometer and reported that spectral interferences were less severe than those reported (by other workers) for an ICP-conventional (non-echelle) direct reading spectrom-
EMISSION SPECTROMETRY
eter. Reednick (140E) has recently described his firms‘ (SpectraMetrics) three-electrode DCP which is an inverted “Y” type plasma. The plasma is formed between two spectrographic carbon anodes and a tungsten cathode, the cathode forms the “leg” of the Y. Johnson, Taylor, and Skogerboe (8OE)com ared the two-electrode and three-electrode plasmas and f o u n f the three-electrode DCP to be superior to the two-electrode DCP in terms of improved stability and lower background. In another publication, Johnson, Taylor, and Skogerboe (78E)reported that solute vaporization interference effects, previously reported using the two-electrode DCP (94C), were minimal when using the three-electrode DCP. Ellebracht e t al. (48E) have used a DC plasma for the determination of sulfur. Sulfur resonance lines in the vacuum UV (180.7, 182.0, 182.6 nm) were monitored using a simple optical purge system to reduce light absorption by oxygen. The DCP coupled with the purge system and appropriate optics and detection equipment enabled the determination of total sulfur in aqueous solutions with the same sensitivity for different sulfur species. A detection limit of 0.5 ppm and a linear dynamic range of 2000 ppm sulfur were reported. In a related paper, Swaim and Ellebracht (1633) used hydrogen sulfide evolution into a DCP for sensitive (10 ng) sulfur determination. Nygaard (130E)and also Gilbert (57E)used DCP emission spectrometry to determine trace heavy metals in salt water matrices and Bankston et al. (10E) have used a DCP for the determination of several elements (at various concentration levels) in silicate rocks. Chemically diverse standard reference rocks were used both for calibration and assessment of accuracy. Braman and Tompkins (21E) have used a DCP for the determination of antimony, germanium, and methylermanium compounds while Eastwood and co-workers (44E) ave used DCP emission spectrometry to study hazardous chemical and oil spills. Cox and Cox (35E)have reported on the suitability of DCP emission spectrometry for the determination of trace metals in marine waters. Several workers have used DCP emission spectrometry for the determination of boron in various materials: Melton et al. (112E)in plants, Burdo and Snyder (28E)in glass, Mifune e t al. (115E) in thermal waters, and Ball et al. (9E) in fresh and estuarine water samples. Kubota (93E) has reported on the effects of major constituents on the emission intensities of 18 elements in a DCP and Holclajtner-Antunovic and co-workers (70E) have proposed a model to establish the axial distribution of added substances in a DCP. Sutton and co-workers (164E) have compared DCP emission and flameless AAS for trace elements in precipitation samples, and Griffon and McNulty (63E)used DCP emission spectrometry for the determination of impurities in lead and high-lead alloys. Miyazaki et al. (116E) determined arsenic in sediments by chloride formation and DCP emission spectrometry, and Fairless (52E)has surveyed several important industrial applications of DCPs. Hollow Cathode Discharges. Mehs and Niemczyk (111E) have designed a system which rapidly and conveniently measures the electron temperature in a hollow cathode discharge. The measurement system is based upon the floating double probe technique. Torok and Zaray (170E, 171E) have commented on current-voltage characteristics of a low-temperature analytical hollow cathode discharge tube, and Broekaert (23E) has studied sample volatilization of copper-base alloys in a hot-type hollow cathode. Intensity vs. time curves for lead, zinc, tin, and copper during the excitation of brass and bronze were measured with the aid of a vidicon spectrometer. Kitagawa, Narita, and Takeuchi (85E) have developed a heated electrode discharge lamp for trace analysis by emission spectrometry, and Caroli and Delle Femmine (32E) studied the voltage-current characteristics of hollow cathode and glow discharge light sources under varying experimental conditions. Ehlers and Leung (47E) discuss some physical properties of tungsten filaments when operated as cathodes in a gas discharge and Zhechev et al. (188E) have developed discharge tubes with transparent hollow cathodes. Dyulgerova and Zhechev (43E) described the electrical and spectroscopic properties of a new type of hollow cathode discharge tube. A conical bottom tube was used instead of the more conventional flat bottom tube resulting in significant enhancement of the spectral line intensity of the cathode material but not of the
fl
inert gas discharge. Murayama et al. (121E) have designed a new spectral-line source, a high frequency discharge lamp with a hollow cathode. The width of the spectral line emitted was comparable to that of a conventional HCL. Beenen, Lessard, and Piepmeier (13E) have compared laser-induced impedance changes in DC and pulsed hollow cathode lamps. The induced signal, observed as a change in lamp voltage, was increased by factors from 1.7 to 650 when the lamp was operated in the pulsed mode. Spectral line broadening due to laser induced saturation was greater in the DC mode. Harrison and Bentz (65E) have described an interesting dual-discharge ionization source, and O’Haver, Harnly, and Zander (131E) have compared the radiant power of an Eimac xenon arc lamp and an HCL source. Several workers have continued development of hollow cathode discharges for use in AAS and AFS, and the most significant papers are discussed here. Niemczyk and Erspamer (128E)have described methods for the preparation of cathodes for use in demountable HCLs, and Myers (124E)has designed a coaxial boosted-output HCL for AAS. Sullivan and coworkers (42E,162E, 163E) have also designed boosted-output HCLs for AAS and AFS. Wolfe and Vickers (183E) have optimized pulsing conditions for HCLs used in AFS,and Tsijii et al. (172E) have described HCLs for the AAS and AFS determination of cadmium, lead, and zinc. Finally, Blank and Pepper (16E) have used a demountable HCL as a light source for the alignment of the secondary slits of an emission spectrometer. Inductively Coupled Plasma Discharges (ICP). As is well known, ICP discharges have become increasingly popular in analytical chemistry during fhe past decade and there are many significant papers in this area that have appeared during the past two years. It is perhaps appropriate to be in with “Detection Limits-1978’’ authored by Boumans and Barnes (18E)listing detection limits that can currently be obtained with ICP sources. Boumans and Bosveld (19E)have published a tentative listing of the sensitivities and detection limits of the most sensitive ICP lines as derived from the fitting of experimental data for an argon ICP to the intensities tabulated for the National Bureau of Standards copper arc. Horlick (71E) has commented on spectral characteristics of ICPs, Greenfield and McGeachin (60E)have performed calorimetric and dimensional studies on ICPs, Newland (126E)has commented on line selection and background correction in ICPs, Motley et al. (118E)have described a high density pulsed ICP, Schleicher ( 150E) has performed a detailed investigation of theoretical and experimental aspects of ICPs as spectrochemical sources, and Mermet (113E) has discussed interference effects in ICPs. Berman and McLaren (14E) have published a preliminary report on the establishment of compromise conditions for multielement analysis using an ICP, and, in a particularly interesting paper, Demers (40E) has evaluated an axially viewed (end-on) ICP which he reported to be easier to align optically and to be better suited for simultaneous multielement analysis than the conventional (side-on) ICP. Ediger and Wilson (46E)have interfaced an ICP and an atomic absorption spectrometer (Perkin-Elmer Model 5000) and concluded, not surprisingly, that ICP detection limits are much better than flame AAS detection limits and that chemical and ionization interferences are much less using the ICP. However, they also state that additional background and spectral interferences are evident with the ICP that do not affect flame AAS. Greenfield and Thorburn Burns (61E) have discussed criteria to be used when comparing plasmas as emission sources, and they were able to show that detection limits are not necessarily reliable indicators of relative intrinsic merits of plasma sources. Zeeman et al. (187E) determined temperatures in a 9.2 MHz ICP using the rotational lines of the N2+band system to evaluate the temperature of the plasma tail flame a t various heights above the load coil. These varied from approximately 8000 K at 17 mm above the coil to 6400 K at 41 mm above the coil. Larson and Fassel (95E),in an important paper, have observed that spectral line broadening and radiative electronic recombination processes may make significant contributions to the total spectral background level when ICPs are observed with spectrometers having low stray light levels. For some elements, such as magnesium, linear Stark-broadened lines produced spectral background a t unexpectedly large disANALYTICAL CHEMISTRY, VOL. 52,
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placements from the line center. Hassell et al. (66E,67E) have discussed a method to reduce stray light effects of magnesium in an ICP, and Kitagawa, Koyama, and Takeuchi (84E) have developed a four-line method for correction of inter-element effects on excitation and ionic processes in ICPs. Broekaert e t al. (24E) have discussed matrix effects in the analysis of rare earth minerals by ICP spectrometry, and Boumans et al. (20E) have outlined a method for general survey spectrographic analysis using an ICP. Allemand and Barnes (2E)have designed a fixed-frequency impedance matching network for an ICP. Plasma impedance is determined by a substitution method in conjunction with the matching network model. Windsor and co-workers (182E) have designed a high power ICP and impedance matching network. Salin and Horlick (14423) have devised a direct sample insertion device for an ICP, and Bogdain (17E) has described an improved nebulizer for ICP spectrometry. Schutyser and Janssens (152E)have evaluated various spray chambers for use with ICPs, and, in a particularly interesting short note, Scott (154E) describes a new method for introducing powders directly into an ICP. The method uses a spark discharge between two graphite electrodes situated above the powder Sam le for the elutriation of fine particles from the sample. Rogin and co-workers (76E,77E) have continued their spectrometric study of a 40-MHz ICP, and Schramel and Ovcar-Pavlu (151E)have commented on the dependence of the signal from an ICP on the acid concentration of the sample solution. Kirkbright and his research colleagues at Imperial College, London, have continued their in-depth ICP studies ( l E ,64E, 82E, 83E, 167E, 168E). Gunn, Millard, and Kirkbright (64E) have described a system in which a graphite rod electrothermal vaporization device is employed for the introduction of microliter liquid samples into an ICP, and Kirkbright and Snook (82E) have used the system to introduce refractory compound-forming elements such as boron, molybdenum, zirconium, chromium, and tungsten into an ICP. Kirkbright and co-workers (167E, 168E) have used a gaseous hydride introduction method for the simultaneous determination of trace amounts of arsenic, antimony, bismuth, selenium, and tellurium by ICP spectrometry, and Kirkbright and Tinsley (83E) have determined platinum metals and gold by ICP emission spectrometry. In related work, Thompson and Pahlananpour (166E)have used a hydride generation technique to determine tin and germanium by ICP spectrometry. Because of the relatively high operating expenses (in terms of argon flow and power consumption) associated with conventional ICPs, there has been some recent activity in designing miniaturized ICP systems. In an important paper, Savage and Hieftje (145E) have developed and described a miniature ICP, given a preliminary report of its analytical capabilities, and directly compared it to a conventional (maxi-) ICP. The Savage-Hieftje mini-ICP is 33% smaller than a conventional ICP. I t was reported to be very economical to sustain requiring less than 1 kW of rf power, approximately 33% less than the conventional ICP to which it was compared. The mini-ICP used about 8 L min-’ of argon coolant gas, approximately 50% of the flow associated with the conventional ICP to which it was compared. Detection limits, multielement capabilities, plasma temperatures, and other analytical capabilities were similar for the two plasmas. However, the authors report that the mini-ICP possesses some unique operating characteristics which simplify sample introduction. In a related paper, Sexton, Savage, and Hieftje (I55E) have used hydrodynamic flow atterns as a simple aid to effective ICP torch design. Kornglum et al. (91E) have reduced argon consumption 10-fold in an ICP by adding a water-cooled jacket. Two designs were described and evaluated. Allemand, Barnes, and Wohlers (3E) have studied ICP discharges with 13-mm torches and 9-mm torches and compared these with the conventional 18-mm torch. The detection limits obtained with the 13-mm torch were roughly equal to those obtained with the 18-mm torch and those obtained with the 9-mm torch were similar or poorer. The power and argon gas consumption of the smaller torches was, of course, less than that of the standard 18-mm torches. ICP methods have been developed for many practical applications including the determination of tungsten (184E), waste water analysis ( 173E),glass fragment analysis (33E), determination of metals in oils (114E),determination of 60R
ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
platinum group metals and gold in ores and related plant materials (83E, 180E), and the analysis of geological ( I I9E) and biological (37E) materials. Nikdel et al. (129E) have reported rare earth detection limits in an ICP and Windsor and Denton (181E) have used an ICP for the elemental analysis of organic compounds. Fraley et al. (56E)have used an ICP as a specific HPLC detector. Ohls and Sommer (133E) have used an ICP for the analysis of compact samples, and in another paper (132E) they describe an interesting air-argon ICP. Winefordner and his research associates a t the University of Florida have used an ICP for analytical and diagnostic studies involving AFS. In one publication (134E),they studied the characteristics of the emission line profiles of cadmium, zinc, and magnesium in an ICP using AFS. In another paper (138E),they studied AFS in an ICP using a continuum dye laser. In another paper (49E) they used an ICP as a narrow line radiation source for the excitation of AFS in several analytically useful flames including nitrogen separated airacetylene and nitrous oxide-acetylene. Detection limits for 14 elements were compared to AFS detection limits using other radiation sources and to those of other atomic spectrometric techniques. The technique was applied t o the determination of zinc in fly ash, cadmium and zinc in simulated fresh water, and co per and zinc in orange juice. Montaser (117E)has also useIan ICP as an excitation source for flame AFS. The ICP has also been used in flame atomic spectrometry in other ways. Magyar and Aeschbach (106E) have coupled an ICP with an AAS system for the analysis of substances which decompose with difficulty in flames, and Koirtyohann and Lichte ( N E )have observed that the high intensity of some emission lines from an ICP can give rise to Rowland ghosts which can interfere with nearby analytical lines when spectrometers with mechanically ruled gratings are used. They solve the problem by using flame AAS as a specific filter to reduce both the parent line and the ghost intensity, thereby reducing the interference. Microwave Discharges. There has been recent interest in improved cavity designs for microwave induced plasma (MIP) spectrometry, and Beenakker and Boumans (11E)have reported some additional characteristics of the cylindrical TMolo(Beenakker type) cavity. They comment on how optimum performance of an argon MIP generated with this cavity can be obtained. Beenakker, Bosman, and Boumans (12E)have used a crossed-flow pneumatic nebulizer with spray chamber in con’unction with a MIP (Beenakker type cavity) and determined the detection limits of 15 elements using 23 spectral lines. Detection limits were reported satisfactory but not as good as ICP detection limits. Interferences were less serious than in a capacitively coupled microwave plasma (CMP) but far more prominent than in an ICP. Mulligan et al. (120E) compared several microwave cavities for the simultaneous determination of arsenic, germanium, antimony, and tin by MIP emission spectrometry and they concluded that the Beenakker type cavity was the easiest to tune and to o erate. Furthermore, it also provided the most reprod uci ! le results. Van Dalen et al. (175E)have described some technical improvements to facilitate the operation of a cylindrical TMlo cavity. By improving the frequency tuning, the impedance matching, and the microwave power couplin of the cavity, it became possible to sustain plasmas under wiiely different conditions with a single cavity. Zander and Hieftje (185E,186E) have observed that the Beenakker type cavity is a durable, stable, and highly efficient excitation source for the emission spectrometric determination of metallic elements. The authors comment that the cavity is easy to ignite and operate and uses low volumes of inert support gas. They note that the Beenakker type cavity MIP shows a significant improvement over other versions of microwave cavities in terms of its tolerance of sample and solvent material. The high temperature of the Beenakker-MIP leads to increased ionization and population of higher excited states; this result requires careful choice of emission lines to be used for analytical measurements. An important advance of the Beenakker type cavity is its ability to sustain an atmospheric pressure helium discharge. The Beenakker type cavity will undoubtedly find increasing usage in the future. In a paper with the fascinating title “Aerosols, Aerodynamics, and Atomic Analysis”, Skogerboe and Olson (157E)
EMISSION SPECTROMETRY
have studied the suppresion of atomic excitation in a MIP (using a modified Evenson cavity) due to the presence of sodium. Three different nebulization systems were used. The results indicated that the sodium suppression effects observed can be largely accounted for by reductions in the analyte transport efficiency due to changes in the aerodynamic characteristics of the aerosol resulting from variations in the salt content of the nebulized solutions. It was further shown that these effects may be generally predicted on the basis of fluid mechanical principles and that these may be used to design systems to eliminate the interferences. Skogerboe and Olson’s important study underscores the essentiality of considering aerodynamic factors in formulating mechanistic explanations for interference effects in plasmas and also in flames. Leis and Laqua (96E) used a laser beam focused onto a specimen to vaporize sample material from a small area. The vapor formed was then introduced into a MIP. In related work, Leis and Laqua (97E)described a rectangular resonant cavity (TEIo2)for the excitation of laser produced vapor in a microwave discharge. The authors investigated the influence of the argon pressure on the intensity of spectral lines and on line-to-background ratios. From relative intensities of Fe I lines, an excitation temperature of 4530 h 100 K was calculated. Murphy and Brophy (122E) have designed a microwave discharge source for the production of intense beams of atomic, radical, and metastable species in vacuo. Brassem et al. (22E) have studied nonthermal excitation in a MIP a t 0.2 Torr, and Crowe and Goldberg (36E) have described a simple automatic initiator circuit for MIPs. The circuit operates by sensing the power reflected from the microwave cavity. Jutte and Agterdenbos (81E)have commented on the use of incident power meters of microwave generators, and Caldwell et al. (30E)have described a simplified method for sealing tungsten electrodes into quartz for MIP usage. Andrews et al. (4E) have described windowless argon discharge tubes, and Schwarz (9OC, 153E) has characterized atomic hydrogen emission in a MIP. Hubert, Moisan, and Ricard (73E) have described a new type of atmospheric pressure microwave plasma. The plasma is obtained by surface wave propagation with a surfatron. The plasma is produced within a quartz tube and is constricted to a diameter of approximately 1 or 2 m m but its length can attain some tens of centimeters with microwave power as low as 100 W. The plasma is reported to be quite uniform along the axis with a typical electron density of 3 X 1014 electrons/cm3. Goulden and Salter (59E) have developed an automatic emission spectrometer for the determination of nitrogen-15. The nitrogen flows in a helium stream through a Broida-MIP and the emitted radiation is analyzed by means of a specially constructed dual-wavelength monochromator and the intensities of the 14N14N(297.7 nm) and I4Nl5N (298.3 nm) bands are measured simultaneously by two photomultipliers. Robbins, Caruso, and Fricke (142E)have determined germanium, arsenic, selenium, tin, and antimony in complex samples by a hydride generation technique used with a MIP and Van Montfort et al. ( 1 77E, 178E) have continued their studies of sample introduction into sealed MIPs, i.e., electrodeless discharge lamps (EDLs). Lifshitz et al. (98E)have described improved high intensity EDLs for AAS and AFS. Spark Discharges. Walters and his co-workers a t the University of Wiscodsin have continued their fundamental studies of spark discharges and several very important papers have appeared during the past two years. Experimental results have been presented (87E) of time and spatially resolved Schlieren studies on the formation of an atmospheric pressure, positionally-stabilized, spark discharge. Results are documented a t repetition rates extending into the kHz region for a pulsed unidirectional discharge sampling current. Scheeline, Coleman, and Walters (147E) have presented a method for calibration of electronic adjustable waveform capacitor discharge spark sources. Both individual component measurements and system measurements were discussed. In a related paper (148E), equations and a calculation procedure for modeling the operation of an electronic, adjustable-waveform, and other types of high voltage spark sources were presented. Comparisons between laboratory and computed results indicated that the calculations predict experiment with accuracy in the 1 to 5% relative error range. This was reported suf-
ficient to make the calculation procedure useful for characterization of research or production spark sources. Scheeline and Walters (146E, 149E) investigated bipolar spark discharges in order to determine whether the two cathodic vapor plumes successively created would mix, and, if so, whether energy transfer between the plume species would occur. Vapor mixing was observed and changes in sampling or excitation mechanisms were also indicated. The authors discussed possible reasons for the changes in emission patterns. Araki and Walters (6E) have described an electrical adjustable waveform current generator for use with a quarter wave resonant spark source and have also (7E)described transient ionic and atomic emission-absorption measurements on a train of positionally-stable copper spark discharges. The results indicated that electrode vapor moves primarily along the interelectrode axis in response to current duration with substantional ionization remaining in the post-discharge period. Neutral atoms were reported to remain in the gap for long times after current cessation. Rentner (141E)has investigated a new type of atmospheric pressure spark discharge for spectrochemical analysis. Strasheim et al. (160E) have compared medium voltage (MV) and high voltage (HV) controlled waveform spark sources as light sources for the analysis of aluminum alloys in an argon atmosphere using a sequential spectrometer. The controlled waveform HV spark source generally yielded better reproducibilities in intensity and intensity ratio than the MV source for the spectral lines used, but the MV source appeared to be slightly more sensitive for very low concentrations of elements and the reproducibility in these concentration determinations was better than the HV source. Matrix effects were similar in both sources, and the authors commented that it was necessary to use very high purity argon for satisfactory results. Nickel et al. (127E)have used an auxiliary spark gap in conjunction with laser-micro-emission spectrometry, and Malamand, Daigne, and Girard (107E) used a very intense electric discharge to ensure the melting, vaporization, and excitation of the material to be analyzed. A new design vacuum grating spectrograph was also described. The paper gives a detailed description of the instrumentation and also reports results of practical analyses with particular reference to steel, titanium alloys, and super-alloys. Lisienko et al. (99E) have studied the spark method of analyzing aerosols of solutions generated by a simple pneumatic nebulizer, and Bubert, Hagenah, and Laqua (15C) have used spark excitation in chemical analysis. As noted previously, Scott (154E) has used spark elutriation for solids analysis in an ICP. Coraor (34E) has investigated the liquid-layer-on-solid sample spark technique, and Koeplin (89E) has used a spark emission detector for gas chromatography. In related work, Sacks and co-workers (143E,20F, 21F, 58F) have continued their studies of short-time radiative processes in exploding metal film and foil plasmas, and McKeever et al. (1lOE) have used a Tesla discharge as a spectroscopic source. Glow Discharge Lamps (GDL). Bystroff, Layman, and Hieftje (29E)have studied the operatin characteristics of a “microarc” atmospheric-pressure glow Jischarge. The stepby-step events occurring in the discharge were explained qualitatively, and a variety of processes were invoked to explain sample volatilization (including sputtering), chemical reactions, and purely chemical effects. The authors reported improved stability by uniformly depositing multielement samples along the electrode, which localizes the initial discharge and promotes ablative cooling of the sample and electrode. Van Calker and Denk (174E) have described a method for measuring the mass and energy distribution of the ion current a t the cathode of anomalous glow discharges, and Berneron (15E) has used a GDL to characterize the surface layer composition of steel products. Pille et al. (137E) have studied internal standardization in the analysis of fine gold with a Grimm-GDL and, in related work, Human et al. (74E)analyzed metals using a GDL with a fluorescent atomic vapor as spectral line isolator. Bubert, Hagenah, and Laqua (27E) have used a Grimm-GDL to determine aluminum, carbon, magnesium, and silicon in various powder samples, and Ferreira and Butler (55E) have used a Grimm-GDL to determine gold, platinum, palladium, and certain base metals in silver. Accuracy and limit of detection results were reported acceptable. ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
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E M I S S I O N SPECTROMETRY
Feldman (54E) has described improvements in the arsine accumulation-helium glow detector procedure for determining traces of arsenic and, in a related paper, Horton, Jenkins, and Feldman (72E) have used a helium GDL as a gas chromatographic detector selective for silicon. Naganuma et al. (125E) have used a Grimm-GDL for the analysis of aluminum alloys, and Asada and co-workers (8E)have also used a Grimm-GDL for general spectrochemical analysis. Gough and Sullivan (58E) have used a boosted GDL source with a polychromator for metal analysis, and Harrison and co-workers (25E,26E) have interfaced GDL sources and mass s ectrometers. O t h e r Excitation Papers. Eckert (45Ephas discussed the theory of trace element determination from a static thermal induced plasma, and Grey Morgan (62E) has commented on single micro-particle and atomic particle detection. Sharp (156E) has published a note on the laser remote sensing of atmospheric pollutants, and Capelle and Sutton (31E) have described metatable transfer emission spectroscopy (MTES) as a simple and relatively inexpensive new technique for qualitative and quantitative measurements. McGonagle and Holcombe (109E) commented on microphotometric errors for photographically recorded spectral lines, and Van Deijck et al. (176E) have described a laser microprobe analyzer as a tool for quantitative analysis in atomic emission spectrometry. Kitagawa, Shigeyasu, and Takeuchi (86E) have applied the Faraday effect to the trace determination of cadmium, and Stephens has commented on the Faraday effect (158E) and also on the Voigt effect (159E) in atomic spectrometry. A paper by Torok and Hafenscher (169E) deals with the interference effect of scattered li ht in a microphotometer. Atomic emission from carbon urnace atomizers continues to be studied with most of the work being done a t the University of Strathclyde (Scotland) by Littlejohn and Ottaway (100E-104E). Investigations have shown (101E) that atomic emission intensities are dependent upon the diffusive and thermal conductivity properties of the furnace purge gas and that the differences in emission signal for a particular species in argon, helium, krypton, and nitrogen arise mainly through variations in the atom vapor concentration rather than from changes in excitation conditions. In related work, Ottaway and Shaw (I35E)have determined various elements in steel by carbon furnace atomic emission, and Matousek and Smythe (108E)have studied lithium furnace emission. Epstein et al. (50E) have determined several trace metals in simulated fresh water by carbon furnace atomic emission spectrometry.
P
SELECTED APPLICATIONS As indicated previously, reviews and compilations of practical emission spectrochemical applications can be found in the "Annual Reports on Analytical Atomic Spectroscopy" (32A, 33A) and in the Application Reviews of this Journal (6A). For that reason, we are being particularly selective in this section. A g r i c u l t u r a l , Clinical, Environmental Materials. David (I 7F) has reviewed atomic spectrometric techniques for the analysis of soils, plants, fertilizers, and other agricultural materials. Mauras and Allain (39F) have determined barium in water and biological fluids, and Pawlaczyk and Makowska (52F) have analyzed dru s. Burridge and Hewitt (I4F) and also Soltanpour et al. ( 6 4 4 have analyzed soils and plants. Garbarino and Taylor (25F) and also Moselhy et al. (45F) have developed multielement emission techniques for environmental samples. Melton et al. (112E) determined boron in plants, Broekaert and Leis (11F)developed an injection method for the determination of boron and several metals in waste-water samples, Hirano et al. (%F) determined various metals in shells, and Sin'kov and Minaeva (63F) have determined several metals in biological materials. McHard, Winefordner, and co-workers have published two interesting papers on the determination of metals in orange juice. In one study (41F),four atomic spectrometric methods were compared, flame-AAS, flame-AES/AFS, DCP emission spectrometry, and ICP emission spectrometry. Substantial differences between methods were observed with re ard to speed, convenience, precision, detection limits, an$ interretation of analytical calibration curves near the detection kkits. In general, however, the four methods all gave plausible agreement in the values obtained. It was reported that flame-AAS and DCP emission spectrometry were most con6 2 R * ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
veniently handled by a sin le operator. Both ICP emission spectrometry and f l a m e - A b / AFS were less convenient as far as wavelen t h selection and sample manipulation. In another paper, k c H a r d , Foulk, and Winefordner (40F) used DCP emission spectrometry (using a three-electrode plasma) to determine Florida and Brazil orange juice concentrates for the purpose of comparing their inorganic elemental content in order to distinguish them. Most of the elements tested were in similar concentration ranges in juice samples from the two geographical region. A few, when compared to ratios to zinc as a reference element, showed geographic differences. Barnes and Genna (7F) used a poly(dithi0carbamate) resin to separate and concentrate ten trace metals in urine, and Allain and Mauras (5F) developed an ICP method for the determination of aluminum in blood, urine, and water. McQuaker et al. (42F) have commented on digestion procedures of environmental materials with respect to digest acid content, digestion efficiency, and precision and accuracy. Aleksandrov et al. (4F) have determined metals in slime samples. Geological Materials. Burman and Bostrom (1327) compared different dissolution and calibration methods for the analysis of geological materials using both an ICP and a CMP. Severe matrix effects were noted for the CMP but the matrix effects in the ICP were very low. The ICP was reported to have annoying nebulizer disturbances when concentrated solutions were used but, with properly diluted solutions, all major and many trace elements could be routinely determined in 50-mg rock samples. Broekaert, Leis, and Laqua (12F) determined rare earth elements in mineralogical samples using an ICP and reported detection limits in the 0.1-30 ng mLrange. It was observed that a high resolving ower spectrometer is required to make full use of the I8P power of detection. Miyazaki, Kimura, and Umezaki (44F) have used DCP emission spectrometry to determine arsenic in sediments and Bhale et al. (8F)have determined barium and strontium in geological samples. Barakat and co-workers (6F)have utilized adhesion on active charcoal to determine gold traces in rocks, and Russell and Watson (57F) have commented on the analysis of chromium-bearing materials with particular reference to ferrochromium slags and chromite ores. Watson and Russell ( 7 0 0 have described a rapid and convenient method for the determination of a number of trace elements in geolo ical samples. The technique involves the diluting of a samp?e in the ratio of one part of sample to three parts of a buffer consisting of graphite containing 20% lithium fluoride and 0.03% germanium oxide as an internal standard. The mixture is loaded into a special electrode and excited in a DC arc a t 12 A for 80 f 2 s. Dale (15F) has developed an emission spectrographic method for the determination of boron in silicate materials. His method is also based upon the use of a lithium fluoride-graphite buffer with germanium as internal standard. Uchida, Uchida, and Chuzo (67F)have determined several major and minor elements in silicates, and Eskenazy and Mincheva (22F) have described a method for the determination of gold, platinum, rhodium, and iridium in geological and other materials by a combination of fire-assay preconcentration and emission spectrography. The technique was reported to be simple and rapid. Botto (9F) has described an automatic fusion device for coal ash ,analysis, Scott et al. (62F) have used an ICP for the analysis of ferro-manganese ores, and Kozuchowski (34F) has developed a method for the determination of mercury in sediments. Metals. Ward and Marciello (68F) have described a technique for analyzing metal alloys in which samples are acid-dissolved before analysis. Because a concentration ratio method is used for analysis, dilution errors of up to 40% can be tolerated without significant loss of accuracy. The ICP technique was used to determine 17 elements in irons and steels, 14 elements in copper-based alloys, and 12 elements in aluminum alloys. Akiyoshi and Tsukamoto (3F) and also Brauner (1OF) have reported im roved methods for the determination of boron in steel, anaAkatsuka and Atsuya (2F) have used an u.h.f. plasma torch for the determination of molybdenum in iron and steels. Various other workers (IF, 18F, 30F, 49F, 54F, 66F,76F) have also described methods for the determination of metals in steel samples. Govindaraju and Quaida (26F) have determined titanium, iron, aluminum,
EMISSION SPECTROMETRY
and manganese; and Kantor, Fodor, and Pun or (32F) have used arc-nebulization in conjunction with AA8 to determine traces of lead, cadmium, and zinc in copper. Lamela et al. (36F) determined various impurities in copper, Mannweiler (37F) reported on the determination of impurities in aluminum, and Kitazume et al. (33F) determined traces of copper in tantalum. Sakamoto et al. (59F) used a low-wattage MIP to determine trace amounts of aluminum in magnesium, and Piatek et al. (53F) have described some interelement effects in the analysis of aluminum brasses. Dalvi et al. (16F) have used carrier distillation and emission spectrography for the determination of tantalum, hafnium, niobium, thorium, and tungsten in uranium and, in related work from the same laboratory, Page et al. (50F)discuss improved spectrographic methods for trace elements in uranium. Schelpakowa and co-workers (60F) compared DC arc emission and flameless-AAS for the determination of trace elements in GaAs. Absolute and relative detection limits were better using flameless-AAS but the advanta e of emission was its multielement capabilities. Duchane ancf Sacks (20F,21F, 58F) have determined several trace elements in micro samples using exploding thin-film excitation. Sugimae and Skogerboe (65F) have described a method in which atmospheric particulates are collected on a high-purity graphite filter disk and analyzed initially by point-to-plane spark excitation and finally by DC arc excitation. Imai et al. (29F) have also used emission spectrometry to determine trace metals in atmospheric particulates, and Watson and Russell (69F)have described a high-power ICP source for general metallurgical analysis. Other Applications. Wise, Burdo, and Sterlace (73F) have reviewed atomic spectrometric techniques for the determination of elements in glass and ceramics, and Schroth (61F) has used an ICP technique for the analysis of ceramic materials. Wolcott and Woodworth (74F) have commented on sampling techniques for pure quartz and glass in order to reduce surface contamination. Nickel et al. (48F) have used a laser-micro-emissidn technique for the analysis of graphite, and Pap (51F) and also Krakovska and Matherny (35F) have analyze1powders by emission spectrometry. Matsumoto (38F) has determined nonmetallic elements by helium excited plasma spectrometry, Muchkaev et al. (46F) have described a complex method for determining oxygen in gases, Dittrich and Abel (19F) have used an emission spectrographic method to determine traces of nitrogen in GaP and GaAs, and Ricard and Lefebvre (55F) used emission spectrometry for the determination of impurities in helium. Jones’s thesis (31F) describes the optimization and application of reduced-pressure MIPS for gas phase analysis, and Yanagisawa, Kawaguchi, and Vallee (75F) used a reduced-pressure (helium discharge) MIP to characterize metal chlorides, nitrates, and sulfates. Fernandez and Bastiaans (23F) have described an interesting ICP-emission spectrometric method for the determination of elemental stoichiometries of a class of complex inorganic ions. The precision of the method was reported to compare very favorably with conventional colorimetric determinations of stoichiometry for the compounds. Middelboe and Johansen (43F) have described a simple and reasonably accurate method for the optical analysis of 12C I3C ratios in carbon dioxide, and Newman and Farrow (47F) ave reported on general applications of the ICP in chemical industry. Windsor and Denton, in two interesting papers, have determined empirical formulas (72F) with an ICP gas chromatographic system and also (71F)performed elemental analysis. Robbins and Caruso (56F)have analyzed selected elemental hydrides by chromatographically coupled microwave plasma emission spectrometry and also used their system for metal speciation (24F).
L
MEETINGS I t seems appropriate to finish this review by making some general comments about important meetings. As wisely pointed out by Hieftje and Copeland (51A),trends and events of importance can be readily recognized from the important biennial Colloquium Spectroscopicum Internationale-International Conference on Atomic Spectroscopy (CSI-ICAS) conferences. The most recent meeting took place in Cambridge, England, from July 1st throu h 6th, 1979, and several hundred papers were presented. Tge quality of the papers
was very high and the recent emphasis on plasma emission spectrometry clearly evident. The next CSI-ICAS will be held in Japan in September of 1981. Detailed information regarding the 1981 CSI-ICAS meeting can be obtained from The Japan Society for Analytical Chemistry, Gotanda Sanhaitsu, 26-2 Nishgotanda 1-chome, Shinagawa-ku, Tokyo 146, Japan. The 1978 American Chemical Society national meetings were held in Anaheim, Calif., and in Miami Beach, Fla. and the 1979 meetin s were held in Honolulu, Hawaii, and in The Honolulu meeting was held jointly Washington, D. with the Chemical Society of Japan and two important symposia of particular interest to emission spectroscopists were held during the joint meeting. Professor Velmer A. Fassel, Iowa State University, was the recipient of the ACS Award in Analytical Chemistry (Fisher Award) and a two-day symposium was arranged in his honor. In his award address, Professor Fassel discussed the simultaneous or sequential determination of the elements at all concentration levels and described the historical development of the ICP. The award address has recently been published (38A) and is certainly recommended reading. Professor John P. Walters, University of Wisconsin, was the 1979 recipient of the Chemical Instrumentation Award sponsored by the Division of Analytical Chemistrv. ACS. There was also a svmDosium in his honor - . a t the Hdnolulu meeting. The 1978 and 1979 Pittsburgh Conferences were held in Cleveland, Ohio, but the 1980 Geeting has moved to Atlantic City, N.J. This is a very large, continually growing, conference with a very extensive exhibition of scientific equipment. The Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) meetings have developed, over the past few years, into highly regarded North American meetings held annually in the autumn. The 5th FACSS meeting met in Boston, Mass., in October 1978, and the most recent 6th FACSS meeting was in Philadelphia, Pa., in September 1979. Approximately 400 papers in all areas of analytical chemistry and spectroscopy were presented. Interested readers may obtain copies of the 6th FACSS program and abstract booklets by writing to one of the authors (P.N.K.) of this review. The next two FACSS meetings will also be held in Philadelphia, the 7th FACSS from September 28th through October 3rd, 1980, and the 8th FACSS from September 20th through 25th, 1981. The 27th Canadian Spectroscopy Symposium has been conveniently scheduled to follow the 1980 FACSS and will be held in Toronto from October 6th through 8th, 1980. This important three-day conference is sponsored by the Spectroscop Societ of Canada. The Knnual gymposium on the Analytical Chemistry of Pollutants continues to alternate between the United States and Europe. The 9th Symposium was held at Jekyll Island, Ga., in May 1979, and the 10th Symposium is scheduled to be held in Dortmund, Germany, from May 28th through 30th, 1980. The 8th International Microchemical Symposium will be held in Graz, Austria, from August 25th through 30th, 1980, and there will certainly be many presentations of interest to emission spectroscopists. During the same week, August 25-30, San Francisco hosts the Second Chemical Congress of the North American Continent, co-sponsored by several societies including the American Chemical Society. G. M. Hieftie and P. N. Keliher have organized a one-day symposium entitled “Atomic Spectroscopy for the 80’s” for this meeting. Invited speakers include R. F. Browner, V. A. Fassel, G. Horlick. S. R. Koirtvohann. R. K. Skoserboe. cJ. Van Loon. and J. P. Wdters. . Finallv. it should be noted that the Annual Reworts on Analyti&l Atomic Spectroscopy (32A, 33A) lis& papers presented at all of the major meetings in a particular year. Full author addresses are given allowing interested persons to directly contact the author for more information. This provides a very useful service.
8.
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ACKNOWLEDGMENT The following all helped, in various ways, in the preparation of this review and we wish to thank them here: Mark Asteris, Suzette T. Avetian, Ramon M. Barnes, Mary Ellen Borkowski, Edward G. Brame, Jr., James J. Cleary, Malcolm S. Cresser, Bernard J. Downey, John Farino, Mary L. Finley, Walter V. Gerasimowicz, William L. Greene, Jr., Howard A. Harner 111, A. Thomas Kashuba, Bonnie M. Keliher, Mark Keliher, Claire ANALYTICAL CHEMISTRY, VOL. 52, NO. 5, APRIL 1980
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Keliher, Gordon F. Kirkbright, James J. Markham, Joseph S. McDonnell, George Norwitz, and Andrew T. Zander.
DEDICATION This review is dedicated, with respect and affection, to the memory of Tsugio Takeuchi (1914-1979), Professor of Chemistry a t Nagoya University, Japan. Professor Takeuchi was the Japanese coordinator at the Fisher Award Symposium held during the joint ACS-CSJ meeting in Honolulu, Hawaii. Professor Takeuchi died suddenly soon after the presentation of his paper on the atomic Faraday effect during the CSI-ICAS meeting in Cambridge, England. Professor Takeuchi was internationally known for his research in various areas of analytical spectrometry and he will be missed by us all. LITERATURE CITED BOOKS AND REVIEWS
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(155E) Sexton, E.: Savage, R. N.: Hieftje, G. M. Appl. Spectrosc. 1979, 33, 643-646. (156E) Sharp, B. L. Proc. Anal. Div. Chem. SOC. 1979, 16, 197-199. (157E) Skogerboe, R. K.; Olson, K. W: Appl. Spectrosc. 1978, 32, 181-187. (158E) Stephens, R. Can. J. Spectrosc. 1979, 2 4 , 10-17. (159E) Stephens, R. Can. J. Spectrosc. 1979, 24, 105-111. (160E) Strasheim. A.; Scott, R. H.; Walters, N. M.; Oakes, A. R. Spectrochim. Acta, Part B 1978, 33, 447-462. (161E) Sugimae, A.; Skogerboe, R. K. Anal. Chem. 1979, 5 1 , 884-888. (162E) Sullivan, J. V. Anal. Chim. Acta 1979, 105. 213-218. (163E) Sullivan, J. V.; VanLoon, J. C. Anal. Chim. Acta 1978, 102. 25-32. (164E) Sulton, D. C.; Morse, R. S.;Legotte, P. A,; Rosa, W. C. Environ. Meas. Lab. Environ. 0.1979, 356,381-414. (165E) Swaim, P. D.; Ellebracht, S.R. Anal. Chem. 1979, 51, 1605-1609. (166E) Thompson, M.; Pahlavanpour, B. Anal. Chim. Acta 1979, 109, 251-258. (167E) Thompson, M.; Pahlavanpour. B.; Walton, S. J.; Kirkbright, G. F. Analyst (London) 1978, 103,568-579. (168E) Thompson, M.; Pahlavanpour, B.; Walton, S. J.; Kirkbright, G. F. Analyst (London) 1978, 103,705-713. (169E) Torok, T.; Hafenscher, I. Spectrochim. Acta, Part B 1978, 33, 283-290. (170E) Torok, T.; Zaray, Gy. Spectrochim. Acta, Part61978, 33, 101-113. (171E) Torok, T.; Zaray. Gy. Spectrochim. Acta, Part 6 1978, 33, 115-121. (172E) Tsijii, K.; Kuga, K.; Murayama, S.; Yasuda, M. Anal. Chim. Acta 1979, 111, 103-109. (173E) Uchida, H.: Neaishi. - R.; Yamazaki. R.; Imai. Y. 6unsekiKaaaku - 1979, 28, 244-248. (174E) Van Calker, J.; Denk, H. J. Spectrochim. Acta, Part B 1979, 34, 151-157. (175E) Van Dalen, J. P. J.; DeLezenne Coulander, P. A.; DeGalan, L. Spectrochim. Acta, Part B 1978, 33, 545-549. (176E) Van Deijck, W.; Balke, J.; Maessen, F. J. M. J. Spectrochim. Acta, Part B 1979, 34, 359-369. (177E) Van Montfort, P. F. E.; Agterdenbos, J.; Denissen. R.; Piet, M.; Van Sandwijk, A. Spectrochim. Acta, Part B 1978, 33,47-52. (178E) Van Montfort, P. F. E.; Agterdenbos, J.; June, B. A. H. G. Anal. Chem. 1979, 51, 1553-1557. (179E) Vukanovic, J.; Vukanovic, D.; Simic, M. Spectrochim. Acta, Part B 1978, 33,481-487. (180E) Wemyss, R. B.; Scott, R. H. Anal. Chem. 1978, 5 0 , 1694-1697. (181E) Windsor, D. L.; Denton, M. B. Appl. Spectrosc. 1978, 32,366-371. (182E) Windsor, D. L.; Heine, D. R.; Denton, M. B. Appl. Spectrosc. 1979, 33, 56-58. (183E) Wolfe, T. C.; Vickers, T. J. Appl. Spectrosc. 1978, 32, 265-268. (184E) Wunsch, G. Talanta 1979, 26. 291-295. (185E) Zander, A. T.; Hieftje, G. M. NTIS Rep. No. ADA051 17812 GA. 1978. (186E) Zander, A. T.; Hieftje, G. M. Anal. Chem. 1978, 5 0 , 1257-1260. (187E) Zeeman, P. B.; Terbhnche, S. P. Appl. Spectrosc. 1978, 32,572-576. (186E) Zhechev, D.; Komltov, L.; Tonchev, E. Spectrosc. Lett. 1978, 11, 423-426. SELECTED APPLICATIONS
(1F) Adrain, R. S.;Airey, D. R. IEE Conf. Pub. 1978, 165. 70-73. (2F) Akatsuka, K.; Atsuya. I. Anal. Chim. Acta 1978, 99, 351-356. (3F) Akiyoshi, T.; Tsukamoto, T. Bunseki Kagaku 1978, 2 7 , 85-89. (4F) Aleksandrov, S.; Gyulmezova, G.; Sanabria, J. Dokl. Bolg. Akad. Nauk 1978, 31, 73-76. (5F) Allain, P.; Mauras, Y. Anal. Chem. 1979, 51. 2089-2091. (6F) Barakat, N.; Abou ECNour, F. Fresenius' Z . Anal. Chem. 1978, 289. 367. (7F) Barnes, R. M.; Genna, J. S. Anal. Chem. 1979, 51, 1065-1070. (8F) Bhaie, G. L.; Awar, K. H.; Rao. P. M. R.; Naik. R. C. Fresenius' Z . Anal. Chem. 1978, 293, 223-224. (9F) Botto, R. I.ICP Inf. Newsl. 1979, 5. 223-241. 1978. 49. 183-187. (IOFI . - , Brauner. J. Arch. Eisenhuettenwes. ( I l F ) Broekaek J. A. C.; Leis, F. A n i . Chim'. Acta 1979, 109, 73-83. (12F) Broekaert, J. A. C.; Leis, F.; Laqua, K. Spectrochim. Acta, Part B 1979, 34,73-84. (13F) Burman, J. 0.; Bostrom, K. Anal. Chem. 1979, 51. 516-520. (14F) Burridge, J. C.; Hewitt, I.J. Commun. Soil Sci. Plant Anal. 1978, 9 , 865-872. (15F) Dale, L. S . Appl. Spectrosc. 1979, 33,404-406. Deodhar, C. S.; Sheshagiri, T. K.; Khalap, M. S.;Joshi. (16F) Dalvi. A. G. I.; 8. D. Talanta 1978, 25, 665-668. (17F) David, D. J. Prog. Anal. At. Spectrosc. 1978, 1, 225-263. (18F) Diemiaszonek, R.; Moulton, J. L.; Trassy, C. Analusis 1979, 7, 96-103. (19F) Dittrlch, K.; Abei, G. Talanta 1978, 25, 41-43. (20F) Duchane. D. V.; Sacks, R. D. Anal. Chem. 1978. 5 0 , 1752-1757. (21F) Duchane, D. V.; Sacks, R. D. Anal. Chem. 1978, 5 0 , 1765-1769. (22F) Eskenazy. G. M.; Mincheva, E. 1. Analyst (London) 1978, 103, 1179-1 181. (23F) Fernandez, M. A.; Bastiaans. G. J. Anal. Chem. 1979, 51, 1402-1406. (24F) Fricke. F. L.; Robbins, W. D.; Caruso, J. A. J. Assoc. Off. Anal. Chem. 1978, 61, 1118-1123. (25F) Garbarino, J. R.; Taylor, H. E. Appl. Spectrosc. 1979, 33, 220-226. (26F) Govindaraju, K.; Quaida, M. B. Analusis 1978, 6, 460-462. (27F) Harris. A. M.; Lengton, J. 8.; Farreli, F. Talanta 1978, 25, 257-262. (28F) Hirano. M.; Onuma, N.; Masuda, F. BunsekiKagaku 1979, 28,313-318. (29F) Imai, S.; Kusaka, H.; Tsuji, H.; Hishiya, Y. Anal. Chim. Acta 1979, 108, 103-1 11. (30F) Janosikova. V.; Charvat, K. Hutn. Listy 1978, 33, 741-743. (31F) Jones, D. G. Diss. Abstr. Int. B 1979, 40,709. (32F) Kantor, T.; Fodor, P.; Pungor, E. Anal. Chim. Acta 1978, 102,15-23. (33F) Kitazume, E.; Sakamoto, T.; Kawaguchi. H.; Mizuike, A. Bunseki Kagaku 1978, 27, 566-570. (34F) Kozuchowski. J. Anal. Chim. Acta 1978, 99, 293-297. ~~
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Anal. Chem. 1980, 52, 6 9 R - 7 5 R (35F) Krakovska, E.; Matherny, M. Chem. Zvesfi 1979, 33, 240-251. (36F) Lamela, M.; Patlno, S. A.; Huelva, S. Rev. Mefal(Madrid) 1978, 74, 158-161. (37F) Mannweilsr. U. Aluminium (DusseMorf) 1978, 5 4 , 765-767. (38F) Matsumoto, K. Kagaku (Kyoto) 1979, 34,314-316. (39F) Mauras, Y.; Allain, P. Anal. Chim. Acta 1979, 170, 271-277. (40F) McHard. J. A.: Foulk. S. J.: Winefordner. J. D. J. Aaric. Food Chem. 1979, 27, 1326-1328. (41F) McHard, J. A.; Foulk, S. J.; Nikdel, S.; Ullman, A. H.; Pollard, B. D. Anal. Chem. 1979. 57. 1613-1616. (42F) McQGke;, N. k.;-Brown, D. F.; Kluckner, P. D. Anal. Chem. 1979, 51, 1082-1084. (43F) Middleboe, V.; Johansen, H. S. Appl. Specfrosc. 1978, 32,511-513. (44F) Miyazaki. A.; Kimura, A.; Umezaki, Y. Anal. Chim. Acta 1979, 107, 395-398. (45F) Moselhy, M. M.; Boomer, D. W.; Bishop, J. N.; Diosady, P. L.; Howlett, A. D. Can. J. Spectrosc. 1978, 23, 186-195. (46F) Muchkaev, A. A.; Nemets, V. M.; Petrov, A. A. Zavod. Lab. 1979, 45. 326-329. (47F) Newman, E. J.; Farrow, R. N. Roc. Anal. Div. Chem. Soc.1978, 75, 311-315. (48F) Nickel, H.; Peuser, F. A,; Mazurkiewicz, M. Specfrochim. Acta, Parf B 1978, 33,675-692. (49F) Niklna, 0. I.; Garevaya, A. E.; Sharapov, I. S.; Popov, Yu. F.; Polupanov, V. I. Zavod. Lab. 1979. 45, 127-129. (50F) Page, A. G.; Godbole, S. V.; Kulkarni, J.; Shelar, S. S.; Joshi, 8 . D. Fresenius’ Z . Anal. Chem. 1979. 297, 388-392. (51F) Papp, L. Appl. Spectrosc. 1978, 32,247-249. (52F) Pawlaczyk, J.: Makowska, M. Acfa Pol. fharm. 1979, 36, 59-62. (53F) Patek, K.; Mueller, E.; Lachowski, M. Pr. Insf. Met. Niezebz. 1978, 7 , 43-48.
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Nucleonics W. S. Lyon” and H. H. Ross
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Analytical Chemistry Division, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37830
Writing this review at the end of the 60’s ( I ) we said, “The technological accomplishment of the decade-landing men on the moon-was followed by return of lunar samples to the Lunar Receiving Laboratory which was designed and directed by scientists and engineers trained in the nuclear field’. How, in the 1970’s, have we followed that act? Perhaps we can paraphrase our 60’s statement as follows: “The technological nonaccomplishment of the decade-the slowing down and essentially dismantling of the nuclear power industry-was climaxed by the return of samples of radioactive water from Three Mile Island (2) to Oak Ridge National Laboratory where the decontamination problem was being studied by engineers and radiochemists trained in the nuclear field”. We cannot help but recall the lines from Pope’s “Essay on Man”: “Atoms or systems into ruin hurled And now a bubble burst, and now a world.”
peared in the nucleonics heaven, but on the other hand, no visible diminution of its scientific light has been noted either. The editors of this journal have asked the authors of these review articles to include some information on the new SI units appropriate to their review topic. In ow 1978 review, we noted the controversy surrounding the acceptance of the new units and questioned the logic behind some of the changes. However, we find that we can no longer hold back the on-rush of SI unit future shock and, therefore, suggest a close perusal of Table I(3). Detailed reports from the International Commission on Radiation Units (ICRU Report No. 23-26) d’ISCUSS the evolution and definition of the new units. A report to the International Congress of Radiology summarizes the ICRU activities since 1973 (4). We still expect, of course, to see some negative comments on the new units; one of the more whimsical observations appeared in the poetic form of “imperial metre” (5). Activation Analysis. Activation analysis continues to play an important role as an analytical and investigative tool, but as we have noted in previous reviews, advances are now mainly incremental in nature. Forensic applications continue to attract attention; for example the reopening of the President Kennedy assassination case has resulted in a re-examination of the bullet fragments found a t the crime site (6). Modern GeLi detectors were used to measure the activation products, but results were essentially the same as reported in 1964. Several data-collecting and evaluation type papers have appeared such as those on glasses (7) and paper and oil (usin pattern reco nition) (8). The field in general was discussej in a Fisher Ecientific Award Lecture in 1978 (9), and that will-0-the-wisp, hair, was chased yet another time with the usual inconclusive results ( I O ) . Closely related to forensic applications is nuclear archaeometry; a typical application is dating great basin petroglyphs (11). And activation analysts have grown bolder-now they are carrying out in vivo applications for oxygen ( I 2 ) ,calcium ( I 3 ) ,and nitrogen (14). They are also continuing to use large machines such as synchrotrons for XRF (15). A proton microprobe with a focusing spot of 2 X 2 pm2 has been reported from Germany (16);this
The period covered by this report-November 1977-November 1979-was indeed a time of systems into ruin hurled, but the nonbursting of the apparently nonexistent bubble on T M I may portend better things for our world. At least the world of nucleonics has survived, even prospered, as environmental and ener considerations continue to demand the attention of the r a g c h e m i s t . Proof of this is shown in the accompanying tables, which as usual list books, reviews, conferences, and proceedin s that are of interest to nucleonics. Readers will note that we fist many conferences in Table IV for which we have not located a published proceedings. We do this to alert you to the possibility that such proceedings may be published in the near future or that they may already exist in some printed form. Papers continue to appear in a variety of journals and listed below are some examples of the typical and, where indicated, some rather novel, special, or outstanding contributions. No wonderous new star has apResearch sponsored by t h e O f f i c e of E n e r g y Research, U.S. D e p a r t m e n t o f E n e r g y u n d e r C o n t r a c t W-7405-eng-26 w i t h t h e U n i o n C a r b i d e Corporation.
0003-2700/80/0352-69R$01 .OO/O
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1980 American Chemical Society
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