Anal. Chem. 1982, 5 4 , 188R-203R (609) Yusupov, M. Yu.; Israilov, M. A.; Skrebtsova, N. V.; Pachadzhanov, D. N. Tashbaev, G. Otkrytiya , Izobret ., Prom. Obraztsy, Tovarne Znakl 1979, (42). 97; Chem. Abstr. 1980, 9 2 , 69037j. (610) Zal’tsberg, V. Kh.; Bogoslavskaya, 0. N. Org. Reagenty Anal. Khirn 1980, 3 , 54-62; Chem. Abstr. 1981, 94, 113947~. (611) Zenkl, M.; Iwaki, K. Bunseki Kagaku 1979, 28, 710-712; Chern. Abstr. 1980. 9 2 , 51355b. (612) Zhang, 2-X. TzuJan Tsa Chlh 1980, 3 , 540-541; Chem. Abstr. W81, 9 4 , 92667q. (813) Zhivopistsev, V. P.; Bondareva, E. G.; Potemkina, S. R.; Osokina, G. P. Org. Reagenfry Anal. Khim. 1980, 3 , 47-49; Chem. Abstr. 1984, 9 4 ,
(597) Yamamoto, Y.; Shibahara, K.; Takei, S. Bull. Chem. SOC.Jpn. 1080, 5 3 , 809-810; Chem. Absfr. 1980, 9 2 , 225818~. (598) Yamashlta, T.; Nakamura, H.; Takagi, M.; Ueno, K. Bull. Chem. SOC. Jpn. 1980, 53, 1550-1554; Chem. Absfr. 1980, 9 3 , 9 6 7 7 1 ~ . (599) Yan, F-X., Li, X-M. Huan Chlng K ’ o Hsueh 1080, 7 , 24-28; Chem. Absfr. 1980, 9 3 , 19176Oa. (600) Yang, C. Y.; Shih, J. S.; Yeh, Y. C. Analyst (London) W81, 706 (1261), 385-388. (601) Yoshimura, K.; Toshimttsu, Y.; Ohashi, S. Taknta 1980, 2 9 , 693-697. (602) Yotsuyanagi, T. Bunseki 1979, (e), 592-597; Chem. Absfr. 1980, 9 2 , 14700q. (603) Yotsuyanagi, T. Kagaku (Kyofo) 1980, 3 5 , 233-236; Chem. Absfr. 1981, 9 4 , 131494~. (604) Yotsuyanagi, T.; Matsunaga, H. Dojin Nyusu 1980, 76, 1-16; Chem. Abstr. 1881, 9 4 , 113712t. (605) Young, E. F. Opt. Spectra 1980, 78, 44-48. (608) Yuki, H.; Yajlma, T.; Kawasaki, H. Chem. Pharm. Bull. 1980, 28, 3375-3380. (607) Yunan University Fen Hsl Hue Hsueh 1978, 8 , 281-283; Chem. Absfr. 1980, 9 2 , 993512. (608) Yusupov, M. Yu.; Israllov, M. A.; Pachadzhanov, D. N.; Panova, E. V. Zavod. Lab. 1080, 46, 390-392; Chem. Abstr. 1980, 9 3 , 160576r.
131582e. . .. .. - -.
(614) Zijlstra, W. G.;Van Kampen, E. J. J . Clln. Chem. Clln. Blochem. 1981, 79, 521-523. (815) Zorawski, A.; Woiinski, J. Przem. Spozyw. 1980, 3 4 , 301-302; Chem. Absfr. 1981. 9 4 . 82342r. (618) Zuchi, G. Fariacla (Bucharest) 1980, 28, 21-30; Chem. Absfr. 1080, 9 3 , 163791t. (617) Zwart, A.; Buursma, A.; Van Kampen, E. J.; Oeseburg, B.; Van der Ploeg, P. H. W.; Zijlstra, W. G. J . Clin. Chern. Clln. Blochem. 1981, 79, 457-463. (618) Zwicker, H. R. Top. Appl. Phys. 1980, 79 (2nd ed.), 149-196.
Emission Spectrometry Walter J. Boyko, Peter N. Kellher,” and Joseph M. Patterson 111 Chemistry Department, Villanova University, Villanova, Pennsylvania 19085
This is the 18th article in the series of biennial reviews in the field of emission spectrometry/spectroscopy and is the second written by the Villanova author group. This year Joseph M. Patterson I11joins us as coauthor replacing James M. Malloy who assisted with the 1980 review (14A). This review article will survey selectively the emission spectrochemical literature of 1980 and 1981. By agreement, however, flame emission publications are reviewed in the section of this review issue entitled “Atomic Absorption, Atomic Fluorescence, and Flame Spectrometry” authored by Gary Horlick. This follows previous custom (5A,I4A, 55A). Because of the late arrival of some journals appearing in December 1981, 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 that we had previously used (14A),this is essentially the format that had been used by the previous author of this review, R. M. Barnes (5A). Because of space constraints in this review issue, however, Analytical Chemistry has asked us to be particularly selective 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 spectroscopists; articles of primary interest to astronomers and/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 (3A). In addition, the latest Application Reviews issue of Analytical Chemistry (2A) contains many recent spectrochemical application references. Readers should also note the excellent annual series Annual Reports on Analytical Atomic Spectroscopy (24A,86A) published by the Royal Society of Chemistry, Burlington House, London, W1V OBN, United Kingdom. These annual reports provide detailed information on emission spectrometry and are absolutely hi hly recommended to those with an interest in the field. &ereas our biennial selective reviews provide several hundred references, each of these annual reviews provides over 2000 references including a wealth of information on meeting 188 R
0003-2700/82/0354-188R$06.00/0
presentations. Volume 10, reviewing 1980,has just appeared (86A)and the Editor, Barry L. Sharp, is commended for his outstanding effort. In going through the 1980-1981 literature, we have selected the following publications 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, Atomic Spectroscopy, 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 Analytical Chemistry, Journal of Chemical Education, Journal of the Optical Society of America, Journal of Quantitative Spectroscopy and Radiative Transfer, Microchemical Journal, Optica Acta, Progress i n 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/International Laboratory, Industrial Research and Development, Laboratory Practice, etc. are not generally cited. However, where we feel that a publication is of fundamental importance, it is cited whatever the source. Readers should note that Atomic Spectroscopy is the new name for the old Atomic Absorption Newsletter, the new name reflects the trend toward optical emission (read “plasma emission”)as we move into the 80s.
BOOKS AND REVIEWS 1980 saw the publication of a most important work, “Line Coincidence Tables for Inductively Coupled Plasma Atomic Emission Spectrometry”, a two-volume set compiled by P. W. J. M. Boumans (IIA). This publication consists of coincidence tables for inductively coupled plasma (ICP) atomic emission spectrometry for which appropriate (semi) quantitative data on line interferences are still lacking. Sixty-seven chemical elements and 896 “prominent” (most sensitive) spectral lines are covered. A separate coincidence table is provided for each prominent line which lists the potentially interfering lines of other elements within a spectral ran e of 0.25 nm from the peak of the prominent line. These tatles should enable ICP users to predict whether or not the choice of particular analysis 0
1982 American Chemical Society
EMISSION SPECTROMETRY
troscopic references to polyatomic molecules and Fukuda (39A)has discussed various atomic processes that can occur in plasmas. Lim’s (70A) latest volume on excited states is recommended reading as is Levi’s (69A)guide to optical design. The monumental “Encyclopaedia of Physics” (66A)has recently appeared and Volume 17 of “Treatise on Analytical Chemistry, Part 11” (65A) has also been published. This volume is particularly useful as it provides the total index for Volumes 1 through 16 and there is much useful emission spectrochemical information in all of these volumes. Goffer’s (44A) hook on archeological chemistry and Bratter and in medicine Schramel‘s (15A) . ~edited ~ hook ~on trace ~ elements , and hiology will t x of interest. Tne Rratter and &amel book (ISAJ is the edited proceedings of the first International Wurkshop held on the subjwt of Neuherberg (Went Germany) in 1980 and includes many emission spectrochemicalpapers. Hameka’s (51A)recent book on quantum mechanics provides fundamental information. Several recent analytical textbooks (ZZA, 37A, 82A, 88A) have useful sections on emission spectrometry and Malmstadt, Enke, and Crouch (73A) have written a useful hook on electronics and instrumentation. Lasers continue to play an important role in spectroscopy and several important books and reviews have been published in the last 2 years. Moore (77A) has edited “Chemical and Biochemical Applications of Lasers” and Wright and Wirth (105A) have an excellent Analytical Chemistry ‘A” page review entitled ”Lasers and Spectroscopy”. Hieftje et al. (54A) have edited “Lasers in Chemical Analysis” with specific chapters on pulsed laser systems, the optogalvanic effect, nonlinear optics, thermal lensing spectroscopy, laser excited AFS, and tunable laser system. htokhov ( @ A )has reviewed p r o g ~ e in s laser applications in atomic, molecular, and nuclear physics and Guimaraes et al. (49A)have edited a book on laser applications. Grasyuk (45A)has reviewed high-power tunahle and optical pumped molecular lasers for spectroscopy and Key and Hutcheon (63A) have an in-depth review of the spectroscopy of laser produced plasmas. Fruengel(38A) discusses sparks and laser pulses and Letokhov (67A)comments on the laser selective detection of single atoms. He discusses the fundamental principles, recent experimental results, and possible applications. On the sub’ect of single atom detection, Alkemade (ZA) has recently pubished ao excellent review article based upon his plenary lecture given at the 6th FACSS meeting in Philadelphia in 1979. He concludes that single atom detection is not expected to bring about a breakthrough in normal routine analysis but it remains a thrilling challenge to become ultimately capable of detecting one single atom in a whole sample. The 61st edition of the “CRC Handbook of Chemistry and Physics” has been published (IOIA) providing much useful spectral data and Volume I11 of the ‘CRC Handbook of Spectroscopy” (84A) has also appeared. This volume gives much useful information including wavelength standards in the visible, ultraviolet, and near-infrared regions. Wavelength dependent and electronic system oscillator strengths for free diatomic molecules are also given. Sobelman et al. ( W A )have edited a hook on the excitation of atoms and broadening of spectral lines and Malmstadt (74A)has written an interesting speculative review entitled “Analvtical Instrumentation for the 1980s”. The International Atomic Energy Agency has published (32A)an interesting report on the elemental analysis of biological materials with special reference to tram elements. The report consists of 15 chapters in four sections, (a) on the need for trace element analyses in the life sciences, (b) sampling and sample preparation, (c) analytical techniques for trace and minor elements in biological materials, and (d) analytical quality control. VanLoon’s recent atomic absorption book ( M A ) contains useful information as does Young’s (106A)book on separation procedures. Chemometrics is certainly a growth area in analytical chemistry and Malinowski and Howery (72A) have written a useful book on the subject. This will certainly be of interest to atomic spectroscopists. Ballhausen and Gray (4A) have a new text on molecular electronic structures and Ewing (35A) has recently published “Topics in Chemical Instrumentation”, a selection of important articles from the J. Chem. Educ. column. Two recent texts on rock and mineral analysis (57A, 58A) contain useful information on emission spectrochemical procedures. ~~~~~~~~~~
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.(center) !s Rotgua of Anatylkal Chemlsby at Villanova Unlusralty. Ha -ked hla AB. (1962)horn SI. Michael’s College and M.Sc. (1967) and R.D. (1969) d e p e s from the Unluersw of London. Dr. Ksilha also M r the Diploma 01 Membsrshlp (D.1.C.) 01 lmwlal CoC legs. Dr. Kelim has p u M W approximately 45 papas in varbus areas of analyllcal chemfsby and is presenlly Treasurer 01 Ik DMslan of Analytical Chamisv. ACS h. Ksilhn is also FACSS (FSderaaOn 01 Analytical Cham lsby and Spacbmcopy Societies) Exhibil Direnot. Ha Is on Ik Board 01 Dkectws. Philadeiphla Saclion. ACS. and an Ahernate. wann J. Boyko (ien) is a graduate student in me Chemlav Dspanmam at Villanova Unkerslty. He recekd hls B.A. degree (l970)horn La Salk Coc &.Rliladeiphia Atter owera1 years of industrial and teaching BxpBrience. he began graduate studies at VlllanOva in the BUtUmn 01 1978. Mr. BO#O la presently finishing hls m.D. degree requirements: his research has centered on sample inbcdunbn lot Ik DCP. ~ o u p hM. Pane111 (right) IS also a waduate 8Mont in the Villanova Unkerslty Chemlsby DepRment. Ha receluad hk B.S. (1978)horn Vil$nova and aner two years In lndusby began his Ph.D. studies at Villanova. He is presently doing research invoMng Inladacing chramatographlc sygtema with varbus optical detectors (plasma. llu~escence.etc.) In wder to inaease S B l e C t M t y and SensMVy p.hr N. K.l*r
lines is a r a t i d proposal for any specified analytical problem when new sample types have to be analyzed. An accompanying computer wfhvare package for the two volumes became available from the publishers in late 1981. In an interesting review article, Boumans (12A) describes his approach to converting the Tables of Spectral-Line Intensities for the copper arc into tahlea appropriate to the ICP. The philosophy behind the approach is discussed in another article (13A). Another useful compilation book is ”An Atlas of Spectral Interferences in ICP Spectroscopy” by Parsons and Forster (79A). This book shows all experimentallyused analysis lines and a list of all currently known transitions between 1850 and Zoo0 A. However, the most important part of the book is the listing of all transitions within about 1 A and 5 A of each important analytical line. Wende has edited an important book, “Spectral Line Shapes” (103A). the Proceedings of the Fifth International Conference on the subject held in Berlin in 1980. There is a wealth of fundamental information in this 12M) page publication including a useful &ion on line broadening by foreign gases. Veprek and Venugolapan (%A) have edited a book with three useful sections: elementary plasma reactions of environmental interest, plasma and material interactions, and preparation of optical waveguides with the aid of plasma activated chemical vapor deposition at low pressures. The English version (89A)of Slickers’ previous German work has appeared. This book addresses those who wish to apply spectrochemical analysis to the solving of routine analytical tasks. Consequently many practical suggestions are given for the correct use of spectrometers and for the application of spectrochemical procedures. Two related books are “Low Temperature Plasma Technology Applications” (78A)and “High Temperature Plasma Technology Applications” (34A). The second book discusses various organic reactions that can occur in a plasma jet and s ~ i z e other s reactions that can occul in high-temperature plasmas. Verma (99A) has written a useful hook on spec-
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Three special issues of Spectrochimica Acta, Part B should be noted here. Two of these are entitled ”Atomic Absorption SpectroscopyPast, Present, and Future” (91A,92A) and were put together to commemorate the 25th anniversary of Alan Walsh’s landmark paper in the journal. There are many worthwhile pa ers (both atomic absorption and emission) in these issues. Inother special issue is “Atomic Spectroscopy in Japan” (93A),this appeared just before the recent CSI/ ICAC meeting in Tokyo and was put together by guest editors, K. Fuwa and H. Haraguchi. There are many excellent articles in this issue including an article by Fuwa and Kamada (43A) giving a brief historical account of spectrochemical analysis in Japan. Chakrabarti (21A)has edited “Progress in Analytical Atomic Spectroscopy, Volume 2”, this is a bound volume representing Volume 2 of the journal. (It is, however, sold separately from the journal.) Several excellent reviews in Progress in Analytical Atomic Spectroscopy have appeared during the past 2 years. Mills and Belcher (75A)have reviewed analytical techniques for the analysis of coal, coke, ash, and mineral matter while Delves (28A) has reviewed various methods for the analysis of biological and clinical materials. Dittrich (29A) has commented on analytical applications of diatomic molecules and Baudin (7A) has reviewed analytical methods for nuclear energy materials. Falk (36A) has described a theoretical approach to atomic spectrometry using tunable lasers and Doolan and Belcher (30A) have reviewed analytical methods for nonferrous alloys. The definitive review on discrete sample nebulization in atomic spectrometry has been written by Cresser (23A)and is highly recommended reading. Brill (16A) has reviewed analytical methods for the determination of lithium in aluminum and Betteridge and Goad (IOA)have discussed the impact of microprocessors on analytical instrumentation. Toxic metals have been considered by Berman (9A)and Brooks et al. (17A)have compared atomic absorption and emission spectrochemical methods for the quantitative measurement of arsenic. Petak and Hirbal(8OA) compared analytical methods for ore processing products, Versieck and Cornelis (100A) discuss normal levels of trace elements in human blood plasma and serum, and Carnahan et al. (20A) have reviewed element selective detectors for chromatography with an emphasis on plasma methods. Stockwell (94A) has discussed the changing face of laboratory automation and comments on present and future trends. The ICP has been reviewed by many workers including Barnes (6A),Burman and Bostroem (19A),DeGalan (25A), Enger et al. (33A), Furuta and Fuwa (40A), Fuwa (42A), Greenfield (46A-48A), Haas and Fassel(5OA),Haraguchi and Fuwa (52A),Huang et al. (56A),Karnowski and Berg (59A), Kasahara et al. (60A),Kawaguchi (61A, 62A), Kirkbright et al. (64A),Robin (83A),Schleicher et al. (85A),Simon (87A), Sugimae (95A),Van Montfort and Agterdenbos (97A),Welz (102A),and Zhu et al. (108A). Greenfield (47A)has published an interesting article describing the relationship between flow injection analysis (FIA) and the ICP; he calls it a “wedding”. Furuta (41A) has written an 84 page in-depth report on multielement analysis via flame and ICP techniques and Helmer (53A) has described a theory of measurement with applications to spectroscopy. Pillow (81A) has written a critical review of spectral and related physical properties of the hollow cathode discharge and Buehring and Buban (18A) have considered the direct current plasma (DCP) as an alternative to AAS and or ICP spectrometry. Zander and Hieftje (107A) have written a detailed review on microwave supported dischar es. Conditions under which a microwave induced plasma VMIP) can be operated are delineated, and instrumentation necessary for MIP spectroscopy is considered. There is much discussion on methods for sample introduction for MIPS, certainly the most difficult step. This review is highly recommended. Beenakker et al. (8A) have also considered the MIP as an excitation source for emission spectrometry and Locke has reviewed (71A) the applications of plasma source atomic emission in forensic science. W. G. Fateley, the Editor of Applied Spectroscopy, is to be congratulated for beginning a series entitled “History of Spectroscopy”. The fiist two articles in this series have already appeared. Mitteldorf‘s article (76A) entitled “View from Behind the Counter” is a very amusing paper describing the development of Spex Industries and Eklund (31A)has written WOR
ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
“Bausch & Lomb-ARL: Where We Come From, Who We Are” describing his firms “roots”. We look forward to more in this series. Delaey and Arkens (26A, 27A) have published a list of hundreds of common (and some not so common) acronyms used in the world of spectroscopy, microscopy, and diffractometry. Some of these can only be described as “cute”, e.g., ASLEEPOPER, Automated Scanning Low Energy Electron Probe with On-line Processing of Experimental Recordings. Lastly, and not belonging in any simple category, Woodriff and Graden (104A) have described a conceptual approach to the dilemma of particles and waves of light and matter in something or nothing. This approach assumes a new kind of ether made up of very small anisotropic particles called “zwitters”. It is further assumed that the presence of particles of charge, mass, or moving charge cause an orientation distortion of the particles of the medium which respectively constitute electric fields, gravity, and magnetic fields.
SPECTRAL DESCRIPTIONS AND CLASSIFICATIONS Zalubas and Albright (98B) presented a bibliography on atomic energy levels and spectra for July 1975 through June 1979 with over 1200 references. Reader and Corliss (82B) reviewed wavelengths of 47 000 spectral lines while Wiese and Martin (93B)reviewed transition probabilities of 5000 spectral lines for the two part “Wavelengths and Transition Probabilities for Atoms and Atomic Ions”. Ener y levels were critically compiled by Martin and Zalubas ?67B, 68B) for magnesium (I-XII) and sodium (I-XI) and by Corliss and Sugar (24B, 88B) for nickel (I-XXVIII) and scandium (IXXI). The measurement and classification of spectra were presented by Svendenius (89B)for phosphorus, Spector and Held (86B) for erbium, and Johansson and Litzen (52B)for singly ionized scandium. Huldt (47B)measured and classified lines for titanium(I1) and accurately determined lifetimes for some low excited levels in zinc(I1) and silicon(1-IV). Fuhr et al. (35B) evaluated and compiled 5100 lines for all stages of ionization in iron, cobalt, and nickel including line strengths, spectroscopic designations, and statistical weights. Palmer, Keller, and Engleman (74B) compiled an atlas of wavelengths and intensities of uranium(1,II)lines while Palmer et al. (75B)accurately measured some uranium and thorium lines to be used as benchmarks for the lines in the atlas (74B). Due to the richness of the uranium spectrum, this atlas should be useful for the calibration of lasers, spectrographs, and monochromators with a uranium HCL or EDL. Rajnak (81B) assigned nearly all levels for uranium(1) and many for uranium(I1). Hutcheon (49B)calculated ionization potentials for the neon isoelectronicsequence while oscillator strengths have been calculated for isoelectronic sequences by Ganas (36B-39B) for oxygen, nitrogen, chlorine, and silicon and by Lindgaard et al. (65B) for copper. Table I presents selective references to atomic spectra including lifetimes, oscillator strengths, transition probabilities, and hyperfine splittings. As in our previous review (14A), values for molecular and highly ionized species are excluded. Mori (70B)reviewed the classificationof spectral lines while Huber and Sandeman (45B)reviewed the classical methods of measuring transition probabilities. Kelly and Mathur (56B) examined the Hanle effect in singlet excited states of alkaline earth elements while Bachor and Kock (6B) discussed limitations in the evaluation of hook spectra. Wynne and Beigang (96B) applied the new method of using phase-matched nonlinear optics to the accurate measurement of relative oscillator strengths of neutral calcium. Pegg and Gaillard (77B) reviewed the use of fast ion beam-laser spectroscopy (FIBLAS) for the measurement of ion lifetimes. Davidovich and Nussenzveig (27B) published a new treatment on the theory of natural line shapes. Mizuta (69B) has reviewed the theoretical problems of spectral line shapes while Ben-Reuven (12B) has discussed recent developments in line shape theory at the important conference on spectral line shapes (103A). Batal and Mermet (8B)have calculated some line profiles (assuming a van der Waals potential) for ICP-AES and Vetter and Berman (92B) and Burgess ( 1 7B) have reviewed the determination of line shapes using lasers. Collisional line broadening has been reviewed by Lewis (62B) and by Peach (76B)while Claude and Valentin (23B)prepared
EM I SS I ON SPECTROMETRY
Table I. Selected References to Atomic Spectra Wavelengths (A),Energy Levels ( E ) ,Ionization Energies (I).Lifetimes (7).Oscillator Strengths (f), Hyperfine spiittings (hfsj, isotope Shifts (isO), and Transition Probabilities ( A ) ref element ionization level type Li 0
ZO,Z1,22Ne Na Mg
Si P Ar sc Ti V Cr
I1 I I I-XI I-XI1 I, I1 I-IV I I I I1 I-XXI I1 I I1 I1 I, I1 I1
Fe
co
I I1
Ni
I-XXWI
I Zn
I
I1 I I I I1 Y I Zr I, I1 Mo I Pd I I, I1 Ag I Cd I1 In I I1 Sn 1291 I Xe I I1 I cs I I1 Ba I1 Nd I I I1 Gd I I, I1 DY I 16’3’63D~ I Er I I Yb I I Lu I Au I I1 Hg Bi I, I1 Fr I U I, I1 I, I1 234,238 U I Ga Kr Rb
7 7
hfs, is0 E E 7
7
E, T
A A E, I
f”’ I, E,
f
A
f
E, f,A,
f
7
E, f,A, E , f ,A, E, I
f, 7 f, 7 7
hfs, is0 A , is0 7
7
f 7 7 7 7
A, 7 7
hfs, is0 7
hf s A, 7
hfs, is0 7
hfs hfs, 7 hfs, is0 7
is0 is0 7
f, 7 is0
hfs E 7 7
is0 7 7 7
A
hfs, is0 h
E
is0
60B 28B 54B 68B 67B 64B 7B, 47B 89B 14B 55B 84B 88B 52B 25B 47B 41B 95B 40B 3 5B 13B 53B 35B 35B 21B 10B, 46B 58B 47B, 48B 51B, 71B 33B, 50B 43B 20B 19B 44B 29B 16B 78B 21B, 57B 91B 51B, 71B 26B 22B 18B,83B 15B 73B 34B 5B, 11B 85B 66B 3B 4B 66B 42B 97B 30B 86B 51B 9B 2B 61B 79B 32B 87B 63B 74B, 75B 81B 31B
tables for the determination of spectral line parameters from spectroscopic dtita for pure Lorentz broadening. Voight profiles of spectral lines were discussed by Wilczek et al. (94B) and by Klim (598) while No11 and Pires (72B) presented a new nonlinear leasbsquares algorithm for Voight spectral lies.
Twitty et al. (9OB)compared fast codes for the evaluation of the Voight profile function. Pratt (80B) has reviewed the theory of the electron bremsstrahlung spectrum. Adams and Whaling ( I B ) have determined the branching ratios for 104 lines of argon(1,II). These can be used to calibrate the relative detection efficiency of a spectrometer over the range of 290-2300 nm.
INSTRUMENTATION Sample Introduction. There has been a lot of activity in this area during the past 2 years and therefore it seems appropriate to begin ithe Instrumentation section of this review with a discussion of this topic. T. Uchida et al. (95C) at the Nagoya Institute of Technology have used a discrete nebulization technique for the determination of metals in small samples while H. Uchida et al. (94C) at the University of Tokyo have described a microsampling technique for simultaneous multielement analysis by ICP spectrometry requiring samples of less than 60 nL. Shabushnig and Hieftje (SIC)have designed a device capable of delivering a controlled volume of uniform droplets whereby samples as small as 40 nL can be delivered with 1.5% precision. Broekaert et al. (13C)have investigated an ICP injection technique for the analysis of small volume samples. Aziz et al. (3C) injected 50-200 p L of diluted serum samples into a high-power ICP via a small funnel coupled to a Meinhard nebulizer. Cresser and Browner (I!?C)have developed a method for investigating size distributions of aqueous droplets in the range 0.5-10 pm produced by pneumatic nebulizers. In a related paper (18C), these investigators determined that increasing temperature changes affect the viscosity of the sample causing substantial change in nebulizer rate resulting in a decrease of nebulizer efficiency at higher tem erature due to smaller droplet size. Novak and Browner (648) have measured droplet size distributions as a function of nebulizer operating conditions and have used ( 6 3 3 a cascade impactor operator in series with an electrical aerosol analyzer to characterize droplet sizes of low volatility liquid sprays producod by pneumatic nebulizers. Chang and Penner (16C) and Bleiweiss, Chang, and Penner (1OC) have used light scatterin to measure particle size in flames and Chlang and Penner &5C) have described a procedure for the simultaneous determination of mean particle radii and mean vallues of fluctuating velocity components in turbulent flows using scattered laser-power spectra. Mohamed and Fry (59C) found that a nonlinear overestimate of median droplet diameter of aerosol path traversed by the laser exceeds the optical delpth of the field chLaracteristic of the diffractometer. Belchamber and Horlick (6C)have made pressure measurements in the nebulizer spray chamber of an ICP. Ripson and DeGalan (74C) have described a sample introduction syEitem for an ICP operating on an argon carrier gas flow of 0.1 L/min. Layman1 and co-workers (49C) have utilized a four-channel variable speed peristaltic pump with a pneumatic nelbulizer and Berman et al. (8C) have developed a method involving ultrasonic nebulization of metal concentrates for the simultaneous determination of trace metals by ICP spectrometry. Taylor and Floyd (87C) have reported lower detection limits for environmental samples with ultrasonic nebulization as compared to when pneumatic nebulization is used. Mohamed, Brown, and Fry (58C) have designed a clog-free Babin ton slurry nebulizer system and Garbarino and Taylor (358)have described a Babington type nebulizer for use in the analysis of natural water samples with an ICP. ‘I’yson and Idris (92C) have described a flow injection sample introduction system for AAS that could have application in plasma emission spectrometry. Sommer and Ohls (82C) have studied direct sample introduction into a stable running ICP. Uchida et al. (93C) have applied an automatically triggered digital integrator to the determination of copper using a discrete nebulization technique. Bauer and Natusch (5C) have developed a method for the analysis of carbonate compounds in coal fly ash by thermally evolved gas analysis of carbon dioxide in a helium MLP. Suzuki et al. (83C) have studied the excitation of barium in a molybdenum microtube atomizer and its use by emission spectrometry. Thelin (88C) has described a nebulizer system for the analysis of high-salt content solutions with an ICP. Scott and Ottaway (78C)determined mercury vapor in air using a passive gold wire sampler and Pickford (71C) has described a very clever syringe hydride technique for the determination of arsenic ANIALYTICAL CHEMISTRY, VOL. 54, NO. 5 , APRIL 1982
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with an ICP. The method was reported to be extremely simple to use. Peacock and Singh (70C) used a simple hydride generator system for arsenic determination by AAS and this could be extended to emission measurements. Patterson (69C) has described a rotary sample valve for flame spectrometry that could also be useful in emission spectrometry and Novak et al. (65C) have investigated the use of a fixed crossflow nebulizer for use with ICPs and flames. Thompson et al. (89C) have used laser ablation for the introduction of solid samples into an ICP and Ishizuka and Uwamino (40C) have examined a laser vaporization-MIP system for various elements in solid samples such as brass, steel, and aluminum. Orlikowski and Assous (67C) investigated the use of powder injection into a wall-stabilizedcascade arc. Estes, Uden, and Barnes (26C) have described a valveless fluidic logic gas switching interface between a high-resolution gas chromatograph and an MIP which vents large quantities of eluent which could discrupt the helium MIP discharge. Boorn, Cresser, and Browner ( I I C ) have studied the evaporation characteristics of organic solvent aerosols used in analytical atomic spectrometry and Alder and DaCunha ( I C ) have evaluated low-pressure argon MIP systems with carbon rod sample introduction for trace metal analysis. Russo and Hieftje (75C) compared experimentally observed aerosol droplets to a calculated velocity using a new mathematical model. They reported excellent agreement between the two methods. Gratings. Maystre, Cadilhac, and Chandezon (52C) have used a ri orous phenomenological theory to define the fundamentaf parameters of a erfectly conducting grating Schroeder and Hilliard (778) have compared theoreticai calculations and experimental measurements of echelle grating efficiencies for R2 echelles. Todorov et al. (9OC) have examined some spectral characteristics of thick phase holographic gratings and Verrill(99C) has commented on the limitations of currently used methods for evaluating the resolution of diffraction gratings. Harada and Kita (36C) have investigated mechanically ruled aberration in corrected concave gratings and Dunning and Minden (25C) have studied the scattering from high efficiency diffraction gratings. Radziemski (72C) has commented on the calculation of dispersion for a plane ating in a Czerny-Turner mount. Breidne and Maystre (12&conducted a systematic numerical study for perfect blaze in non-Littrow mounting and Hilborn (38C) has reported on increasing spectroscopic resolution with separated gratings and prisms. Moharam and Gaylord (60C) have conducted a rigorous cou led-wave analysis of planar-grating diffraction. They reportefthat ultra high resolution is possible with widely spaced gratings. Nubbemeyer and Wende (66C) have examined the optical properties of a 5-m echelle vacuum spectrometer. Shope (79C) has commented on the echelle grating spectrograph and ways that it can solve some problems commonly encountered in other instrumental analysis. Josse and Kendall (46C) have investigated a rectangular-profile diffraction grating from single-crystal silicon and Kielkopf (47C) has compared echelle and holographic gratings for scattering and spectral resolution. Optics. In a particularly interesting paper, Anderson, Forster, and Parsons (2C) have described a fully computerized scanning system for an echelle monochromator. The system has been evaluated with respect to wavelength movement, positioning, precision, resolution, and overall scanning ability. Wavelength position can be determined with a precision of one step of the stepper motor which corresponds to 0.0001 nm in favorable cases (this is dependent upon the spectral order) and transitions as close as 0.01 nm apart can be base line resolved and features much closer can be identified. In another interesting publication, Ottaway, Bezur, and Marshall (68C) have modified an echelle monochromator system for the measurement of sensitive carbon furnace atomic-emission signals. A 4 0 - H ~wavelength modulation was used with this system. Downey, Shabushnig, and Hieftje (24C) have investigated the reduction of spectral interferences in FES by selective spectral-line modulation and Michel et al. (55C) have described a new mechanical arrangement for wavelength modulation. They use a rotating quartz mechanical chopper rather than the usual oscillating refractor plate. McLaren and Berman (54C) have applied wavelength modulation ICP-echelle spectrometry to the determination of cadmium and lead 192 R
ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
in marine samples and Ito (4IC) has developed a method for element detection utilizing coherent forward scattering of resonance radiation from atoms irradiated by continuum spectral sources. Shepherd (80C) has presented a model for photodetection of single mode cavity radiation and Fujiwara (330 has examined transfer functions of spectroscopic systems using a sinusoidally modulated spectrum. Spectrochimica Acta, Part B has begun a new “Instrument Column”with an article by Broekaert (14C) surveying emission spectroscopic instrumentation. Taylor and Floyd (86C) have evaluated a multichannel ICP optical emission spectrometer modified to minimize and correct scattered light effects. Vermaak et al. (98C) investigated the feasibility of using an Ulbricht Sphere for the absolute calibration of an ICP or other source at specific wavelengths. Mikes (56C) gives a brief review on plane holographic diffraction gratings in optical systems and Mathews et al. (50C) present a system for time and space resolved photography of self-luminous electrical discharges for arcs, sparks, and plasmas. Fourcade et al. (31C) have observed variations of the relative intensities of the fine structure components of the helium 587.5-nm yellow line under different conditions of excitation. DeSerio (21C) has analyzed wavelength dispersion problems associated with some commercial scanning monochromators and Jolly and Stephens (43C) have described the isolation of the sodium 589.0-nm line by a Voight effect filter. Colegrave and Abdalla (17C) give a cononical description of the Fabry-Perot cavity and Yoshino et al. (102C) have described a photoelectric scanning spectrometer for vacuum UV cross section measurements. Walden et al. (IOOC) have described a new, inexpensive, nitrogen-pumped dye laser with sub-nanosecond pulses and Bennen, Hosch, and Piepmeier (7C) have described a method for accurate wavelength calibration of an etalon-tuned dye laser. Talmi and his research colleagues (84C) have described an interesting laser microelemental determination with an o tical multichannel detection system while Kozma et al. ( 4 5 6 have studied spectrographic measurements with a laser microdensitometer. Sainz and Coleman (76C) have reported on a method for the experimental alignment of a spectrometer system using laser diffraction. The technique uses diffraction of a helium-neon laser through the entrance slit of the monochromator. Diffraction pattern symmetry serves as a sensitive visual guide. The authors report that considerable time savings using this approach have been realized. Laporte et al. (48C)have described a complete vacuum UV spectrometer device including the source and a computerized data acquisition system for both reflectance and transmittance measurements in the 105-200 nm range. Computer Interfacing. In an important publication, Floyd, Fassel, and D’Silva (29C) have described a computer-controlled, scanning monochromator system that can be used for the determination of 50 elements in geochemical and environmental matrices. The monochromator is combined with an ICP so that elements at major, minor, and trace levels may be determined in sequence without changing experimental parameters other than the spectral line observed. A single set of spectral lines was found to be applicable to a broad range of sample compositions and to show negligible spectral interferences regardless of the sample matrix. In a related paper from the same laboratory, Fassel and co-workers (30C) developed a system for the rapid sequential determination of various elements using an ICP and a computer-controlled scanning monochromator. Barnhart, Farnsworth, and Walters (4C) have constructed an integrated, microcomputer-controlled adjustable waveform spark source for AES. Including in this report are electrical schematics, construction details, and performance examples for an electronic, adjustable-waveform spark source. McCarthy et al. (53C) have described an ICP basic programmable computer-controlled double monochromator for sequential multielement analysis and Ng and Horlick (61C) have illustrated the use of computer generated cross-correlation masks by evaluating nickel and vanadium spectra obtained with an ICP using a photodiode array spectrometer. Fisher and co-workers (28C) have described interactive procedures for correcting ICP spectral interferences while Janssens and his co-workers (42C) described experiences and some results obtained with a commercial computer-controlled scanning monochromator that performs spectral line search and line
EMISSION SPECTROMETRY
profile measurements in an ICP solely by grating slewing. Background correction by software techniques was also investigated. Optical Detectors. Yamashita (101C) has discussed the time dependence of rate dependent photomultiplier gain and its implications. Blades and Horlick (9C) have presented a photodiode array measwement system for implementing Abel inversions on emission from an ICP. A complete map of analyte emission throughout the plasma was acquired via the measurement of a series of horizontal emission profiles. Such horizontal emission proffiles profile only lateral intensity information but these lateral intensities are converted to radial intensities by Abel inversion. Furuta et al. (34C) have evaluated a silicon-intensified target image detector for ICP spectrometry and Matveev et al. ( 5 1 0 investigated intracavity spectra with a photon detector based upon stepwise atom photoionization. VanWoerkom et al. (97C) described the design and construction of a microreactor for generating infrared emission spectra from a heterogeneous catalyst system. An IR transmitting window detector wag also described. Chromatographic Detector Systems. As noted by Carnahan, Mulligan, andl Caruso in their recent review article (20A), there hari been an increased interest in coupling chromatographic systems with optical atomic detectors such as AAS and plasma emission in order to obtain selectivity and sensitivity. Treybig and Ellebracht (91C) have used a DCP as a sulfur-specificgas chromatographic detector. The detector was reported to be 1inea.r over at least 3 orders of magnitude g was achieved. It should and a detection limit of 3 X be noted, however, that lines in the vacuum UV (180.7,182.0, and 182.6 nm) were used and it was necessary to purge the monochromator. Estes, Uden, and Barnes ( 2 7 0 interfaced fused silica gas chromatographic columns to a helium MIP. A TMlo (Beenalrker type) resonant cavity allowed axial viewing of plasma emiesion and a quartz refractor plate background corrector wm reported to improve selectivity ratios for elements whlose emission occurs in the high-carbon (cyanogen) background region. Hausler and Taylor (37C) developed a simultaneous on-line ICP detector for metal species separated by effective molecular size. A new spray chamber to facilitate thiii analysis in relatively high volatility organic solvents and to serve as the interface between the LC-(ICP/AES) interface was evaluated. Rice et al. (73C:) have described an atmospheric pressure nitrogen afterglow as a detector for gas chromatography and Din jan and DeJong (22C) have presented a comparative stufy of two cavities for generating a MIP in helium or argon as a gas chromatographic detector. Tanabe, Haraguchi, and Fuwa (85C) have examined an atmospheric pressure helium MIP aa an element-selectivedetector for gas chromatography. Detection limits, dynamic ranges, and selectivities were obtained for hydrogen, carbon, fluorine, chlorine, bromine, iodine, and sulfur. Fraley and co-workers (32C) have studied ICP-AES as a multiple element detector for metal chelates separated by HPLC. Optical Emission/iMass Spectrometry. A few publications on optical eniissionJmassspectrometry indicate that this interface may be very important in the future. In a significant paper, Fassel and co-workers (39C) have injected solution aerosols into an ICP to generate a relatively high number density of positive ions. A small fraction of these ions is extracted through a sampling orifice into a differentially pumped vacuum system housing an ion lens and quadrupole mass spectrometer. This approach offers a direct means of performing trace elemental and isotopic determinations on solutions by mass spectrometry. In a related paper, Date and Gray (20C) have described the performance of an instrument using an ICP as an1 ion source with a high resolution mass filter to analyze the extracted ions. The cument performance of the technique for simple solution analysis is described and the future potential for trace element analysis and isotope ratio measurement is assessed. Douglas and French (23C) have coupled an MIP source to a quadropole mass spectrometer. The atmospheric pressure plasma was reported to have an excitation temperature of 5400-5900 K and an electron density Elemental . ions are extracted from the plasma of 1014~ m - ~ through a differentially pumped interface designed by using gas dynamic molecular beam techniques. Miscellaneous. Ure and co-workers (96C) have constructed a three-channel flame AA/ES system which could
be extended to be used with a plasma emission system. Nord and Karlberg (62C) have described an automated excitation system for flame AAS which could also be applied to AES. Miyaishi et al. (67C) have studied laser fluorescence systems for ultratrace analysis while Kawaguchi et al. (44C) have examined a water-cooled torch for ICP spectrometry. Axial emission profiles from the plasma were measured by using a photodiode array spectrometric system.
SlTANDARDS, SAMPLES, NOMENCLATURE, CALIBRATION, CALCULATIONS Alkemade, Winefcirdner, and co-workers have continued their series “A Review and Tutorial Discussion of Noise and Signal-to-noise Ratiori in Analytical Spectroscopy”. The third paper in the series is on the subject of multiplicative noises (11))and is certainly recommended reading. The sources of noise, the mathematical representation of noise, and the major types of noises in emission and luminescence spectrometry are discussed. Heltai and Zimmer (80) have discussed the influence of photographic and photometric factors on the shape of the blackening curve and Ng and Horlick (180)have commented on practical aspects of Fourier transform and correlation based processing of spectrochemical data. Maddams (150) discusses the scope and limitations of curve fitting while Kawaguchi et al. (100) have developed a method of data processing for improved precision of intensity measurements in 1CP OES with a programmable monochromator. Prudnikov (220) has developed a simple formula for the calculation of limits of detection which takes into account the blank sample values. An expression is proposed for the standard deviation due to apparatus parameters, blank values, and concentration of an element. In a related publication, Prudnikov (210) discusses the dependence of the standard deviation in atomic emission spectral analysis on element concentration. Koirtyohann, Jones, and Yates (110)have proposed a nomenclature system for the ICP, their suggested system seems eminently reasonable to the authors of this review. Tanabe, Haraguchi, and Fuwa (250) have published a wavelength table for emission lines of nonmetallic elements with transition assignments and relative intensities observed in an atmospheric pressure helium MIP. Bankston, in a particularly interesting paper, has discussed (30)data processing from the commercially available DCP-echelle emission Spectrometer and Liteanu and Rica (140) have published an interesting book on the statistical theory of trace analysis. Bader has developed (20) a systematic approach to standard addition methods in instrumental analysis and Karp (90) has developed a method for computing the electron density of a partially ionized plasma, Young has commented (310) on cylindrically symmetric radiation sources and Ziegler (320) has discussed the properties of digital smoothing polynomial (DISPO) filters. Several Analytical Chemistry “A” page reports are of interest. Woodard et al. (300) have reported on microprocessor -based laboratory data acquisition systems and Taylor (260) has commented on the quality assurance of chemical measurements. Leyden and Wegscheider (130)have reviewed preconcentration methods for trace element determinations in rtqueous samples end Kratochvil and Taylor (120) have a general discussion off sampling for chemical analysis. Burns ( 5 0 ) has reviewed automatic sample preparation. VanDalen and DeCtalan’s paper (280) on the formulation of analytical procedures involving flame AAS has application to the optimum adjustment of instruments for emission spelctrometryand Smjt (240) has reviewed the principles and problems of computer-based instruments and networks in analytical chemistry. Systematic errors are considered by Tschopel et al. (270) and VanGrieken et al. (290) warn that sample contamination can occur from a commercial grinding unit. Oehme and Lund (190) have compared various methods of preparing high-quality water in terms of the cadmium, lead, and copper content of the water. The best system of those tested was reported to be the Millipore Milli-Q system but it was also strongly recommended that it be fed with distilled (not dimineralized) water. Losses of metals in solution is the subject of several reports. Majer and Khalil (160) have commented on adhesion of calcium and magnesium on surfaces and Massee et al. (170) have discussed losses of silver, arsenic, cadmium, selenium, and zinc by sorption of various container surfaces. Adhesion ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
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of trace metals is also the subject of a paper by Gardner and Hunt ( 7 0 ) and Salmele et al. (230) have discussed the effect of washing procedures on trace element content of human hair. Braun et al. ( 4 0 ) have discussed preconcentration of phenylmercury, methylmercury, and inorganic mercury from natural waters and Cheam and Agemian ( 6 0 )have commented on the presence of inorganic arsenic species at microgram levels in water samples. Finally, Opekar and Trojanek (200) have discussed signal sampling with liquid pulses in systems with peristaltic pumps.
EXCITATION SOURCES Arc Discharges. A number of interesting papers have appeared during the past 2 years. Radic-Perk and Peric (178E) have studied an arc plasma in air with calcium and fluorine and measured the equilibrium composition of the gaseous system containing nitrogen, oxygen, carbon, fluorine, and calcium between 298 and 7000 K. In a related publication, Radic-Peric et al. (179E) studied the radial distributions of temperature, Ca, and Ca+ spectral line intensities, and CaO and CaF band intensities in a dc arc. The results, when combined with the calculations of the plasma composition (178E),make it possible to determine the radial distribution of the total calcium in the plasma with and without fluorine. The addition of fluorine causes a higher gradient in the radial density distribution of calcium in the plasma. Tripkovic and Vukanovic (209E)have studied the effect of iodine in the arc and, in a related paper, Tripkovic et al. (208E) have developed a new spectrometric method for the determination of trace elements in petroleum by a double plasma arc source in a graphite tube. Belcher and Georgieva (21E,22E) have studied a dc discharge in an alternating magnetic field and Pavlovic and Mihailidi (177E) have examined the influence of an external rotating field on the electric arc plasma. They were able to draw some interesting conclusions on the influence of the particle concentration axial distribution on the spectral line intensity distribution for several elements. Dittrich, Sulewa, and Niebergall (68E) have studied the influence of an easily ionizable constituent (NaC1) on the intensities of atomic lines in a dc arc plasma and, in a related paper, Oreschokow, Petrkiew, and Dittrich (172E) studied the axial distribution of the emission and the particle densities of chemical elements in a pulsed, unipolar arc. The following parameters were varied: polarity and position of the electrodes, electrode ga , ionization potential by using different elements, and the aEsence or presence of the easily ionizable element, lithium (as the carbonate). Watanabe and Yamane (2253)have studied multichannel discharges in a low pressure inert gas-mercury discharge caused by anode oscillation and Decker (64E) has commented on the relationship between electrode pressure and temperature in a dc arc. Walsh et al. (2223) have studied voltage-current curves for pulsed arc discharges, Shindo and Imam (194E) have studied a wallconfined argon arc plasma, Christopoulos and Endean (58E) have studied “prebreakdown“ of nearly saturated cesium vapor, and Oreshkov and Petrakiev (171E) have examined the distribution of magnesium atomic and ionic lines in a unipolar arc discharge. Kantor, Hanak-Juhai, and Pungor (122E) have studied halogenation with CC14 and CF2C12vapors in arc emission spectrometry and Marinkovic and Antonijevic (142E) have evaluated a “U”shaped dc arc for the spectrometric analysis of solutions. Kabiel and his research associates (118E)have published an interesting paper on the use of line widths in quantitative spectrographic analysis and Bogomolov et al. (34E) have studied vacuum UV spectra of a high-pressure arc discharge. Eid et al. (82E)have commented on criteria for selecting lines for temperature measurements in a dc carbon arc and Venkatasubramanian (214E)has developed a new carrier method for direct spectrographic determination of trace alkalies and alkaline earths in high-purity thorium oxide. Schoenfeld (191E)has developed a direct spectrochemical method for chromium in ruby crystals and Kamat et al. (121E) have studied trace impurities in phosphor grade CaW04 using a dc arc spectrographic method. Sastry and co-workers (184E) have determined several trace elements in V308and Bangia et al. (12E) have studied trace metals in pure graphite using arc methods. Finally, Van den Hoek and Visser (21E) have studied thermal relaxation in high-pressure mercury and sodium arc discharges and Balmain (11E)has commented on l94R
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surface discharge effects in arc discharges. Direct Current Plasmas (DCP). In a significant publication, Decker (63E) has performed an in-depth investigation of a commercially available three-electrode DCP; this plasma operates in an inverted “Y” configuration. This aper is particularly significant since this three-electrode D8P is (as far as the authors of this review know) the only commercially available DCP at this point in time. As noted by Decker (and many others), this particular DCP was designed to be used in conjunction with a high-resolution echelle spectrometer system. Decker has made the following observations regarding this plasma: (A) for atoms the position of maximum line intensity in the plasma is determined by the norm temperature of the spectral line, (B) the source is stable over long periods of time, (C) high concentrations of alkali metals in the sample can disturb the plasma resulting in an enhancement of both atomic and ionic spectral lines, (D) detection limits are generally less than 1 order of magnitude higher than those obtained with an ICP, and (E) precision of analysis is better than 2% expressed as relative standard deviation. Decker notes that the DCP is significantly less expensive than an ICP and that running costs are similar. Eastwood and co-workers (74E) have used the three-electrode DCP to determine transition metals and also beryllium in salt and brackish water. The effects of salinity on enhancement of emission intensities of the analyte lines were studied by using an empirical approach combined with statistical analysis. In another important paper, Johnson, Taylor, and Skogerboe (116E) have studied atomic and ionic emission enhancement in the three-electrode DCP. Their results showed that the addition of the concomitants (A) caused enhancements in both atomic and ionic emission, (B) did not cause significant changes in the electron temperature of the electron population of the plasma excitation zone, (C) resulted in a downward shift in the rotational temperature of that zone, and (D) did not cause significant changes in the efficiency with which analyte species were delivered to the DCP. Their observations indicated that the enhancement effect cannot be readily explained based on plasma temperature increases or the classical ionization repression mechanism. As an alternative, they suggested that the enhancement may result from increases in the population of metastable argon with coincident increases in excitation via collision with this species. Nygaard and Gilbert (168E) have also studied emission line enhancement in the three-electrode DCP. They note that enhancement is shown to be inversely related to the ionization potential of the matrix element. The temperature of the plasma core is shown to decrease in the presence of an easily ionizable element, while the effective temperature experienced by the analyte is shown to increase under the same conditions. Eisentraut and co-workers (46E)have used a three-electrode DCP to determine wear metals in aircraft lubricating oils, the method was reported to be much faster and convenient than previously reported methods. Bosch et al. (38E) have used a three-electrode DCP for the determination of phosphorus, boron, and arsenic in steel and Berndt and Messerschmidt (23E) have used the same source for the simultaneous determination of sodium, potassium, magnesium, calcium, lithium, iron, copper, and zinc in human serum. Czech and Wunsch (62E)have determined tungsten in steels and alloys with a three-electrode DCP. The relative intensities of 17 tungsten spectral lines are listed. Smith (195E) has used a three-electrode DCP to determine mercury in iodine monochloride. The method was reported applicable over the range 0.50 to at least 130 pG Hg mL and it was stated to be about 10 times faster than flame ess AAS for the purpose. Bricker (43E) used his own designed helium DCP to determine mercury in natural waters at the low parts-per-trillion level. Coleman, Braun, and Allen (61E) have described several modifications to a two-electrode DCP (no longer commercially available) resulting in significantly enhanced analysis capabilities. The authors comment that reducing the electrode an le, decreasing the aerosol chimney size, and operating in a diffuse mode with helium provide improved stability, sensitivity, freedom from interferences, and detection limits. In a related publication, Williams and Coleman (2263) have noted that background corrected ion and atom emission profiles for group 2 elements in the two-electrode DCP show great variation in both vertical and horizontal emission zones.
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Kovacic and co-workers (131E,206E) have interfaced a DCP with a mass spectrometer in order to study the products have studied formed in the plasma. Nakao and Tanaka (1631%‘) lower hybrid waves with a DCP, Grankin et al. (IOOE)have used a DCP for ion sputtering, and Dittrich, Niebergall, and Zschoke (67E) have performed quantitative temperature measurements in a DlCP. Glow Discharge ]Lamps (GDL). In a series of papers, Alimonti, Caroli, and Senoforte have described a modified Grimm GDL for use a13 a demountable emission source. Their first paper (6E)gives construction details and the next paper in the series describes (55E) current-intensity-voltage characteristics. Yet another paper (193E) gives data on the behavior of blackening curves for copper. DeGregorio et al. (6%‘) discuss the determination of iron in steel using a GDL and Klockenkaemper et al. (127E) compare X-ray analysis with emission using a GDL by applying both methods to the analysis of silver-copper binary alloys. Both analysis methods were considered suitable. In a related paper, Dogan (70E)has used a GDL ao a souirce for binary analysis. Much of the work on GDL’s continues to come from the National Physical Research Laboratory in South Africa and the last 2 years have seen several important publications. Ferreira and Human (88E) have studied the sputtering of atoms from the cathode of a modified Grimm-type GDL and Ferreira, Human, and Butler (89E) have discussed kinetic temperatures and electron densities in the plasma of a side view Grimm-type glow discharge. Human, Strauss, and Butler (111E)have determined carbon, phosphorus, and sulfur in steel and cast iron with a GDL and an atomic fluorimeter as spectral line isolator. Walters and Human (2233)have used a GDL with supplementary excitation by an rf discharge, some preliminary measurements were reported. Ferreira, Kruger, and Human (9OE)have made line profile measurements of radiation from a GDL, in a magnetic field. Zeeman splitting was shown to be present in the source. Kruger, Bombelka, and Laqua (132E) have discussed some basic characteristics of the Grimm magnetic field GDL with reference to steel analysis and have also (133E) applied the source to the analysis of mild and alloyed steel. Durr and Vandorpe (72E) have compared a GDL and a spark source for the routine analysis of steels and nickel alloys and Bubert and Hagenah (49E)have excited several elements in Grimm GDL; radiation was detected by a silicon photoarray showing good response From 500 to 1000 nm. Calibration curves, detection limits, and the weight fractions of the elements lithium, rubidium, barium, sodium, potassium, and lanthanum in rock samples are reported. Chang et al. (57E) have described a new GDL source and Mikoshiba et al. (149E) have described a low-pressure xenon discharge tube. Bezlepkin et al. (24E) have commented on various sources with selective modulation for AAS and Larkins (134E) has described a gas control unit for use with cathode sputtering celk. Feldman (86E)has used a helium GDL for the determination of fluorine and, in a related paper, Tomkins and Feldman (2?07E)have determined primary and secondary amines in energy relatled materials using an element selective GDL detector. The derivatized amines are separated by gas chromatography and specifically detected by using a GDL tuned to a fluorine line at 685.6 nm. As little as 14 ng of fluorine can be detected with a selectivity of at least 2OO:l. Hollow Cathode Discharges. I n a significant paper, Mehs and Niemczyk (145E) have studied excitation temperatures in a hollow cathode discharge. It was found that the temperatures measured do not significantly change over the range of conditions studied. These results were compared to those obtained in other low-pressure discharges and temperature values as well as trends were found to be very similar. Dobrosavljevic and Pesic (69E) have measured rotational temperatures in an uricooled hollow cathode discharge and Gyulgerova et al. (73E) have measured the intensity of the copper 324.7-nm line and the concentration of copper atoms in a hollow cathode diincharge under pulsed and steady-state conditions. Caroli and Senoforite (56E) have compared the hollow cathode with a GDL for aluminum and graphite analysis; in general, the hollow cathode source gave better reproducibility. Thelin (205E)has used a high-temperature discharge for the determination of trace elements in steels, nickel-based alloys, and ferroalloys while Goebel et al. (94E)have discussed lan-
thanum and molybdenum emission in hollow cathode discharges. Hershcovitch and Prelec (104E) have used hollow cathode discharges for H-production. Inductively Coupled Plasmas (ICP). The increasing popularity of the ICP is clearly seen in the number of citations in this section of the review compared to the previous review (14A). Many fundamental and applied papers have appeared during the past 2 years. Winefordner and co-workers at the University of Florida have continued their fundamental studies and have reported on molecular emission spectra in the ICP (180E),noise power spectra in the ICP (216E),atomic and ionic fluorescence spectra with pulsed dye lasers in the IICP (84E),and relative spatial profiles of barium ions and atoms in the ICP as obtained by laser excited fluorescence (170E). Savage and Hieftje (187E) have characterized the background spectrum from a miniature ICP. The complex nature of the background emission spectrum from the mini-ICP indicates that careful line selection criteria and background correction procedures should be employed. In a related paper, Savage and Hieftje (186E) discuss some vaporization and ionization interferences in the mini-ICP. The thesis by Savage (185E)gives more details on this subject. Lowe (138E) has described a low argon flow ICP utilizing a flame-AAS nebulizer and, in a particularly interesting publication, Ebdon et al. (76E) have described a new versatile torch for ICP spectrometry. Their demountable torch incorporates a flared intermediate tube, a capillary injector tube, and internal jets a t the gas outlets. The new torch can be operated over a wide range of gas flows and shows considerable promise as an argon-cooled ICP. Ebdon et al. (75E)have also applied a variable step-size simplex procedure for the ICP. Koirtyohann et a1 (129E) have used an automated profile Nystem to determine vertical intensity distributions for atomic and ionic lines of several elements in the ICP; this paper also discusses the nomenclature system for the ICP mentioned previously (1ID). A most important “ICP Center” is certainly Ames, Iowa, and Fassel and his co-workers at Iowa State University continue their ICP studies with several important publications appearing in the past 2 years. Montaser, Fassel, and Zalewski (154E) have critically compared argon and nitrogen-argon lCPs using ultrasonic nebulization in this study. In another paper, Montaser, €passel,and Larsen (153E) describe a convenient and rapid technique to estimate the electron number densities, ne,in ICP spectrometry. The method is based on previously reported observations that the principal quantum number of the last discernible line in a series limit depends upon ne. As noted previously, Fassel and co-workers have interfaced the ICP with mass spectrometry (39C) and Houk, Svec, and Fassel (L07E) have recently provided mass spectrometric evidence of suprathermal ionization in an ICP. In related work, Edelson and Fassel (77E)have performed isotopic abundance determinations using an ICP. Blades and Horlick (27E-29E) have described some interesting spatial characteristics of analyte emission with an ICP and Horlick and Blades (106E) have classified some alnalyte emission characteristics of an ICP using emission spatial profiles. Salin and Horlick (182E) have discussed signal-to-noiseratio performance characteristicsof an ICP and IIeine et al. (103E) have commented on some qualitative aspects of an ICP between 120 and 185 nm. Another important “ICP Center” is certainly Atlanta, Georgia, and Browner and his associates at the Georgia Institute of Technology have continued their ICP studies concentrating on sample introduction and fundamental stud ies. In addition to the nample introduction papers already cited ( I l C , 18C, 19C, 62C-65C), Black and Browner (25E) have dlescribed a volatile metal-chelate sample introduction system fior the ICP and Black, Thomas, and Browner (26E) have applied the system to biological materials. In an important paper, Borowiec et al. (37E)have discussed interference effects from aerosol ionic redistribution in analytical atomic spectrometry. Examples of interference effects attributable to aerosol ionic distribution in flame and ICP sources are discussed. At yet another important “ICP Center”, Barnes and his colleagues at the University of Massachusetts continue their fundamental studies. Barnes and Meyer (15E) have constructed a low-power ICP (nitrogen discharge) for spectrochemical analysis and Barnes and Schleicher (14E)have made ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
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temperature and velocity distribution measurements in an ICP. In related work, Barnes and Genna (13E)discuss gas flow dynamics in an ICP and Boulos, Gagne, and Barnes (40E) have studied the effect of swirl on flow and temperature fields in the ICP. Kirkbright and his research associates (now at the University of Manchester Institute of Science and Technology, England) are continuing their ICP studies, recent papers include Millard, Chan, and Kirkbright (150E)describing a ICP sample introduction system with a graphite rod vaporization device and Alder, Bombelka, and Kirkbright (2E)discussing electronic excitation and ionization temperature measurements in an ICP. Boumans and co-workers (41E), in an important paper, have analyzed the limiting noise and identified some factors that dictate detection limits in a low-power ICP, and Mermet and co-workers (16E,148E)have continued their spectrometric studies of a 40-MHz ICP with a discussion of spectral interferences and line intensities (148E)and of the argon continuum in the visible region of the spectrum (16E).In the latter paper, the authors state that radiative recombination is predominant below 500 nm but “bremsstrahlung” must be considered above that wavelength. Nonmetal atomic emission in the ICP is the subiect of several reDorts boron (99E.218E). bromine (109E), carion (108E,IlOEj,chlorine (109E),fluorhe (91E), hydrogen (108E), nitrogen (&E, 108E,167E),oxygen (47E.108E.166E).DhosDhorus (113E.152E.156E.219E).and sulfur (llOE,135Ei217E,221E). Most of these studies were done either in the near-IR or in the vacuum UV. Fuwa, Haraguchi, and co-workers have published an interesting paper (210E)on the spatial distributions of metastable argon, temperature, and electron number density in an ICP. Some AA measurements in the ICP were also reported using an MIP as a light source. Another paper (211E)also describes the AA measurements. In this connection, we should note Magyar and Aeschbach’s interesting paper (139E)entitled “Why not ICP as Atom Reservoir for AAS?” (This paper appeared in the Alan Walsh honor issue of Spectrochimica Acta (91A)JKawaguchi et al. (123E)have studied the effects of the matrix on spatial emission profiles in an ICP and have also performed some gas temperature measurements (124E).Morita, Uehiro, and Fuwa (157E)discuss speciation and elemental analysis of mixtures combining HPLC with an ICP, and Kalivas and Kowalski (120E)have developed a generalized standard addition method for elimination of interferences with an ICP. Some very pra matic papers have appeared in the past 2 years. Greenfielf and Burns (101E)have compared argoncooled and nitro en-cooled plasma torches under optimized conditions basecf upon the concept of intrinsic merit. The differences found suggested that the mode of excitation may be different in argon and in nitrogen containing systems. Wallace (220E)has described a torch extension device to reduce ICP base line structure, Ediger (78E-81E)has commented on the optimization of ICP background correction, Devine, Brown, and Fry ( M E )have developed a method for extending or repairing ICP torches, and Terblanche et al. (203E)have developed a modified sequential simplex optimization method for ICP spectrometry. Montaser and Mortazavi (155E)have described ICP spectrometry with an argon-nitrogen atmosphere and Nikdel and Winefordner (165E)have discussed the interference of potassium on barium measurements in the ICP. Nikdel’s excellent Ph.D. thesis (164E)provides a wealth of detailed information on the utilization of ICPs in emission spectrometry and also in AFS. Jacinth0 et al. (115E)discuss flow injection systems that can be used with the ICP. The ICP has been used for the determination of minor and the determination of trace elements in silicate rock (212E), arsenic (44E,158E,161E,175E),the determination of selethe determination of arsenic and selenium in soils (176E), the determination nium in water, fish, and sediments (98E), the determination of chromium of cerium in paint (227E), (151E), the determination of various metals in sewage and the determination of various metals sewage effluents (159E), the determination of silicon and aluminum in serum (192E), the determination of various in biological materials (137E), trace metals in seawater using dithiocarbamate preconcenand the simultaneous determination of major, tration (144E), minor, and trace elements in marine sediments (143E). Suddendorf et al. (198E)have described a simple apparatus 196R ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
for the determination of mercury by either AAS or with the ICP, and Hiraide et al. (105E)have developed a multielement preconcentration technique for trace metals involving coprecipitation and flotation with indium hydroxide. Hausler and Taylor (102E)have used size exclusion chromatography of organically bound metals and coal-derived materials with the ICP and Broekaert, Leis, and Laqua (45E)have discussed the application of the ICP to the analysis of organic solutions. Ikeda et al. (112E)have determined lead a t the parts-perbillion level by reduction to plumbane and measurement in the ICP. Microwave Discharges. Bollo-Kamara and Codding (35E)have published a very interesting paper discussing some considerations in the design of an MIP utilizing the TMolo (Beenakker type) cavity. The design of a unique plasma discharge tube is presented. This discharge tube was reported to utilize a tangential support gas flow (argon or helium) to generate a suspended plasma discharge which does not touch the wall of the discharge tube. The resulting discharge was reported to have superior spatial and temporal stability compared to previously reported plasma discharges. The use of TMoloresonant cavities having 2 and 3 cm internal thicknesses is discussed. These cavities result in physically longer plasmas providing greater analyte residence times and enhanced analytical performance. Results with and without prior aerosol desolvation are presented. Goode and Otto (96E)have made some fundamental measurements of an atmospheric-pressure MIP. Optical and electrical measurements were made on argon and argon/nitrogen plasmas in the region 1-7 cm outside the Beenakker type cavity, as the applied microwave power and the plasma composition were varied. The stability of the plasma, atomic emission from the argon support gas, and emission fom the analyte species were reported proportional to the electron density. In related work, Goode and Pipes (97E)have discussed the constriction of an MIP by a magnetic pinch and Goode et al. (95E)have built a high-power microwave supply for EDL’s and other spectrochemical emission sources. Alder, Jin, and Snook (3E,4E)have used a helium MIP for the determination of traces of chloride in solution. The method is based on the evolution of chloride from a KMn04 solution in HzS04 and measurement of the C1 molecular emission at 257 nm. The detection limit was reported to be 10 ng and log-log calibration plots were reported linear over several orders of magnitude. Volland, Tschopel, and Tolg (215E)have determined traces of elements in the nanogram and picogram range with a helium MIP after electrolytic preconcentration in a graphite tube followed by electrothermal atomization. Different types of MIP excitation sources were investigated. Ishizuka and Uwamino (114E)have analyzed solid samples with laser vaporization into an MIP and Wrobel et al. (229E)have described polymerization of organosilicones into microwave discharges. Burridge and Hewitt (53E)have described a procedure for fiiling a discharge tube, permanently attached to a vacuum line, with NH3 in the range 1.5-5 torr, without any carrier gas. The l6N:l4Nisotope ratio is determined from the Nz spectrum emitted when the tube is excited by a 2450-MHz microwave source. Bosisio et al. (39E)have discussed oil desulfurization using microwave plasmas, Glangetas (93E)has described a new design for a microwave discharge lamp, Aston (9E)has used a microwave discharge to initiate a HCL discharge, and Sturgeon et al. (197E)have used microwave attenuation to determine electron concentrations in graphite and tantalum tube electrothermalatomizers. Wong has characterized (2283) an atmospheric pressure argon MIP and Outred (174E)has performed microwave power measurements for microwave excited EDL sources. Ferraro and co-workers (87E)have discussed improved instrumentation for mercury determination by AFS with an EDL and Tanabe, Chiba, and Haraguchi, in a particularly interesting paper, have determined mercury at the ultratrace level by atmospheric pressure helium-MIP spectrometry. A Beenakker type cavity was used in this investigation. MIPShave been used as chromatographic detectors by S a r t ~ et al. (183E), Bauer and Natusch (17E), Mulligan, Caruso, and Tanabe et al. (202E), and Wasik and Schwarz Fricke (160E), (2243). Atsuya and Akatsuka (1OE)have used a capacitively COUpled microwave plasma to determine trace amounts of arsenic
EM I SS ION SPECTROMETRY
in sewage sludge, iron, and steels. A hydride generation technique was used. In related work, Akatsuka and Atsuya (1E) determined nickel in various materials. Beenakker, Boummls, and Rommers (18E)have reviewed the MIP as an excitation source for AES and, as previously mentioned, an excellent in-depth review has very recently been published by Zander and Hieftje (107A). Spark Discharges. In 1939, Kaiser and Wallraff published a classical paper in German on electrical sparks and their use for excitation of spectra. This paper has recently been republished in English (219E) in Spectrochirnica Acta and is, we feel, “must reading” for anyone interested in spark discharges. The translators of the article, I). B. Farnsworth and J. P. Walters of the University of Wisconsin, state in their introduction (85E)to the article that “the experiments reported in the article are of themselves of such remarkable quality that the passage of 40 years has not diminished their value”. The authors of this review certainly concur!!! Walters and his research associates have continued their fundamental studies of spark discharges and several very important papers have appeared during the past 2 years. Klueppel and Walters (128E) have described a series of experiments designed to characterize the physical and chemical nature of spark discharges in argon at atmospheric pressure. Results are reported concerning the expansion properties of the spark and the distribution and longevity of cathode material in and around the spark channel following cessation of the discharge current. Scheeline, Travis, DeVoe, and Walters (19OE)have observed an electrical pulse of negative polarity in the vicinity of a high-voltage spark. The pulse’s behavior with respect to spark cathode composition, gas flow, spatial distribution, and related parameters was characterized. The same authors (Y89E)hlave also recently commented on particulates formed by a stabilized high-voltage spark discharge. Ekimoff and Walters (83E) have discussed the emission and electrode erosion properties of a positionally stable spark discharge train, Scheeline (188E)hac3 derived equations for computing the current waveform and instantaneous power dissipation in high-voltage spark sources containing a branched waveshaping network. For constant or dual valued circuit parameters, examples of waveform characteristics are presented. In related work, Thang and Scheeline (204E)have described a compact adjustable waveform spark source. Oberauskas et al. (169E)have studied spark discharges between aluminum and aluminum-copper electrodes in air at atmospheric pressure. The relationship between the measured characteristics and plasma, and spectral-lineparameters is discussed. Kishi (125E, 126E) has studied negative ions formed by vacuum spark discharges and Coleman et al. (60E) have discussed high-frequency excitation of spark sampled metal vapor. Spark discharges in iodine vapor have been studied by Lewis and Woolsey (136E),Bommelli (36E) has studied the nature and lifetime of dielectric contaminants in spark discharges, and Maly (141E) has developed an ignition model for spark discharges. Blythe and Carr (30E) have characterized propagating electrostatic discharges on dielectric films and Andreev et al. (71F) have studied a long sliding spark. Malamad, Daigne, and Armand (140E)have used a large vacuum W spectrograph in conjunction with spark techniques to determine oxygen initrogen, hydrogen, and carbon in a variety of alloys. Lastly (admittedly a nonanalytical application) Johnson (117E)has studied the ignition of flammable vapors by human electrostatic discharges. Other Excitation Papers. D’Silva, Rice, and Fassel (71E) have described an Atimospheric Pressure Active Nitrogen (APAN) source for analytical spectrometry. The afterglow source was generated in pure flowing nitrogen excited in an electrodeless ozonizer discharge. The afterglow, which contains several metastable species, was observed to be an efficient source for the excitation of atomic emission through energy transfer. The application of the APAN afterglow source for the detection and determination of ultratrace levels of mercury, arsenic, bkmuth, germanium, lead, antimony, selenium, tin, and tellurium was documented in the paper. Melzer, Jordan, and Sutton (147E)have determined trace amounts of lead by methistable transfer emission spectrometry and Mehs and Niemczyk (146E) have discussed plasma models applicable to lovv-pressure discharges. Srivastava and Ghosh (196E) have reported on population densities of He(1) and
He(I1) excited states and Brenning (42E) has measured electron temperatures in low-density plasmas. Fujiwara et al. (92E)have evaluated selectivity in emission spectrometry. Sacks and co-workers have continued their studies with exploding thin film excitation, in one paper (199E) they describe a saturable inductor based controlled waveform source and in another paper (200E) they comment on excitation temperature, degree of ionization of added iron species, and e1,ectron density in an exploding thin film plasma. Clark and Sacks (59E) have used the technique for the direct determination of selected metals in refractory powder microsamples. In somewhat related work, Nakajuma et al. (162E) discuss shock tube excitation of powdered samples. Molecular Emission Cavity Analysis (MECA) continues to be studied with most of the reports coming from the same group of workers. Burguera, Bogdanski, and Townshend ( 5 0 9 have recently published a detailed MECA review. Burguera and Townshend (51E) have reported on an improved method for boron using the technique, and Burguera, Townshend, and Bogdanski (52E) have described a method for fluoride using SiF4volatilization. E3ogdanski, Henden, and Townshend (31E) used a flame generator within the MECA cavity to determine bloron and selenium, and Bogdanski, Townshend, and Yenigul (33E)determined sulfite in soft drinks. MECA has also been used for sulfate @E, 32E), selenium (19E, 130E), amines (181E), and ammonium (20E). Cardwell et al. (54E) have studied the effect of variation in cavity position on the sulfur etnission and Osibanjo and Ajayi (173E) have developed an interesting method for phenol using MECA. Tribromophenol is produced from phenol, filtered off, and determined by production of InBr emission a t 376 nm in an air-hydrogennitrogen flame. Recoveries of 97-99% were obtained from spiked lake water.
SELECTED APPLICATIONS Because of space considerations, we have chosen only a very few typical applications of emission spectrometry for this section. As indicated previously, reviews and compilations of practical emission spectrochemical applications can be found in the “Annual Reports on Analytical Atomic Spectroscopy” (24A,86A) and in the Application Reviews of this journal (2A). Falk, Hoffmann, and Ludke (4F) have developed Furnace Atomic Nonthermal Excitation Spectrometry (FANES) a new technique that should find useful application. The sample wpor is formed by an electrothermal furnace excited with the hlelp of a glow discharge. The limits of detection found with FANES were reported to be comparable with the best furnace-AAS values and better than ICP values. The technique was used to determine the silver content of gold wife. Bellary et al. (IF) have used spectrographic analysis to dietermine various elemenb in rocks and soils and, in related work, have (2Fj determined trace elements in soil samples. Brenner et al. (3F) have applied ICP spectrometry to the analysis of geological and related materials for their rare-earth content and Hamner and De’Aeth (6F) determined boron in silicon bearing alloys, steel, and other alloys by pyrohydrolysis and ICP spectrometry. Hoult (7F)has determined sulfur, miagnesium, sodium, and potassium in brines by ICP emission spectrometry and Kurosawa et al. ( 1 2 9 have performed the simultaneous determination of metallic elements in precipitates and inclusions extracted from steel by ICP spectrometry. Manzoori ( 1 3 9 has used an ICP to determine molybdenum, cobalt, and boron in soil extracts. Some interferences caused by common metals and acids were noted. Sturgeon et al. (16F) hiwe compared several methods for the determination of trace elements in seawater. Fuller, Hutton, and Preston (5F) have compared flame, electrothermal, and the ICP atomic techniiques for the direct analysis of slurries. Kamat et al. (9F, 1OF) have determined trace impurities in semiconductors wing a dc arc spectrochemical method with carrier distillation and Walsh (19F)has developed a simultaneous method for the determination of various metals in silicate rock. Sommer, Ohls, and Koch (15F) have determined tin in metals using the ICP with hydride generation and Sugimae (17F,18F) has determined various elements in water with the ICP. Kitagawa et al. (11F) have studied the degree of atomization for an electrothermal atomizer by comparing the emission lines of copper atoms and CuCl molecules and ANALYTICAL CHEMISTRY, VOL. 54, NO. 5, APRIL 1982
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Pahlavanpour, Thompson, and Thorne (14F)have determined traces amounts of arsenic, antimony, and bismuth in soils and sediments using hydride generation in conjunction with the ICP.
MEETINGS We fiiish this review as we did 2 years ago (14A)by making some general comments about important meetings since trends and events of importance can be gleaned from meetings. The most important meeting of the past 2 years was certainly the recently held Colloquium Spectroscopicum InternationaleInternational Conference on Atomic Spectroscopy (CSI/ ICAS). The 22nd CSI/9th ICAS joint meeting was held in Tokyo, Japan, from Sept 4 to 8th, 1981. Approximately 700 scientists from all over the world attended this meeting and the quality of the papers was particularly excellent. There was even a local (English language) newspaper report (8F)on this important conference. There were four plenar presentations (L. S. Birks, V. A. Fassel, G. F. Kirkbright, Walsh) and many invited presentations. The Conference Organizers H. Kamada (Organizing Committee) and K. Fuwa (Program) and their associates did an outstanding job in putting together this CSI-ICAS meeting. Several pre- and postconference meetings were held in Japan in conjunction with the CSIICAS. The Spectroscopical Society of Japan had a preconference discussion on the ICP held at Shirakabako-Lake in the beautiful Japanese Alps. This well run meeting was organized by K. Maeda of the Society. H. Haraguchi and K. Fuwa held a preconference meeting at the Universit of Tokyo that was well attended. Postconferences were heldlin Kyoto, Okayama, and Fukuoka. The 23rd CSI/lOth ICAS meeting will be held in Amsterdam, The Netherlands, from June 26 to July 1,1983. Information on this meeting may be obtained by writing to Professor L. DeGalan, Laboratory for Instrumental Analysis, Technische Hogeschool Delft, The Netherlands. The 1980 American Chemical Society meetings were held in Houston, TX, and in Las Vegas, NV. The Las Vegas meeting was switched to that city because of a hotel strike in San Francisco and, as we had mentioned previously (14A), there was a symposium at that meeting on "Atomic Spectroscopy for the 809". The 1981 meetings were held in Atlanta, GA, and in New York City. Recent Pittsburgh Conferences have been held in Atlantic City, NJ, and this very large conference with an extensive exhibition of scientific equipment just seems to grow and grow approaching 20 000 attendees. The Federation of Analytical Chemistry and Spectroscopy Societies (FACSS) continues to stay in Philadelphia. FACSS meetings have developed, over the past few years, into highly regarded North American meetings held annually in the autumn. The 1981 FACSS meetin was held from September 20th through 25th at the Philafelphia Sheraton, but 1982 through 1984 meetings will be held at the new Franklin Plaza Hotel in the center of Philadelphia. Meeting dates are: September 19-24,1982; September 25-30,1983; September 23-28,1984. Further information on these meetings can be obtained by writing to one of the authors (P.N.K.) of this review. A limited number of 1980 and 1981 Program and Abstract booklets are available upon request. The 29th Annual Conference of the Spectroscopy Society of Canada has conveniently been set to follow the 1982 FACSS and will be held in the Laurentian Mountains (ca. 75 miles N.W. of Montreal) from September 26 to 29, 1982. Information on this meeting may be obtained from Dr. Ian S. Butler, Chemistry Department, McGill University, Montreal, Quebec, Canada. The 1980 Winter Conference on Plasma Spectrochemistry was held in Puerto Rico and the 1982 Winter Conference has just been held (January 4-9th) in Orlando, FL. This very specialized conference provides a forum for workers using various types of plasmas (DCP, ICP, MIP) to communicate with each other. This was a very successful meeting and, in fact, parts of this review were written (under a palm tree) during this conference. A 1984 Winter Conference is tentatively planned; information on this may be obtained from Dr. Ramon M. Barnes, Chemistry Department, University of Massachusetts, Amherst, MA 01003. Another interesting "club-type" conference is the National Conference on Spectrochemical Excitation and Analysis. The
1.
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1981 meeting was held on the island of Martha's Vineyard (off the coast of Massachusetts) in September. The 1982 meeting will be held at the same delightful location from September 7-10. Information on this meeting can be obtained from Mr. Hank Griffin, Texas Instruments, MS10-16, 39 Forest Street, Attleboro, MA 02703. The 8th International Microchemical Symposium (IMS) was held in Graz, Austria, in 1980 and the 9th IMS is scheduled to be held in Amsterdam from August 28 through September 2, 1983. There will undoubtedly be many presentations of interest to emission spectroscopists. Information on IMS 83 is available from the Municipal Congress Bureau, Oudezijds Achterburgwall99, Amsterdam, The Netherlands. The Annual Symposium on the Analytical Chemistry of Pollutants continues to alternate between the United States and Europe with the 1981 meeting in Jekyll Island, GA, and the 1982 meeting in Amsterdam. The 1983 meeting is scheduled to be held on Jekyll Island from May 16th through 18th and further information on this meeting can be obtained from Ms. Elaine McGarritv, _ . EPA. College Station Road. Athens, GA 30613. Finally, a new British meeting should be noted, the First Biennial National Atomic Spectroscopy Symposium. This will be held in Sheffield, England, from July 13 through 15, 1982. Information on this meeting may be obtained from Miss P. E. Hutchinson, Royal Society of Chemistry,Burlington House, London W1V OBN, England. It should be noted, in concluding this review, that the Annual ReDorts on Analvtical Atomic Swectroscowv (24A. 86A) lists papers present6d at all of the major mee6Ggs in a particular year. Full author addresses are given allowing interested persons to directly contact the author(s) for more information. This provides a most useful service. I
ACKNOWLEDGMENT The following all helped, in various ways, in the preparation of this review and we wish to thank them here: Mark Asteris, Ramon M. Barnes, Koichi Chiba, Bernard J. Downey, John R. Edwards, Mary L. Finley, Richard D. Furman, Keiichiro Fuwa, Lawrence C. Gallen, William L. Greene, Jr., Hiroki Haraguchi, Howard A. Harner 111,Bonnie M. Keliher, Mark Keliher, Claire Keliher, Bonzo Keliher, Gordon F. Kirkbright, Kogoro Maeda, James J. Markham, Joseph S. McDonnell, Tahei Miki, Lydia Moccero, George Norwitz, Barry L. Sharp, and Andrew T. Zander. LITERATURE CITED BOOKS AND REVIEWS
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(197E) Sturgeon, R. E.; Berman, S.S.;Kashyap, S.Anal. Chem. 1980, 5 2 , 1049-1053. (198E) Suddendorf, R. F.; Watts, J. 0.; Boyer, K. J . Assoc. Off. Anal. Chem. 1981, 6 4 , 1105-1110. (199E) Suh, S.Y.; Roiiins, R. J.; Sacks, R. D. A.m 1981, 3 5 . . / . Smctrosc. . 42-52. (200E) Suh, R. Y.; Sacks, R. D. Spectrochlm. Acta, Part B 1981, 36, 1081- 1098. (201E) Tanabe. K.; Chiba, K.; Haraguchi, H.; Fuwa, K. Anal. Chem. 1981, 53, 1450-1453. (202E) Tanabe, K.; MatSlJmOtO, K.; Haraguchi, H.; Fuwa, K. Anal. Chem. 1980. 5 2 . 2361-2365. (203E) Terblanche, S. P.; Visser, K.; Zeeman, P. B. Spectrochim.Acta, Part 151981, 36, 293-297. (204E) Thang, T.; Scheeline, A. Appl. Spectrosc. 1981, 3 5 , 536-540. (205E) Theiln, B. Appl. Spectrosc. 1981, 3 5 , 302-307. (205E) Todorovic, M.; Ikonomov, N.; Kovacic, N.; Rekaiic, M.; Peric, M. Fre.senius' Z . Anal. Chert. 1980, 302, 382-386. (207E) Tomkins, B. A.; Feklman, C. Anal. Chlm. Acta 1980, 119, 283-290. (208E) Tripkovic, M.; Todorovlc, M.; Vukanovic, V.; Simic, M. Fresenlus' Z . .4nal. Chem. 1981, 306, 362-364. (209E) Tripkovic, M.; Vukanovic, V. Spectrochlm. Acta, Part B 1981, 36, 1-8. (210E) Uchida, H.; Tanabe, K.; NoJlri, Y.; Haraguchi, H.; Fuwa, K. Spectroshim. Acta, Part B 1981, 3 6 , 711-718. (211E) Uchlda, H.; Tanabe, K.; Nojlri, Y.; Haraguchi, H.; Fuwa, K. Spectro,chlm. Acta, Part B 1980, 3 5 , 881-883. (212E) Uchida, H.; Uchida, T.; Iida, C. Anal. Chlm. Acta 1980, 116, 433-437. (213E) Van den Hoek, W. J.; Visser, J. A. J. Appl. Phys. 1980, 5 1 , 5292-5294. (214E) Venkatasubramanian, R. Anal. Lett. 1981, 14, 731-740. (215E) Volland, G.; Tshopel, P.; Toig, G. Spectrochim. Acta, Part B 1981, 36, 901-917. (216E) Waiden, G. L.; Bower, J. N.; Nikdei, S.;Bolton, D. L.; Winefordner. J. ID. Spectrochlm. Acta, Part B 1980, 3 5 , 535-548. (217E) Wallace, G. F. At Spectrosc. 1980, 1 , 38. (218E) Wallace, G. F. At Spectrosc. 1981, 2 , 81-84. (219E) Wallace, G. F.; Hoult. D. W.; Ediger, R. D. At. Spectrosc. 1980, 1 . 120-1 22. (220E) Wallace, G. F. At Spectrosc. 1981, 2 , 93. (221E) Wallace, 0. F.; Ediger, R. D. At. Spectrosc. 1981, 2 , 189-172. (222E) Waish, P. J.; Lama, W.; Hammond, T. J. J. Appl. Phys. 1981, 5 2 , 5467-5482. (223E) Waters, P. E.; Human, H. G. C. Spectrochim. Acta, Part B 1981, 3 6 , 585-589. (224E) Waslk, S. P.; Schwarz, P. F. J . Chromatogr. Scl. 1980, 18. 660-863. (225E) Watanabe, Y.; Yamane, M. J. Appl. Phys. 1980, 5 1 , 6124-6129. (226E) Wliiiams, R. R.; Coleman, G. N. Appl. Spectrosc. 1981, 35, 312-3 17. (227E) Wong, K. L. Anal. Chem. 1981, 53, 2148-2149. (228E) Wong, S. K. UTIAS Tech. Note 1980, 225, 81 pp. (229E) Wrobei, A. M.; Klemberg, J. E.; Wertheimer, M. R.; Schreiber, H. P. J . Macromol. Sci., Chem. 1981, A15, 197-213. SELECTED APPLICATIONS
(1F) Beiiary, V. P.; Kapoor, S. K.; Sankaran, A. V. Fresenlus' Z . Anal. Chem. 1981, 305, 390-393. (2F) Beliary, V. P.; Sarma, Y. A. Fresenlus' Z . Anal. Chem. 1980, 302, 276-280. (3F) Brenner, I. 6.; Watson, A. E.; Steele, T. W.; Jones, E. A,; Goncaieves, M. Spectrochlm. Acta, Part B 1981, 3 6 , 785-797. (4F) Faik, H.; Hoggmann, E.; Ludke, Ch. Spectrochlm. Acta, Part B 1981, 3 6 , 787-771. (5F) Fuller, C. W.; Huttonl, R. C.; Preston, B. Analyst (London) 1981, 106, 913-920. (6F) Hamner, R. M.; De'Aeth, L. A. Talanta 1980, 2 7 , 635-538. (7F) Houit, D. W. At. Spectrosc. 1980, 1 , 82-83. (8F) Japan Times, Tokyo, Japan, Friday, Sept 4, 1981, p 5. (9F) Kamat, M. J.; Kalmal, R.; Saranathan, T. R. Fresenlus' Z . Anal. Chem. 1981. 19-20 ., 307. ... .. (1OF) Kamat, M. J.; Sugandhi, V.; Saranathan, T. R. Fresenlus' 2 . Anal. Chem. 1980. 302. 59-61. (11F) Kitagawa, K l ' I d e , Y.; Takeuchi, T. Anal. Chim. Acta 1980, 113, 21-32. (12F) Kurosawa, F.; Tanaita, I.; Sato, K.; Otsuki, T. Spectrochim.Acta, Part B 1981, 3 6 , 727-733. (13F) Manzoori, J. L. Talnnta 1980, 2 7 , 682-884. (14F) Pahiavanpour, B.; Thompson, M.; Thorne, L. Analyst (London) 1980, 105. 756-763. (15F) Sommer, D.; Ohls, K.; Koch, A. Fresenius' Z . Anal. Chem. 1981, 306. 372-377. (16F) Sturgeon, R. E.; Berman, S.S.; Desauiniers, J. A. H.; Mykytiuk, A. P.; McLaren, J. W.; Russell, D. S. Anal. Chem. 1980, 5 2 , 1585-1588. (17F) Sugimae, A. Anal. Chim. Acta 1980, 121, 331-336. (18F) Sugimae, A. Kogai to Talsaku 1981, 17, 307-316. (19F) Waish, J. N. Spectrochim. Acta, PartB 1980, 35, 107-111. ~~~
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