Abstract
A method for the determination of trace impurities (U, Th, Ca, Fe, Cr, Ni, Cu, and Cd) in the refractory metals molybdenum and tungsten with isotope dilution mass Spectrometry (IDMS) has been developed. This method enables determinations of uranium and thorium down to the lowest pg/g level with high precision and accuracy. Selective chromatographic, extractive and electrolytic methods for the trace-matrix separation were combined with positive thermal ionization mass spectrometry. Different samples of high purity (4N) and of ultra high purity (UHP) materials for advanced technologies were analysed. The detection limits reached are (in ng/g): U 0.006, Th 0.008, Ca 10, Fe 19, Cr 0.5, Ni 0.6, Cu 2.7, and Cd 0.12. A comparison of results with other sensitive analytical methods (ICP-MS, GDMS, SIMS) makes obvious the urgent necessity of a reliable calibration method like IDMS because the analytical results obtained by the other methods often spread over a wide range.
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H. M. Ortner, W. Blödorn, G. Friedbacher, M. Grasserbauer, V. Krivan, A. Virag, P. Wilhartitz, G. Wünsch,Kontakte (Darmstadt) 1988, 38.
H. M. Ortner, W. Blödorn, G. Friedbacher, M. Grasserbauer, V. Krivan, A. Virag, P. Wilhartitz, G. Wünsch,Mikrochim. Acta 1987,I, 233.
H. M. Ortner, P. Wilhartitz, M. Grasserbauer,Key Engineering Materials 1989,29–37, 21.
S. Sawada, in:Proceedings of the 12th International Plansee Seminar 1989, Vol. 4 (H. Bildstein, H. M. Ortner, eds.), Metallwerk Plansee, Reutte/Tyrol, 1990, p. 201.
K.-H. Theimer, V. Krivan,Anal. Chem. 1990,62, 2722.
M. Grasserbauer, P. M. Charalambous, N. Jakubowski, D. Stuewer, W. Vieth, H. E. Beske, A. Virag, G. Friedbacher,Mikrochim. Acta 1987,I, 291.
K. G. Heumann, in:Inorganic Mass Spectrometry (F. Adams, R. Gijbels, R. van Grieken, eds.), Wiley, New York, 1988, p. 301.
K. G. Heumann,Fresenius' Z. Anal. Chem. 1986,324, 601.
J. D. Fassett, P. J. Paulsen,Anal. Chem. 1989,61, 643A.
P. Herzner, K. G. Heumann (in preparation).
H. M. Ortner, P. Wilhartitz,Fresenius' J. Anal. Chem. 1990,337, 686.
T. B. Gibbons,Adv. Mater. 1990,2, 217.
J. Völkening, K. G. Heumann,Adv. Mass Spectrom. 1986,10B, 1059.
A. Götz, K. G. Heumann,Int. J. Mass Spectrom. Ion Processes 1988,83, 319.
J. Trettenbach, K. G. Heumann,Fresenius' Z. Anal. Chem. 1985,322, 306.
K. G. Heumann,Int. J. Mass Spectrom. Ion Phys. 1972,9, 315.
K. G. Heumann, E. Kubassek, W. Schwabenbauer,Fresenius' Z. Anal. Chem. 1977,287, 121.
O. Kujirai, K. Yamada, M. Kohri, H. Okochi,Fresenius' Z. Anal. Chem. 1991,339, 133.
J. Peters, D. Thiessel, B. Bischofer,Fresenius' Z. Anal. Chem. 1990,336, 16.
J. Völkening, K. G. Heumann,Fresenius' Z. Anal. Chem. 1989,335, 478.
P. Chaudari,Spektrum Wiss. 1986, 106.
J. D. Meindl,Spektrum Wiss. 1987, 64.
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Herzner, P., Heumann, K.G. Ultra-trace analysis of U, Th, Ca and selected heavy metals in high purity refractory metals with isotope dilution mass spectrometry. Mikrochim Acta 106, 127–135 (1992). https://doi.org/10.1007/BF01242083
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DOI: https://doi.org/10.1007/BF01242083