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Analysis of mo and its high-purity compounds, with preconcentration of impurities

Die Analyse des Molybdäns und seiner hochreinen Verbindungen. Anreicherung der Verunreinigungen

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Summary

A procedure for concentrating microimpurities (especially W) in high-purity Mo by extraction chromatography (stationary phase trioctylammonium hydrochloride) has been developed. Extraction with 1-phenyl-3-methyl-4-benzoylpyrazol-5-one in molten naphthalenediphenyl mixture was also examined, but proved less useful. The extraction of W in the presence of macroamounts of Mo is suppressed in the extraction chromatography, allowing quantitative separation of these two elements. The electrochemical behaviour of Mo and W in each other's presence has been studied and a polarographic technique for determination of 10−6 M developed. The polarographic results for W are not affected by the presence of a 100-fold ratio of Mo. If the extraction chromatography and polarographic analysis are combined, the detection limit for W in Mo appears to be 10−5%.

Zusammenfassung

Anreicherungsverfahren für Mikrobeimengungen (in erster Linie von Wolfram) in hochreinem Molybdän mit Hilfe der Extraktions-Chromatographie (unbewegliche Phase Trioktylammoniumchlorid) und der Extraktion mit leicht schmelzenden Extraktionsmitteln (PMBP-Naphthalin-Diphenyl) wurden untersucht. Die Unterdrückung der Wolfram-Extraktion durch Makromengen Molybdän wurde bei der Trennung ausgenützt. Das elektrochemische Verhalten von Mo und W bei gemeinsamer Anwesenheit wurde untersucht und die Methodik der polarographischen Bestimmung von 10−6 M Wolfram ausgearbeitet. Die Anwesenheit eines 100fachen Überschusses an Molybdän beeinflußt die Ergebnisse für Wolfram nicht. Bei Kombination des extraktions-chromatographischen Verfahrens mit der Polarographie beträgt die Bestimmungsgrenze für Wolfram in Molybdän 10−5%.

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Authors and Affiliations

  1. Institute of Solid State Physics, Chernogolovka, The USSR Academy of Sciences, USSR

    S. S. Grazhulene, S. A. Poluyanova, O. I. Charitonova & Y. I. Popandopulo

Authors
  1. S. S. Grazhulene
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  2. S. A. Poluyanova
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  3. O. I. Charitonova
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  4. Y. I. Popandopulo
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Grazhulene, S.S., Poluyanova, S.A., Charitonova, O.I. et al. Analysis of mo and its high-purity compounds, with preconcentration of impurities. Mikrochim Acta 77, 231–242 (1982). https://doi.org/10.1007/BF01237811

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  • DOI: https://doi.org/10.1007/BF01237811

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