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Pd-conditioned graphite tubes, placed in the furnace of an atomic absorption spectrometry instrument, are used for entrapment of germane as generated in an associated flow injection system. Two different approaches are tested with the ultimate aim to allow multiple determinations, that is, introduction of the modifier as a liquid Pd-salt solution, and use of electrolytically Pd-precoated tubes. While the former treatment resulted in satisfactory analytical performance, although requiring separate regeneration of the tubes prior to each sampling sequence, the electrolytically precoated tubes did not function at all. This in turn led to a closer investigation as to the function of Pd in entrapping hydrides and releasing the analyte. Based on evaluation of the behaviour of the two types of tubes, and supplemented by scanning tunnelling microscopy studies of tubes with and without modifier and treated in different manners, it is suggested that the role of Pd primarily is that of a catalyst, that the electrochemically precoated tubes do not allow the germane to be entrapped during the short contact time available, and that the liquid Pd-modifier do not affect the graphite tubes per se, yet must be injected prior to each analytical cycle.
Original languageEnglish
JournalJournal of Analytical Atomic Spectrometry
Volume12
Issue number5
Pages (from-to)585-588
ISSN0267-9477
StatePublished - 1997

    Keywords

  • Palladium modifier, Electrolytically pre-coated, Role of modifier, Hydride determination, Graphite tube, Scanning tunnelling microscopy, Germane, Flow injection
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