For quality tests of ceramic Bi-Pb-Sr-Ca-Cu-O superconductor materials (precursors and final products) accurate stoichiometric determinations of the metallic major components are necessary. Three methods were developed during the last decade in our group. Their properties and the results obtained are compared. The first classical analytical procedure requires to much manpower. The second combined chemical-spectrometric procedure is a routine method today, but also unsuitable for rapid tests. A new fully spectrometric procedure was recently developed using a simultaneously working Echelle spectrometer with CID detector, autosampler and a special self-made data evaluation software. The basis of this method are multiline measurements of each analyte element, a new method of spectral line selection for main component precision determinations, multi-component calibrations, and frequent external standardizations. For this method the sum of the confidence intervals of all element determinations was less than 1%, and no systematic error was detected.
Seit langem lassen sich Metalle und einige Nichtmetalle in Lösungen mit Hilfe der optischen Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP‐OES) bestimmen. Durch die Kombination der ICP‐OES mit einer elektrothermischen Verdampfungseinheit‐ähnlich dem Graphitrohrzubehör der AAS‐ist es möglich, Elemente direkt aus Feststoffproben qualitativ und quantitativ zu analysieren, ohne sie vorher aufzuschließen.
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