Accurate and precise spectrochemical analysis of Bi-Pb-Sr-Ca-Cu-O high-temperature superconductor materials

摘要

For quality tests of ceramic Bi-Pb-Sr-Ca-Cu-O supercounductor materials (precursors and final products) accurate stoichiometric determinations of the metalic 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 metod are multiline measurements of each analyte element, a new method of sepctral line selection for main component precision determinations, multi-component calibrations, and freqeunt external standardizartions. For this method the sum of the confidence intervals of all element determinations was less than 1%, and no systematic error was detected.