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

Abstract

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.

Critical aspects on preparation of Bi-2223 glassy precursor by melt-process

“…The oxygen contents in the glasses were determined by CGHE followed by a simultaneous detection of CO and CO 2 using a TC436DR, LECO. Both of these latter methods have been described in detail in [67][68][69].…”

Accurate determinations of Ge atom fractions in SiGe semiconductor chips using high performance ICP-OES

“…Kucharkowski et al 12,13 utilized ICP-OES to achieve similar measurements with superconducting materials. Multiple lines (typically 3) were selected for the analyte and internal standard elements in the determination of the stoichiometry.…”

“…Stoichiometric measurements on the SiGe semiconductors in the present study were performed using the high performance ICP-OES (HP-ICP-OES) approach. HP-ICP-OES and the approach used by Kucharkowski et al 12,13 are similar in principle but differ in execution. The approach of Kucharkowski et al utilizes volumetric measurements in the preparation of the standards and samples.…”

Investigation of a medium power radiofrequency capacitively coupled plasma and its application to high-temperature superconductor analysis via atomic emission spectrometry

“…For many years, the classical chemical methods of analysis based on wet procedures, such as complexometric and iodimetric titrations with and without photometric, potentiometric or coulometric equivalence point detection, have been used for the determination of the chemical and stoichiometric composition of the superconducting materials. [5][6][7][8][9][10] Although they offer a sufficient precision and accuracy, unfortunately the classical methods involve very complicated separation schemes for analyte or masking concomitants, and they are very time-and reagentsconsuming.…”

“…As a consequence more rapid and sensitive spectrometric procedures, especially based on inductively coupled plasma atomic emission spectrometry (ICP-AES) using scanning spectrometers and charge coupled device (CCD) or charge injection device (CID) multichannel spectrometers are required. [9][10][11][12][13] It is known that the quality of the superconducting materials is dependent on the precursor's purity, but its determination can only be achieved by using the ICP-AES method. 14 Therefore, ICP has been found to be a very robust and powerful excitation source for many applications in the product control, but it is too expensive to buy and maintain for some special applications, where smaller and cheaper spectral sources could be used.…”