Atomic emission and atomic absorption spectrometric analysis of high-purity powders for the production of ceramics |
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Authors: | T. Graule A. von Bohlen J. A. C. Broekaert E. Grallath R. Klockenk?mper P. Tsch?pel G. T?lg |
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Affiliation: | (1) Stuttgart, Laboratorium für Reinststoffanalytik, Max-Planck-Institut für Metallforschung, Bunsen-Kirchhoff-Strasse 13, D-4600 Dortmund 1, Germany;(2) Institut für Spektrochemie und angewandte Spektroskopie, Bunsen-Kirchhoff-Strasse 11, D-4600 Dortmund 1, Germany;(3) Present address: ETH Zürich, Institut für Nichtmetallische Werkstoffe, Sonneggstrasse 5, CH-8092 Zürich, Switzerland |
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Abstract: | Summary Direct analysis methods and multistage combined analytical procedures for the determination of impurities at the g/g level and the upper ng/g level in high-purity powders of Al2O3, AlN, Si3N4 and SiC are described. Results obtained with a novel direct slurry-atomization technique using a Babington nebulizer and inductively coupled plasma optical emission spectrometry (ICP-OES) are presented. A comparison of analysis results of combined analytical procedures including wet chemical decomposition and determinations with graphite furnace atomic absorption spectrometry (ETAAS) or ICP-OES with those of slurry-atomization ICP-OES show the capabilities of this technique for routine analysis in production control. Detection limits for Al, B, Ca, Co, Cu, Fe, Mg, Mn, Si, Ti, W, V, and Zn in the matrices mentioned are between 0.03 and 2.5 g/g. For elemental concentrations 10 g/g relative standard deviations of the measurements are generally below 10%. The technique is shown to be a powerful tool for trace determinations in powder samples. This is shown by its use for analysis of a series of the ceramic powders mentioned and comparative results of other direct techniques such as total reflection X-ray fluorescence spectrometry and instrumental neutron activation analysis.
OES und AAS von hochreinen Pulvern für die Keramikherstellung Herrn Prof. Dr. G. Tölg zum 60. Geburtstag von seinen Mitarbeitern gewidmet |
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