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CRITICAL COMPARISON OF ICP-OES, XRF AND FLUORINE VOLATILIZATION-FTIR SPECTROMETRY FOR THE RELIABLE DETERMINATION OF THE SILICON MAIN CONSTITUENT IN CERAMIC MATERIALS

Kaiser, G. and Meyer, A. and Friess, M. and Riedel, Ralf and Harris, I. and Jacob, E. (1995):
CRITICAL COMPARISON OF ICP-OES, XRF AND FLUORINE VOLATILIZATION-FTIR SPECTROMETRY FOR THE RELIABLE DETERMINATION OF THE SILICON MAIN CONSTITUENT IN CERAMIC MATERIALS.
In: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY, 352 (3-4), Springer Verlag, New York, USA, pp. 318-326, ISSN 0937-0633,
DOI: 10.1007/BF00322228,
[Article]

Abstract

or the optimization of preparation processes for ceramic powders and compacts by pyrolysis of inorganic polymers, the intermediate and final products have to be monitored by in-situ analysis (in its original place) for main, subsidiary and trace components. In the determination of silicon in Si-N-C- based ceramic samples by ICP-OES after pressurized decomposition at temperatures between 220 degrees-250 degrees C too low concentrations of Si were found. Completely independent analytical procedures were applied to trace systematic errors, i.e. XRF after decomposition of the sample in a metaborate/boric acid melt and FTIR-spectrometry after reaction of the sample with fluorine. The low recoveries of Si were found to be due to losses, which amount up to 25% depending on the temperature and time applied for the pressurized decomposition. With the latter two procedures Si can be determined in the %-range with a relative standard deviation of less than or equal to 0.4% and less than or equal to 0.2%, respectively.

Item Type: Article
Erschienen: 1995
Creators: Kaiser, G. and Meyer, A. and Friess, M. and Riedel, Ralf and Harris, I. and Jacob, E.
Title: CRITICAL COMPARISON OF ICP-OES, XRF AND FLUORINE VOLATILIZATION-FTIR SPECTROMETRY FOR THE RELIABLE DETERMINATION OF THE SILICON MAIN CONSTITUENT IN CERAMIC MATERIALS
Language: English
Abstract:

or the optimization of preparation processes for ceramic powders and compacts by pyrolysis of inorganic polymers, the intermediate and final products have to be monitored by in-situ analysis (in its original place) for main, subsidiary and trace components. In the determination of silicon in Si-N-C- based ceramic samples by ICP-OES after pressurized decomposition at temperatures between 220 degrees-250 degrees C too low concentrations of Si were found. Completely independent analytical procedures were applied to trace systematic errors, i.e. XRF after decomposition of the sample in a metaborate/boric acid melt and FTIR-spectrometry after reaction of the sample with fluorine. The low recoveries of Si were found to be due to losses, which amount up to 25% depending on the temperature and time applied for the pressurized decomposition. With the latter two procedures Si can be determined in the %-range with a relative standard deviation of less than or equal to 0.4% and less than or equal to 0.2%, respectively.

Journal or Publication Title: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY
Volume: 352
Number: 3-4
Publisher: Springer Verlag, New York, USA
Uncontrolled Keywords: PYROLYSIS; DECOMPOSITION; COATINGS
Divisions: 11 Department of Materials and Earth Sciences
11 Department of Materials and Earth Sciences > Material Science
11 Department of Materials and Earth Sciences > Material Science > Dispersive Solids
Date Deposited: 22 Aug 2018 08:20
DOI: 10.1007/BF00322228
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