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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. ; Meyer, A. ; Friess, M. ; Riedel, Ralf ; Harris, I. ; 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)
doi: 10.1007/BF00322228
Artikel, Bibliographie

Kurzbeschreibung (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.

Typ des Eintrags: Artikel
Erschienen: 1995
Autor(en): Kaiser, G. ; Meyer, A. ; Friess, M. ; Riedel, Ralf ; Harris, I. ; Jacob, E.
Art des Eintrags: Bibliographie
Titel: CRITICAL COMPARISON OF ICP-OES, XRF AND FLUORINE VOLATILIZATION-FTIR SPECTROMETRY FOR THE RELIABLE DETERMINATION OF THE SILICON MAIN CONSTITUENT IN CERAMIC MATERIALS
Sprache: Englisch
Publikationsjahr: Juni 1995
Verlag: Springer Verlag, New York, USA
Titel der Zeitschrift, Zeitung oder Schriftenreihe: FRESENIUS JOURNAL OF ANALYTICAL CHEMISTRY
Jahrgang/Volume einer Zeitschrift: 352
(Heft-)Nummer: 3-4
DOI: 10.1007/BF00322228
Kurzbeschreibung (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.

Freie Schlagworte: PYROLYSIS; DECOMPOSITION; COATINGS
Fachbereich(e)/-gebiet(e): 11 Fachbereich Material- und Geowissenschaften
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft
11 Fachbereich Material- und Geowissenschaften > Materialwissenschaft > Fachgebiet Disperse Feststoffe
Hinterlegungsdatum: 22 Aug 2018 08:20
Letzte Änderung: 22 Aug 2018 08:20
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