Direct analysis of silicon carbide powder by total reflection X-ray fluorescence spectrometry

I. Csató, G. Záray, K. Gál-Solymos, J. Hassler

Research output: Contribution to journalArticle

11 Citations (Scopus)

Abstract

Three silicon carbide powders having different grain size distributions were analyzed by total reflection X-ray fluorescence (TXRF) spectrometry with the application of slurry sampling. For the elements investigated (Fe, Ti, V, Cu, Ni, and Ca) the line-to-background ratios show a maximum value at a surface concentration of 12.5 μm/mm2. For the realization of this surface concentration, a 25-μL aqueous slurry with a concentration of 1% (m/V) and pH of 10 was dropped onto the Hydrophobic quartz carrier plate. For quantification of the intensity data, gallium was added as an internal standard to the slurries. Under these experimental conditions, the analytical data of the fine-grained powders (80-90% of the powder particles were less than 1.5 μm) are in good agreement with concentrations determined in various laboratories by inductively coupled plasma atomic emission spectrometry (ICP-AES), ICP mass spectroscopy (MS), electrothermal vaporization- (ETV)-ICP-AES, slurry sampling graphite furnace atomic absorption spectroscopy (GF-AAS), and neutron activation methods. Powders with a mean grain size greater than 1.5 μm deviate much more from the refer-ence data. Calculated limits of detection (LODs) range from 2 to 25 μg/g. The precision expressed as relative standard deviation (RSD) varies between 4 and 14% for Fe, Ti, and V, whose concentrations in the fine-grained silicon carbide samples exceed by a minimum of tenfold their limits of detection; however the precision is very poor for Cu (66.6%) and Ni (62.3%), which have concentrations near the limits of the detection.

Original languageEnglish
Pages (from-to)1067-1072
Number of pages6
JournalApplied Spectroscopy
Volume51
Issue number7
Publication statusPublished - Jul 1997

Fingerprint

Silicon carbide
silicon carbides
Powders
fluorescence
Inductively coupled plasma
Spectrometry
spectroscopy
x rays
Sampling
Atomic spectroscopy
Gallium
Quartz
Graphite
Slurries
grain size
sampling
Absorption spectroscopy
Vaporization
Neutrons
slurries

Keywords

  • Silicon carbide
  • Total reflection x-ray fluorescence spectrometry

ASJC Scopus subject areas

  • Spectroscopy
  • Instrumentation

Cite this

Direct analysis of silicon carbide powder by total reflection X-ray fluorescence spectrometry. / Csató, I.; Záray, G.; Gál-Solymos, K.; Hassler, J.

In: Applied Spectroscopy, Vol. 51, No. 7, 07.1997, p. 1067-1072.

Research output: Contribution to journalArticle

Csató, I. ; Záray, G. ; Gál-Solymos, K. ; Hassler, J. / Direct analysis of silicon carbide powder by total reflection X-ray fluorescence spectrometry. In: Applied Spectroscopy. 1997 ; Vol. 51, No. 7. pp. 1067-1072.
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