In the accurate elemental analysis of ceramic powders by X-ray fluorescence spectrometry with few or no available standards, the glass bead technique combined with the fundamental parameter (FP) method has been found to be suitable. As an example of ceramic powder analysis, we determined the amounts of Y
2O
3, BaO, and CuO contained in a superconductor YBa
2Cu
3O
7-δ with this combined method.
The results were as follows:
(1) Satisfactory glass beads with near-infinite thickness to both incident and fluorescent X-rays were found to be prepared from 10 g of Na
2B
4O
7, 1 g of YBa
2Cu
3O
7-δ, and 0.20 g of KI.
(2) Absorption enhancement effects for YKα, BaKα, and CuKα as below were taken into account in the analysis. YKα is more absorbed by substituting Y
2O
3 in the mixed reagents (Y
2O
3-BaO-CuO) with either BaO or CuO. BaKα is enhanced or a little more absorbed depending on the substitution of BaO in the mixed reagents with CuO or Y
2O
3. CuKα is more absorbed or a little enhanced depending on the substitution of CuO in the mixed reagents with BaO or Y
2O
3.
(3) The amounts of Y
2O
3, BaO, and CuO in the superconductor were determined with the good accuracies (σ
d's) of 0.11, 0.18, and 0.19wt%, respectively by this combined method.
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