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A Study of EPMA Analysis for Nitric Acid Insoluble Alloys
Analytical Science and Technology / Analytical Science and Technology, (P)1225-0163; (E)2288-8985
1998, v.11 no.6, pp.485-494
Park,
S., Park,
Y., Kim,
J., Son,
S., &
Joe,
K.
(1998). A Study of EPMA Analysis for Nitric Acid Insoluble Alloys. Analytical Science and Technology, 11(6), 485-494.
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Abstract
Ternary and quaternary alloys composed of Mo-Ru-Rh-Pd were prepared and their crystal structure and quantitative chemical compositions were analysed by XRD, WDX, EDX and ICP/AES. The results of X-ray diffraction studies showed that the alloys were crystallized in hexagonal close packing, well known as <TEX>${\varepsilon}$</TEX>-phase with <TEX>$P6_3/mmc$</TEX> of space group. The optimum accelerating voltage for Zr~Cd(40~48) analyzed by EPMA using PET crystal was found to be 15 kV and the linear regression coefficient(R) of atomic number and X-ray intensity was approximately 0.998 without Tc standard specimen. The WDX results of alloys of Mo and Pd by linear regression equations were detected to be 0.1% lower compared to WDX analysis results using standard specimen, while Ru, Rh were detected 3% higher. These alloys were completely dissolved in mixed acid of 12.5 mL HCl and 1 mL <TEX>$HNO_3$</TEX>, at <TEX>$220^{\circ}C$</TEX> for 22 hours using autoclave with PTFE vessel. There was no reprecipitating phenomnon when diluted 100 times with 1N-HCl. The results of ICP/AES analysis deviated less than 4% comparing with those of normal WDX analysis.
- keywords
- EPMA, ICP, insoluble alloys, interpolation
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