A Study of EPMA Analysis for Nitric Acid Insoluble Alloys

질산불용성 합금의 EPMA분석

  • Park, Soon-Dal (Department of Nuclear Chemistry, Korea Atomic Energy Research Institute) ;
  • Park, Yong-Joon (Department of Nuclear Chemistry, Korea Atomic Energy Research Institute) ;
  • Kim, Jong-Goo (Department of Nuclear Chemistry, Korea Atomic Energy Research Institute) ;
  • Son, Se-Chul (Department of Nuclear Chemistry, Korea Atomic Energy Research Institute) ;
  • Joe, Kih-Soo (Department of Nuclear Chemistry, Korea Atomic Energy Research Institute)
  • 박순달 (한국원자력연구소 원자력화학연구팀) ;
  • 박용준 (한국원자력연구소 원자력화학연구팀) ;
  • 김종구 (한국원자력연구소 원자력화학연구팀) ;
  • 손세철 (한국원자력연구소 원자력화학연구팀) ;
  • 조기수 (한국원자력연구소 원자력화학연구팀)
  • Received : 1998.06.23
  • Published : 1998.12.25

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 ${\varepsilon}$-phase with $P6_3/mmc$ 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 $HNO_3$, at $220^{\circ}C$ 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.