Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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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
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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 ${\varepsilon}$-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.

질산불용성합금의 특성을 갖는 Mo-Ru-Rh-Pd 합금을 만들어 XRD, WDX, EDX, ICP 분석을 하였다. XRD 분석결과 이 합금은 육방밀집(hcp) 구조와 $P6_3/mmc$의 공간군을 갖는 것으로 나타났다. EPMA 분석시 최적 가속전압은 15 kV였으며 Tc을 제외한 Zr~Cd 표준시편의 원자번호와 X-선 세기간의 직선성을 나타내는 R값은 0.998 범위였다. 내삽법에 의한 WDX 분석과 표준시편을 사용한 WDX 분석에서 구한 X-선 계수비를 비교한 결과 Mo, Pd은 표준시편을 사용한 WDX분석에 비해 0.1% 낮게 검출되었고 Ru, Rh은 약 3% 높게 검출되었다. 이 합금은 염산 12.5대 질산 1의 혼합산으로 $220^{\circ}C$, 22시간 용해시켰을 때 완전히 녹았으며 1N-HCl로 100배 희석시 재침전이 없었다. ICP 분석결과는 표준시편을 사용한 WDX분석에 대해 4% 이하의 편차를 보였다.

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