Depth Profile Analysis of Precipitates and Inclusions Existing in the Surface of the Steel by Inductively Coupled Plasma Mass Spectrometry with Microwave Decomposition

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  • INOSE Masao
    Analysis & Characterization Research Dept., Steel Research Laboratory, JFE Steel Corporation
  • FUJIMOTO Kyoko
    Analysis & Characterization Research Dept., Steel Research Laboratory, JFE Steel Corporation
  • KINOSHIRO Satoshi
    Analysis & Characterization Research Dept., Steel Research Laboratory, JFE Steel Corporation
  • CHINO Atsushi
    Analysis & Characterization Research Dept., Steel Research Laboratory, JFE Steel Corporation

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Other Title
  • マイクロ波加圧分解／誘導結合プラズマ質量分析法による鋼材表層析出物及び介在物の深さ方向分析
  • マイクロハ カアツ ブンカイ ユウドウ ケツゴウ プラズマ シツリョウ ブンセキホウ ニ ヨル コウザイ ヒョウソウ セキシュツブツ オヨビ カイザイブツ ノ フカサ ホウコウ ブンセキ

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Description

An analytical method of precipitates/inclusions existing a few μm from the surface in steel sheets has been established. Less than 0.1 g of a steel surface was electrolyzed, and the extracted precipitates/inclusions were decomposed with 2-step microwave digestion (1st step with H2SO4 and 2nd step with HF-HNO3). Al, Ti, Mn, Cu, Nb, V and Mo in the sample solution was determined by ICP-MS. The lower limits of detection in the surface of the steel sample were less than 1 μg g-1 for all elements that formed precipitates/inclusions. Furthermore, the concentration of the chelating agent (acetylacetone) in the electrolyte was reduced to 0.2%, which enabled us to quantitatively extract precipitates/inclusions that were unstable in the conventional 10% AA electrolyte. The procedure was applied to steel samples before and after annealing, and depth profiles of the precipitates/inclusions were obtained.<br>

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 56 (2), 93-98, 2007

    The Japan Society for Analytical Chemistry

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