マイクロスケール陽極溶解／ストリッピングボルタンメトリーによる高純度タンタル線中の銅の定量

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タイトル別名
  • Determination of copper in high-purity tantalum wire by microscale stripping voltammetry after anodic dissolution of the sample.
  • マイクロ スケール ヨウキョク ヨウカイ ストリッピング ボルタンメトリー ニ

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About 36mg of Ta is anodically dissolved from the surface of a helical wire sample (0.5 mm diam. × 200 mm) in 200μl of 5 M hydrofluoric acid-1M nitric acid-1.75 × 10-4 M Hg (II) electrolyte by constant current electrolysis at a current density of about 8 mA/cm2 for 510 min using a glassy carbon cathode. After replacement of the sample by a Pt anode, greater than 95% of Cu in the electrolyte is electro-deposited together with Hg on the glassy carbon cathode at -0.7Vvs. SCE within 10 min for differential pulse anodic stripping voltammetry. Fractional μg/g of Cu in high-purity Ta wire is determined, with a relative standard deviation of about 5%, by the proposed method within an hour. In the stripping voltammetric determination of trace impurities in high-purity solid materials, use of microliter electrolytes is more favorable than conventional techniques using milliliter electrolytes from the viewpoints of sensitivity, precision and rapidity, provided that appropriate apparatus are devised to overcome operational difficulties due to miniaturization. Another advantage of microscale techniques is minimization of high-purity reagents consumption and experimental wastes.

収録刊行物

  • 分析化学

    分析化学 37 (3), 128-132, 1988

    公益社団法人 日本分析化学会

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