誘導結合プラズマ発光分析用のニオブ及びタンタル標準溶液の調製

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タイトル別名
  • Preparation of standard solutions of niobium and tantalum for inductively coupled plasma atomic emission spectrometry.
  • ユウドウ ケツゴウ プラズマ ハッコウ ブンセキヨウ ノ ニオブ オヨビ タン

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This report describes preparation of niobium and tantalum standard solutions for ICP atomic emission spectrometry. A mixture of 2 ml nitric acid (1+1), 1 ml hydrofluoric acid (1+1) and 4 ml sulfuric acid (1+1) was used to dissolve 200 mg of niobium or tantalum metal powder, and the solution obtained was evaporated till sulfuric acid began fuming. The resulting syrupy residue was dissolved in a solution containing a necessary amount of complexing reagent, filtered if precipitate appeared and finally made up to 200 ml. As complexing reagents, ammonium ox alate, tartaric acid, hydrofluoric acid, hydrogen peroxide and sulfuric acid were tested to evaluate their stabilizing effects on niobium and tantalum solutions. As a result, following reagents and concentrations were recommended for preparation of 1 mg ml-1 stock solution of each element: For niobium, 0.1 M ammonium oxalate, 0.6 M tartaric acid or 2% hydrogen peroxide plus 0.5 M sulfuric acid; for tantalum, 0.1 M ammonium oxalate, 1.2 M tartaric acid or 0.025 M hydrofluoric acid. The stock solutions thus prepared could be preserved more than one year without precipitation, though the concentrations of the complexing reagents were much lower as compared with those of conventional standard solutions used for colorimetry. Working standard solutions prepared by diluting the stock solutions ten-fold with water were stable as well. The complexing reagents had negligible interferences on the emission intensities of niobium and tantalum.

収録刊行物

  • 分析化学

    分析化学 34 (12), 791-795, 1985

    公益社団法人 日本分析化学会

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