アルシン-原子吸光法による排水および土じょう中の微量ヒ素の定量

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  • 中村 靖
    日本鉱業株式会社佐賀関製錬所技術部分析課
  • 永井 博
    日本鉱業株式会社佐賀関製錬所技術部分析課
  • 窪田 大四郎
    日本鉱業株式会社佐賀関製錬所技術部分析課
  • 姫野 俊治
    日本鉱業株式会社佐賀関製錬所技術部分析課

書誌事項

タイトル別名
  • Determination of arsenic in waste water and soils by atomic absorption spectrometry using the arsine generation method
  • アルシン-ゲンシ キュウコウホウ ニ ヨル ハイスイ オヨビ ドジョウナカ ノ ビリョウ ヒソ ノ テイリョウ

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説明

Arsenic was determined by atomic absorption spectrometry with a high sensitivity and presision by using the arsine generation method. A slightly modified and simplified D.C. Maning's apparatus was used and no special device was required.<BR>The sample solution (3 M HCl) was treated with potassium iodide solution, stannous chloride solution and zinc powder. The generated arsine was led to the burner by argon and atomized with H2-argon (entrained air) flame. The effects of the reductant, zinc powder, the concentration of hydrochloric acid and diverse ions were examined. The most effective reductant was stannous chloride solution combined with potassium iodide solution. The absorbance was constant when the volume of the stannous chloride solution (200 g/l) was between 2 ml and 5 ml and that of the potassium iodide solution (200 g/l) was between 1 ml and 5 ml. The profile of absorbance was satisfactorily sharp with the use of abqut 200 mesh zinc powder and absorbance was decreased when the powder of greater particle size was used. The absorbance was constant in the concentration range of hydrochloric acid between 2 M and 5 M. Ten milligrams of copper, iron, nickel and antimony ions 2 g of sodium chloride and 200 mg of nitric acid were tolerable. The recommended procedure for determination of arsenic in soils are as follows.<BR>Take 0.1 g of air-dried sample in a Griffine beaker and add 2 ml of perchloric acid, 2 ml of nitric acid, 5 ml of hydrochloric acid and 2 ml of sulfuric acid (1+1). Heat gently until the decomposition completes, then evaporate to dryness. After cooling, add 10 ml of hydrochloric acid and heat to dissolve the residue. Transfer the solution into a volumetric flask (200 ml). Adjust the volume to 200 ml with water and introduce 10 ml portion of the diluted solution into the generator. Add 10 ml of hydrochloric acid, 3 ml of sulfuric acid, 1 ml of potassium iodide solution (200 g/l) and 2 ml of stannous chloride solution (200 g/l), and let stand for 10 minutes. Add 1 g of zinc powder and immediately connect the generator to the atomic absorption spectrometer. Measure the absorbance of resonance line of arsenic at 193.7 nm.<BR>The standard deviations of this method were 0.0000.003 ppm at the level of 0.0040.083 ppm for waste water and 0.00010.0002% at the level of 0.00140.0036% for soils. Sensitivity was 0.02 μg (1% absorbance).

収録刊行物

  • 分析化学

    分析化学 22 (12), 1543-1548, 1973

    公益社団法人 日本分析化学会

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