海水，河川水中のセレン（ＩＶ），セレン（ＶＩ）のけい光定量

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タイトル別名
  • Fluorometric determination of selenium (IV) and selenium (VI) in sea water and river water
  • カイスイ カセンスイチュウ ノ セレン 4 セレン 6 ノ ケイコウ テイリョ

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A simple and convenient chemical separation procedure for determination of Se(IV) and Se(VI) by spectrofluorometric analysis is proposed and appliled to the study of the valence state of Se (IV) and Se (VI) in sea water and river water. Immediately after the collection of water samples, (23) 1 of sample water was filtered through a 3μ and a 0.3 μpore-size Membrane filter successively. Thirty milligrams of Fe(III) as FeCl3 was added to the sample water with continuously stirred and pH of the solution was maintained to 5. After being allowed to stand for (23) hrs., the precipitate was filtered. By this time, Se(IV) was coprecipitated with Fe(OH)3, and Se (VI) was remained in filtrate completely. The precipitate was dissolved in (12) ml of concentrated hydrochloric acid and diluted to 25 ml with water. To remove Fe (III), an aliquot of the solution was taken, 3 ml of 1 M acetic acid was added to the solution, and pH of the solution was adjusted to 5 by adding saturated sodium acetate solution. The solution was extracted with 10 ml of 1 M capric acid-CHCl3 solution. The aqueous layer was washed with CHCl3, and Se (IV) was measured by 2, 3-diaminonaphthalene (DAN) fluorometric method [This Journal, 22, 712 (1973)]. Selenium(VI) in the filtrate was concentrated by tellurium coprecipitation method. The filtrate was acidified to 1 M HCl, and (1020) mg of Te(IV) solution, (100300)g of hydrazine sulfate were added to this solution and boiled for 30 minutes at (80100)°C. The ash-colored metallic tellurium was dissolved with nitric acid and (0.52) ml of perchloric acid, and evaporated to dryness.The residue was dissolved with 5 ml of 6 N HCl and boiled for 3 minutes and diluted to 25 ml with water. An aliquot of this solution was taken, and selenium was measured by DAN fluorometric method. In this procedure, the recovery of Se (IV) and Se (VI) were about up to 95%. Coastal seawater of Japan and river water has been found to contain (0.010.05)μg Se(IV)/l and (0.030.28)μg Se(VI)/l. The method of determination of particle size distribution of selenium in suspended matter was also proposed.

収録刊行物

  • 分析化学

    分析化学 26 (2), 91-96, 1977

    公益社団法人 日本分析化学会

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