水酸化ベリリウム共沈／アルシン分離／モリブドヒ酸青吸光光度法による高純度鉄中微量ヒ素の定量

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タイトル別名
  • Determination of arsenic in high purity iron by hydride generation/reduced molybdoarsenate spectrophotometry after separation by beryllium hydroxide coprecipitation.
  • スイサンカ ベリリウム キョウチン アルシン ブンリ モリブドヒサン アオキュ

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A new analytical technique of micro amounts of As in high purity iron was developed. Arsenic was separated by coprecipitation with beryllium hydroxide as a BeNH4AsO4 from iron. Arsenic in the precipitate was digested using hydrochloric acid and reduced to AsH3 with dropwise addition of 5ml of 25g/l NaBH4 solution. This reduction technique was simple and rapid (1012 min) as compared with reduction with metallic zinc, because pre-reduction of As(V) to As(III), temperature control of the sample solution for hydride generation and long reduction time (1h) were unnecessary. On the Ag-DDTC spectrophotometry, AsH3 was absorbed into a pyridine or brucine-chloroform solution containing Ag-DDTC, but those solvents had a disagreeable odour or toxicity respectively. In this technique, AsH3 was absorbed into KMnO4 solution containing ammonium molybdate and small amounts of polyvinyl alcohol and then determined by reduced molybdoarsenate spectrophotometry. By this method, the absorption solution is harmless as compared with the Ag-DDTC method. Moreover, a molar absorptivity for the reduced molybdoarsenate spectrophotometry (ε=27000) is larger than it forAg-DDTC method (ε=15000). Therefore, this technique was more practical and could be conveniently applied to the determination of micro amounts of As. The relative standard deviation of this method was approximately 13% for the determinations (n=9, x=0.96μg/g) of 1.0μg/g As in a synthetic sample and the detection limit was 0.3μg/g as for a 1.0g of sample.

収録刊行物

  • 分析化学

    分析化学 40 (6), 263-269, 1991

    公益社団法人 日本分析化学会

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