Detection of trace silicon in high purity iron by molybdosilicic acid blue spectrophotometry following fluoride separation.

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  • フッ化物分離／モリブドケイ酸青吸光光度法による高純度鉄中の微量ケイ素の定量
  • フッカブツ ブンリ モリブドケイサン アオ キュウコウ コウドホウ ニ ヨル コ

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Abstract

A modified fluoride separation-molybdosilicic acid blue spectrophotometry using masking reagent of iron was applied to determine trace silicon in high purity iron samples. The analytical procedure used is as follows; decompose 1.0 g of sample with a solution of sulfuric acid 2 ml and nitric acid 0.5 ml. After cooling the solution, add phosphoric acid 5 ml as masking reagent and hydrofluoric acid (1 %) 0.5 ml and then sulfuric acid 20 ml, to yield volatile silicon tetrafluoride. Transfer the fluoride completely into a boric acid solution by purging it with nitrogen. Then, move the solution into a 25 ml flask, and add hydrocloric acid and ammonium molybdate to form molybdosilicate. After adding oxalic acid and Ascorbic acid, measure the light absorbance of the solution at 810 nm. By this method, ppm level silicon in commercial high purity irons (4N and 5N) and subppm level silicon in JSS standard high purity iron sample were successfully determined. Recovery (n=10) was 96% for 10μg of silicon and the detection limit givcn by 3σ of blank value was 0.06 ppm.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 42 (4), 219-222, 1993

    The Japan Society for Analytical Chemistry

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