Absorptiometry of Chromium in Steels Using On-Line Coprecipitation Enrichment

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  • Watanabe Kunihiro
    Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science
  • Akiyama Mariko
    Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science
  • Shitanda Isao
    Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science
  • Itagaki Masayuki
    Department of Pure and Applied Chemistry, Faculty of Science and Technology, Tokyo University of Science

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Other Title
  • オンライン共沈濃縮法を利用する鉄鋼中クロムの吸光光度定量
  • オンライン キョウチン ノウシュクホウ オ リヨウ スル テッコウ チュウ クロム ノ キュウコウ コウド テイリョウ

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An on-line coprecipitation concentrarion method has been proposed for the determination of chromium in steels based on the reaction of chromium with 1,5-diphenylcarbonohydrazide (DPC). In an analysis of trace elements in steels, a removed method of an iron matrix with 4-methyl-2-pentanone has been used mainly, but there is a trend to avoid the use of organic solvents, which has been a burden on environment in recent years. Therefore, the iron matrix removal method had been investigated without any environmental burden using Teflon filter tube. Iron ions were collected with a filter tube as Fe(OH)3 in the flow system. After Fe(OH)3 was removed, a sample solution with Cr(VI), which came through a Teflon filter tube, was merged with a La(III) solution. Chromium was coprecipitated at pH 9.0 with La(OH)3, which was collected with another filter tube. The precipitation was eluted with HCl (5 M), and the chromium(VI) in the eluate reacted with a DPC. The absorbance of the obtained Cr(III)-DPC complex was measured by spectrophotometry at 542 nm. The calibration curve with 10-minute concentration operation for chromium (sample flow rate = 1.4 mL/min) was linear over the range of 0 to 200 ppb. The limits of detection and determination for chromium in the sample solution were 1.1 and 3.4 ppb, respectively. The method with a 10-minute concentration operation improved sensitivity by 17 times compared to a method with no concentration. The proposed method was applied to the determination of standard steel samples. The results of the determinations were in good agreement with the certified values.

Journal

  • BUNSEKI KAGAKU

    BUNSEKI KAGAKU 58 (10), 873-879, 2009

    The Japan Society for Analytical Chemistry

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