２，３‐ジアミノナフタレンを用いる蛍光検出高速液体クロマトグラフィーによる鉄鋼中の微量セレンの定量

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書誌事項

タイトル別名
  • Fluorometric Determination of Trace Amounts of Selenium in Steel by High-Performance Liquid Chromatography with 2,3-Diaminonaphthalene
  • 2,3-ジアミノナフタレンを用いる蛍光検出高速液体クロマトグラフィーによる鉄鋼中の微量セレンの定量
  • 2 3 ジアミノナフタレン オ モチイル ケイコウ ケンシュツ コウソク エキタイ クロマトグラフィー ニ ヨル テッコウ チュウ ノ ビリョウ セレン ノ テイリョウ

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説明

A novel method for the determination of trace amounts of selenium in iron and steel has been demonstrated by a HPLC using 2,3-diaminonaphthalene (DAN) as a derivatizing reagent. Certified reference materials of iron and steel were used to prepare digestive samples by decomposition with hydrochloric acid and nitric acid followed by phosphoric acid huming. Selenium(IV) in the digestive samples was extracted with DAN into cyclohexane. The 100 μl of cyclohexane phase was injected into the HPLC with fluorometric detection. Cyclohexane - tetrahydrofuran (90 : 10 v/v) mixture was used as an eluent and effluent was monitored at 380 nm and 530 nm as excitation and emission wavelength, respectively. A linear calibration was observed in the selenium concentration range from zero to 6.0 ng/ml. The detection limit (3σ) of Se(IV) was 0.12 ng/ml, which corresponded to 0.12 ppm in iron and steel samples. The good agreement between determined values with both the proposed method and GD-MS indicates that the proposed method is of great promise for the determination of selenium present in iron and steel.<br>

収録刊行物

  • 分析化学

    分析化学 54 (10), 959-963, 2005

    公益社団法人 日本分析化学会

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