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

概要

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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 100μl of cyclohexane phase was injected into the HPLC with fluorometric detection. Cyclohexane-tetrahydrofuran (90:10v/v) mixture was used as an eluent and effluent was monitored at 380nm and 530nm as excitation and emission wavelength, respectively. A linear calibration was observed in the selenium concentration range from zero to 6.0ng/ml. The detection limit (3σ) of Se(IV) was 0.12ng/ml, which corresponded to 0.12ppm 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.
社団法人日本分析化学会の論文
2005-10-05