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. Cyclohexanetetrahydrofuran (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.
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