エチレンジアミン四酢酸を用いるプレカラム誘導体化/逆相分配高速液体クロマトグラフィーによる鉄鋼中の微量ビスマスの定量(<特集>分析技術と方法論の最近の進歩)

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Determination of trace amounts of bismuth in steel and iron was demonstrated with high performance liquid chromatography using ethylene-diaminetetraacetate (EDTA) as a pre-column derivatizing reagent. Standard materials of steel and iron were decomposed with a mixture of nitric acid and hydrochloric acid, followed by subjected to sulfuric fuming. The residues were dissolved with 0.1 mol dm^<-3> hydrochloric acid to prepare digested sample solutions. Bismuth ions in the digested solution were separated from iron matrix with an anion exchange column under 0.1 mol dm^<-3> hydrochloric acid. The adsorbed bismuth ions on the anion exchange column could be recovered with 0.1 mol dm^<-3> nitric acid, quantitatively. After the recovered bismuth ions were derivatized with EDTA under pH 3.0, HPLC separation of the bismuth-EDTA complex was performed with an ODS column using an aqueous solution containing 0.01 mol dm^<-3> monochloroacetate buffer (pH 3.0) and 2.0×10^<-3> mol kg^<-1> of tetrabutylammonium bromide was monitored at 265nm spectrophotometrically. A linear calibration was observed in the concentration range from 1×10^<-8> to 1×10^<-6> mol dm^<-3> of bismuth. The detection limit (3σ) of Bismuth was 8.8×10^<-8> mol dm^<-3>, which corresponded to 0.92 ppm in iron and steel samples. An analytical recovery of a steel sample obtained with the HPLC method agreed with that obtained with GD-MS. The recoveries of bismuth added to the digested solution of iron and steel were with in 99.5 to 118%, indicating potential of the HPLC method for iron and steel analyses.
社団法人日本鉄鋼協会の論文
2007-02-01

エチレンジアミン四酢酸を用いるプレカラム誘導体化/逆相分配高速液体クロマトグラフィーによる鉄鋼中の微量ビスマスの定量(<特集>分析技術と方法論の最近の進歩)

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