ジメチルグリオキサールビス(4-フェニル-3-チオセミカルバゾン)担持樹脂による濃縮と吸光検出逆相高速液体クロマトグラフィーとの組み合わせによる微量水銀の定量

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Amberlite XAD-7 resin coated with dimethylglyoxal bis(4-phenyl-3-thiosemicarbazone)(DMBS) was prepared, and applied to the preconcentration of trace Hg (II) from aqueous solution. Hg (II) was quantitatively collected with the resin coated with the reagent (DMBS-XAD7) from acidic solution by the batch method. After collection, Hg (II) was eluted easily as its DMBS chelate with a small volume of N, N-dimethylformamide(DMF). This collection and elution method was applied to the determination of trace Hg (II). The recommended procedure is follows : to 100ml of solution containing up to 1μg of Hg (II) adjusted pH2 with 5M nitric acid in a 150ml screw-capped glass bottle, add 0.1g of DMBS-XAD7 and shake for 15min. Filter the solution with a polyethylene column (i.d. 9mm×65mm height), and then elute Hg (II)-DMBS chelate from the resin with 1 ml of DMF, and inject 5μl of the DMF solution to HPLC with spectrophotometric detection by using an ODS column (i.d. 6mm×250mm in length) and 80(v/v)% acetone-water mixed solution as a mobile phase. The calibration curves of peak height was linear in the concentration range of 0.1〜1μg for Hg (II)(0.0025 absorbance unit full-scale at 415 nm). The relative standard deviation (sample size concentration of 0.5μg and 5 determinations) was 2.2%. The proposed method was applied succesfully to the determination of mercury in hair (NIES standard sample) and other.
社団法人日本分析化学会の論文
1994-08-05