逆相分配高速液体クロマトグラフィーによる金属-ジアセチルビス(4-フェニル-3-チオセミカルバゾン)錯体の相互分離

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The complex formation of zinc(II), cadmium(II), lead(II), nickel(II), copper(II) and mercury(II) with diacetyl bis(4-phenyl-3-thiosemicarbazone) (DBS) was studied in 80 v/v% N,N-dimethylformamide-water mixture, and reversed phase partition chromatography with a spectrophotometric detection was applied to the separation of metal-DBS complexes by using a ODS column (6mm i. d.×250 mm in length). The elution peaks of Cd-DBS and Pb-DBS, and of Ni-DBS and Cu-DBS on their chromatogram were not separated successfully by using a methanol-water and a acetonitrile-water as mobile phases. The resolved separation of Zn, Cd, Pb, Ni, Cu and Hg-DBS was achieved by using a 67.5 v/v% acetone-water mobile phase containing 0.01 mol dm^<-3> sodium acetate (apparent pH 8.8). The calibration curves of the peak area for Cd-DBS and the peak hights for others were linear in concentration ranges of (0.2〜2.0)×10^<-5> mol dm^<-3> for Zn and (0.4〜4.0)×10^<-5> mol dm^<-3> for others (0.04 absorbance unit full-scale at 425 nm, injected volume 25 mm^3). All the relative standard deviation (sample size concentration of 1.0×10^<-5> mol dm^<-3> for Zn and 2.0×10^<-5> mol dm^<-3> for others, n=5) was better than 1.9%.
社団法人日本分析化学会の論文
1986-09-05