Separation of metal-diacetyl bis(4-phenyl-3-thiosemicarbazone) complexes by reversed phase partition HPLC.

HOSHI Suwaru, TAKAHASHI Norimitsu, INOUE Sadanobu, MATSUBARA Mutsuya

doi:10.2116/bunsekikagaku.35.9_819

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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
ギャクソウブンパイコウソクエキタイクロマトグラフィーニヨルキンゾ
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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Abstract

The complex formation of zinc(II), cadmium(II), lead(II), copper(II) and mercury(II) with diacetyl bis(4-phenyl-3-thiosemicarbazone) (DBS) was studied in 80v/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.×250mm 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 67.5v/v% acetone-water mobile phase containing 0.01mol 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 (0.22.0)×10^-5 mol dm^-3 for Zn and (0.44.0)×10^-5mol dm^-3 for others (0.04 absorbance unit full-scale at 425nm, injected volume 25mm³). All the relative standard deviation (sample size concentration of 1.0×10^-5mol dm^-3 for Zn and 2.0×10^-5mol dm^-3 for others, n=5) was better than 1.9%.

Journal

BUNSEKI KAGAKU

BUNSEKI KAGAKU 35 (9), 819-822, 1986

The Japan Society for Analytical Chemistry

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