無機薄層クロマトグラフィーの研究(第14報)金属ジチゾネートの薄層からの溶出比色定量

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Quantitative analysis of metal dithizonates was carried out by extraction with chloroform, thin-layer chromatography, elution with chloroform, and colorimetry. The metal ions Hg^<2+>, Cu^<2+>, Pd^<2+> and Bi^<3+> were extracted from the sample solution (200 ml) with 0.1% dithizone-chloroform solution (5 ml) at pH 1.8-2.0,and Ni^<2+>, Co^<2+>, Zn^<2+>, and Pb^<2+> at pH 7.0-8.0. The extracted dithizonates of Bi^<3+>, Pb^<2+> and Zn^<2+> were unstable compared to other metal dithizonates. The extract solution (100 μl) was applied on MN-silica gel S-HR layer by chromatocharger. The layer was developed with benzene or a solution of carbon tetrachloride-methylene chloride-benzene (1 : 7 : 4). After the thin-layer chromatographic separation, zones of each dithizonate were scraped off from the thin-layer plate by a vacuum extractor and eluted from the adsorbent with chloroform (4 ml). The eluate was made up to 5 ml with chloroform and amount of metals determined by colorimetry. The determination ranges of metal ions obtained by this method were as follows : Cu^<2+> and Ni^<2+>, 0.125-1.0 ppm ; Pd^<2+>, 0.125-2.125 ppm ; Zn^<2+>, 0.125-0.625 ppm ; Co^<2+>, 0.125-1.0 ppm ; Hg^<2+>, 0.25-2.5 ppm ; Bi^<3+>, 0.5-2.5 ppm, and Pb^<2+>, 0.5-3.0 ppm. The coefficient of variation of these determined metal values was about 4%.
公益社団法人日本薬学会の論文
1975-02-28