マイクログラム量のアンチモンの分析化学的研究-3-

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Paperchromatographic spots of antimony split into three or four bands according to the treatment of the sample and the oxidation state of the developer. A main peak of the chromatogram has been found to appear at the acid front if the spotted sample of trivalent antimony chloride or of pentavalent chloroantimonic acid in concentrated hydrochloric acid medium is treated with a developer such as butanol containing hydrochloric acid together with hydrogen peroxide or nitrite as an oxidizing agent. On the other hand, a sample previously oxidized in slightly acid solution or a sample of irradiated unit of 124SbCl3 solution (presumably oxidized into the pentavalent state by prolonged irradiation with β and γ rays) has shown a main spot at the start and partly tracing bands in succession up to the acid front. The tracing bands in some cases showed maxima, the Rf value of each of which was dependent on the period of migration, and might be properly named "kinetic bands" formed by the reaction of hydrolysed products of pentavalent chloroantimonic acid with conc. hydrochloric acid in the mobile phase. Experiments also showed that a sample of antimony (V) chloride in the conc. hydrochloric medium or trivalent antimony chloride produced a quite similar sharp peak at the acid front. Therefore, by the use of n-butanol containing conc. hydrochloric acid as a developer, the Rf values of 0.80-0.72 for Sb (V) and of 0.69-0.76 for Sb (III) can not be distinguished. The typical pentavalent chloroantimonic acid chromatograms are composed of four spots : namely, first, a hydrolysed product of chloroantimonic acid at the start; second, a diffused band of a reaction product at the intermediate zone; third, a sharp chloroantimonic acid peak at the acid front; and fourth, a faint extracted chloroantimonic acid at the developer zone.
社団法人日本分析化学会の論文

マイクログラム量のアンチモンの分析化学的研究-3-

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