Abstract

An ion chromatographic technique for the measurement of the concentrations of metal-oxygen cluster anions and the determination of their elemental compositions has been developed. The method depends on the decomposition of the heteropoly anions into their simpler constituent ions by the addition of a basic hydroxide and the subsequent separation and analyses of these constituent ions. Although the susceptibility of the metal-oxygen cluster anions to decomposition in basic solutions is well known and ion chromatography has been supplied to the analysis of tungstate, molybdate and phosphate ions the application of the former observation and the latter method in combination for the analyses of metal-oxygen cluster anions has not been reported previously. The analytical method described here thus constitutes the first reported application of ion chromatography for the determination of concentration and elemental composition of metal-oxygen cluster anions. The method additionally offers the possibility of application in the study of the mechanism of the synthesis and decomposition of the metal-oxygen cluster anions.

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