同位体希釈‐表面電離質量分析法によるカドミウムの定量

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  • Determination of Cadmium by Isotope Dilution-Surface Emission Mass Spectrometry

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A minute amount of cadmium can be determined by the isotope dilution method with surface emission mass spectrometry using 116Cd as a spike. After extracted into 15 ml of 0.00125% dithizone chloroform solution from the sample spiked with 116Cd, cadmium is back extracted into 5 ml of 7 N nitric acid. The nitric acid solution is treated with 0.1 ml of 60% perchloric acid and dried up in a heated pyrex glass oven supplied with a high purity nitrogen gas. The residue is dissolved in a mixture of 60 μl of 0.003% silica gel suspended water and 5 μl of 2% phosphoric acid. An aliquot of the dissolved solution is loaded onto the center of a rhenium single filament in a surface ionization device of the mass spectrometer. The present method can determine the ratio of 114Cd/116Cd with the precision from 0.4 to 1.1% in coefficient of variation, where the detection limit for Cd+ ion is 10-14∼10-18 g. The application of the present method to orchard leaves delivered by National Bureau of Standards, U. S. A., as a standard reference material in environments has proved its superior usefulness by giving results in close agreement with those certified by N. B. S.

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