キシレノールオレンジによる地質試料中の微量ジルコニウムの吸光光度定量

概要

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A rapid and accurate method for the determination of Zr in geological materials is presented. The interference of F^- was reduced by masking with Al^<3+>, and Fe^<3+> was reduced to Fe^<2+> with hydrazinium dichloride. A sample (0.2 g) was decomposed with a mixture of HNO_3, HClO_4 and HF, and the solution was evaporated to dryness. Then the dried sample was fused with a mixture of 2 g Na_2CO_3 and 0.3 g H_3BO_3, and the melt was dissolved in 17 ml of HCl (1 + 1), and it was diluted to 50 ml with water. Fifteen ml portion of the sample solution was transferred to a 50 ml volumetric flask. To it, 8 ml of Al chloride solution (Al^<3+> 25 mg/ml) and 5 ml of hydrazinium dichloride solution (15 w/v%) was added. The solution was heated in boiling water for 15 min. After cooling, 5ml of Xylenol Orange solution (0.1 w/v%) was added and diluted up to the mark with water. Absorbance was measured at 535 nm. Ten samples could be analyzed in 5 h. This method was satisfactorily applied to a variety of geological reference materials.
社団法人日本分析化学会の論文
1988-12-05