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建立了一种以次氯酸钠作氧化剂,碱性加压氧化法溶解王水不溶渣中钌的方法。以酒精沉淀,盐酸溶解,硫脲分光光度法进行样品中钌含量的测定。方法对王水不溶渣中钌的溶解效果好,操作简单;王水不溶渣加压氧化浸出液共存的主要杂质离子 Na+、Cl-、Pb2+、Bi2+等(不含 Os)对吸光度无影响。采用硫脲分光光度法测定样品中13.771μg/mL钌,RSD (n=6)为1.536%,加标回收率为98.73%~102.76%。

Ruthenium in aqua regia-insoluble residue was dissolved by an alkaline pressure oxidation method with sodium hypochlorite as antioxidant in alkaline system, followed by content analysis of ruthenium using the thiourea-spectrophotometry. Ruthenium could be converted into the solution and the accompanying main impurity ions (such as Na+, Cl-, Pb2+, Bi2+) had no interference with the determination of ruthenium. The relative standard deviation (n=6) was 1.536%in the sample containing 13.771 μg/mL of ruthenium, and the recovery of the addition of standard ruthenium was 98.73%~102.76%.

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