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研究了将难溶氧化铂通过水合肼还原成海绵铂,用王水溶解海绵铂,采用氯化铵沉淀法测定铂,从而建立了难溶氧化铂中铂含量的测定方法。对还原剂的选择、还原温度、还原酸度、还原后沉淀过滤洗涤方式及共存元素的干扰等条件进行了一系列实验,解决了难溶氧化铂中铂测定的难题。该方法易于操作,准确度高。将该方法应用于5个不同品位难溶氧化铂样品中铂的测定,相对标准偏差(RSD)为0.10%~0.30%(n=9)。采用该方法测定基准物质氧化铂(PtO2· H2O)中的铂含量,测定值和标准值相符合,从而证明该方法的可行性和可靠性。

A determination method of platinum content in indissolvable platinum oxide is by making platinum ox -ide reduced by hydrazine into platinum sponge which is afterwards dissolved with aqua regia and precipitated by plati -num using ammonium chloride .This paper discussed a series of parameters such as the selection of reducing agent ,re-duction temperature ,reduction acidity ,washing method of the reduction sedimentation and the interference of coexis-ting elements.This method solved the problems of determination of platinum in indissolvable platinum oxide .It was easy to operate with high accuracy .Applied to five indissolvable platinum oxide samples , relative standard deviation (RSD) was in 0.10%-0.30%(n=9).For the benchmark substance of platinum oxide (PtO2· H2O),the meas-ured values and standards were in line ,which proved the feasibility and reliability of the method .

参考文献

[1] GB/T 19720-2005.铂合金首饰铂、钯含量的测定氯铂酸铵重量法和丁二酮肟重量法[S].北京:中国标准出版社,2005.
[2] 北京矿冶研究总院分析室.矿石及有色金属分析手册[M].北京:冶金工业出版社,1990:184-202.
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