During the analysis of geochemical sample's, arsenic and stibium are usually detected by atomic fluorescence spectrometry with aqua regia dissolving samples, but the values of national standard samples obtained by this traditional method are generally lower than the certified values.A determination method of arsenic and stibium in geochemical samples by atomic fluorescence spectrometry has been developed.The samples are dissolved with a mixed acid of HF-HNO3-H2SO4.The method has been applied to determination of arsenic and stibium of national standard samples of stream sediment, soil, and rocks.The results, in comparison with traditional method with aqua regia dissolving samples, are better in agreement with certified values.%在地球化学样品分析中,采用传统的王水分解样品—原子荧光法测得的国家标准物质的砷、锑结果往往比标准值低,因此建立了一种采用HF-HNO3-H2SO4混合酸分解样品—原子荧光仪测定地球化学样品中砷、锑的方法.经水系沉积物、土壤和岩石等国家一级标准物质验证,并与传统的王水分解样品—原子荧光法测定结果相比较,发现该方法测定结果与标准值符合得更好,更接近被测元素的全量.
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