密闭高温高压溶样ICP-MS测定24个国际地质标样中的Sb和Bi

研究了ICP-MS分析中Bi，Sb，Te和As产生的记忆效应，其记忆效应Bi>Sb>Te>As。在低浓度硝酸介质中(0.01%～1%)，贮存样品的聚丙烯瓶和ICP-MS的进样管道会对Bi元素产生严重的吸附作用。0.1%氢氟酸的清洗效果优于6%的硝酸，而6%的硝酸的清洗效果要优于0.1%高氯酸。在给定的仪器操作条件下，Sb和Bi的检出限分别为0.001和0.000 1 ng·mL-1。采用该清洗方法，结合密闭高温高压溶样，测定了24个国际地质标样中的Bi和Sb。大部分标样的测定结果与已有参考值吻合较好。文章还给出了国际标样AGV-2(安山岩)、BHVO-2(玄武岩)和BCR-2(玄武岩)中Bi和Sb的测定值。

Determination of Sb and Bi in 24 International Geological Reference Materials by Using Pressurized Acid Digestion-ICP-MS

The authors studied in detail the memory effect of Bi, Sb, As and Te in ICP-MS. The produced memory effects of these element were in the order of Bi>Sb>Te>As. Bi was seriously adsorbed by the polypropylene sample storing bottle and the sample introduction system in the low nitric acid medium (0.01%-1% HNO3). The washout effect of 0.1% HF was found to be better than those of 6% HNO3 and 0.1% HClO4. Under the given experiment conditions, the instrumental limit of detection was 0.001 and 0.0001 ng x mL(-1) for Sb and Bi, respectively. The authors report the determination of Sb and Bi in 24 international geological reference materials by using pressurized acid digestion-ICP-MS (including AGV-2, BHVO-2, BCR-2, etc.). Most of the results were found to be in reasonable agreement with the reported values in the literature. The authors' determined values of Sb for GSR-1 (granite; 0.30 microg x g(-1)) and JP-1 (peridotite; 0.045 microg x g(-1)) are obviously higher than those reported values. This is attributed to the efficient pressurized acid digestion, which is generally much more efficient than conventional wet digestions for insoluble minerals.