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。
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% HC104. Under the given experiment conditions, the instrumental limit of detection was 0. 001 and 0. 000 1 ng·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. 30μg·g^-1 ) and JP-1(peridotite; 0. 045μg·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.