In this paper,a method was developed for the determination of arsenic and antimony in geological samples by hydride generation inductively coupled plasma mass spectrometry (HG-ICP-MS)with hydrochloric acid nitric acid mixed acid system (HCl ∶ HNO3 ∶ H2O=3 ∶ 1 ∶ 4)was extracted by water bath extraction.The influence of the concentration of reductant NaBH4 solution on the test result was discussed and the instrument parameters were optimized.The introduction of hydride generation technique for determination of arsenic antimony detection limits were 0.188,0.033g· g-1,accuracy (△ logC) was-0.022~0.006,-0.025~-0.001,precision(RSD%)was 3.99~9.07,5.97~8.53.The method was verified by national standard material,and the result is accurate and reliable.It can meet the requirement of determination of As and Sb in geological samples such as rock,soil,water system,sediment and so on.%本文建立了盐酸-硝酸混酸体系(HCl∶HNO3∶H2O=3∶1∶4)水浴浸提,氢化物发生-电感耦合等离子体质谱法(HG-ICP-MS)测定地质样品中砷锑的分析方法.探讨了还原剂NaBH4溶液的浓度对测试结果的影响,优化了仪器参数.引入氢化物发生技术用ICP-MS测定砷锑的检出限分别为0.188、0.033μg·g-1,准确度(△logC)分别为-0.022~0.006、-0.025-0.001,精密度(RSD%)分别为3.99~9.07、5.97~ 8.53.方法经国家一级标准物质验证,结果准确可靠,可以满足岩石、土壤、水系沉积物等地质样品中As、Sb的测定要求.
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