无助熔剂熔融制样LA-ICP-MS法测定铀矿勘查岩石样品中的难溶微量元素  

Determination of Refractory Trace Elements of Samples in Uranium Exploration Using LA-ICP-MS With Flux-free Fusion Preparation

作　　者：李黎 郭冬发[1] 刘瑞萍[1] 李伯平[1] 崔建勇[1] 谢胜凯[1] 张良圣[1] 王娅楠 LI Li;GUO Dongfa;LIU Ruiping;LI Boping;CUI Jianyong;XIE Shengkai;ZHANG Liangsheng;WANG Yanan(Beijing Research Institute of Uranium Geology,Beijing 100029,China)

机构地区：[1]核工业北京地质研究院,北京100029

出　　处：《铀矿地质》2021年第6期1131-1140,共10页Uranium Geology

基　　金：核能开发项目(编号:测HDJS2102);地勘项目(编号:测D1907)联合资助。

摘　　要：采用湿法分解溶液进样ICP-MS法对铀矿勘查样品中的难溶微量元素进行分析时,高场强元素Nb、Ta、Zr、Hf等在酸性条件下易水解,稀土元素(REEs)不能完全消解。针对上述问题,文章采用无助熔剂熔融法制备样品,结合固体进样激光剥蚀电感耦合等离子体技术(LA-ICP-MS)测定标准样品(GSR-3、BHVO-2、BCR-2)和铀矿勘查样品中的Nb、Ta、Zr、Hf、REEs、U、Th等元素含量。LA-ICP-MS结果表明,在1450℃、10 min的条件下获得的熔融玻璃除了含量低的微量元素Tm、Lu外,大部分元素相对标准偏差(RSD)与相对误差(RE)均小于10%。在实际铀矿勘查样品分析中,将该法的测试结果与溶液进样ICP-MS方法进行对比,两种方法的相对偏差基本在18%以内。由此得出结论,无助熔剂熔融制样LA-ICP-MS方法避免了繁琐的湿化学消解流程,适用于分析铀矿勘查样品中的难溶高场强元素、REEs、U、Th等元素。When ICP-MS is used to analyze the refractory trace elements in samples of uranium exploration,the high field strength elements such as Nb,Ta,Zr,Hf are hydrolyzed under acid digestion,while the rare earth elements(REEs)are partially dissolved.To solve this problem,standard sample fused glasses(GSR 3,BHVO-2,BCR-2)and uranium exploration samples were prepared by means of flux free fusion,the laser ablation inductively coupled plasma technique(LA-ICP-MS)was used to analyze Nb,Ta,Zr,Hf,REEs,U,Th and other elements.Analytical results of reference about RE and RSD using our method were better than 10%under the condition of 1450℃and 10min for most elements,respectively.When it was used in practical samples and compared with the solution-ICP-MS,the relative deviation of the two methods was basically within 18%.Therefore,LA-ICP-MS combined with flux free fusion sample preparation can save the complicated chemical digestion process,and was suitable for the analysis of refractory elements,REEs,U,Th and other elements in samples of uranium exploration.

关 键 词：难溶元素 稀土元素 铀矿勘查 无助熔剂熔融法 LA-ICP-MS 

分 类 号：O657.63[理学—分析化学]