LA-ICPMS技术优化及应用
发布时间：2018-07-29 20:28
【摘要】：激光剥蚀-电感耦合等离子体质谱是由激光剥蚀系统和电感耦合等离子体质谱仪联用的新型仪器(英文缩写为LA-ICPMS),该分析技术具有原位、实时、快速的分析优势和灵敏度高、空间分辨率较好等优点。尽管LA-ICPMS固体微区原位分析应用广泛,但对地质样品中元素含量的准确分析仍旧受到多种因素的制约,诸如仪器条件、分馏效应随样品基体组成的变化、基体匹配标准物质的不足、定量化计算策略和有效的灵敏度漂移校正等。在开展LA-ICPMS锆石U-Pb测年正常运行了数年的基础上,本文通过对LA-ICPMS分析技术优化改进,包括将仪器自带的常规剥蚀池更换为旋转式双通道剥蚀池、增加信号匀化器、在等离子体中心气流(Ar+He)中加入少量氮气(气体流量为2.5 ml/min)等措施,实现了提高仪器灵敏度、降低检出限和改善分析精密度。利用优化后的LA-ICPMS分析技术,开展了激光束斑为24μm和16μm的锆石U-Pb测年。以NIST SRM 610为标样校正元素含量,以锆石91500为国际标准校正年龄值,以Zr91为内标元素,获得了激光束斑为24μm条件下三个锆石标准Plesovice、Mud Tank和Qinghu 206Pb/238U年龄加权平均值分别为337.0±3.1 Ma、732.0±6.8 Ma、158.2±1.6 Ma,激光束斑为16μm三个锆石标准Plesovice、Mud Tank和Qinghu 206Pb/238U年龄加权平均值分别为339.6±4.1 Ma、732.9±8.1 Ma、159.8±1.8 Ma,上述结果与推荐值吻合较好。说明本实验室开展的小激光束斑锆石U-Pb测年方法是可行的,该锆石U-Pb测年方法适用于颗粒较小和成因复杂的锆石,对于获得更精细的年龄有着重要意义。本实验室还开展了硅酸盐主微量元素的测试工作。利用优化后的LA-ICPMS分析技术,在激光束斑为44μm、频率为5 Hz的条件下,对BCR-2G、BIR-1G、ATHO-G、GOR132-G、T1-G和St Hs6/80-G这六个国际标准物质的熔融玻璃进行了LA-ICPMS的10种主量元素和47种微量元素分析,对同一套数据分别以NIST SRM 610、GSE-1G和MPI-DING国际标准物质做外标,采用Ca为归一化元素,分别采用无内标法和以Ca为内标法的校正策略,对每一个样品所获得的6组结果进行对比,结果表明本实验室建立的硅酸盐单矿物LA-ICPMS主微量元素测试方法是可行的,并且对比了不同校正策略所获的结果之间的差别,并初步探讨了其可能的原因。此外,还尝试了碳酸盐的主微量元素的测试工作。以NIST SRM 610、GSE-1G和MPI-DING国际标准物质做外标,采用44μm、60μm的激光束斑,5 Hz的激光频率,以无内标法和以Ca为内标的校正策略,对碳酸盐国际标准物质MACS-3进行了主量和微量元素的分析测试。分析结果表明,大部分元素测试值与推荐值的相对误差(RE)在20%以内,相对标准偏差(RSD)基本都在10%以内,同时我们用无内标法能够准确地测定出碳酸盐的主微量元素,说明本实验室尝试建立的碳酸盐主微量元素LA-ICPMS微区原位测试方法设计可行性。
[Abstract]:Laser denudation-inductively coupled plasma mass spectrometry (ICP-MS) is a new type of instrument (abbreviated LA-ICPMS), which is used by laser denudation system and inductively coupled plasma mass spectrometer (LA-ICPMS). It has the advantages of in-situ, real-time, rapid analysis and high sensitivity. Good spatial resolution and other advantages. Although LA-ICPMS solid microanalysis is widely used in situ analysis, the accurate analysis of element content in geological samples is still restricted by many factors, such as instrumental conditions, fractionation effect and changes of sample matrix composition. The deficiency of matrix matching standard material, quantitative calculation strategy and effective sensitivity drift correction etc. Based on the normal operation of LA-ICPMS zircon U-Pb dating for several years, this paper optimizes and improves the LA-ICPMS analysis technology, including replacing the conventional denudation tank with the instrument into a rotary two-channel denudation pool, and increasing the signal leveller. A small amount of nitrogen (gas flow rate 2.5 ml/min) was added to the plasma central gas flow (Ar He) to improve the instrument sensitivity, reduce the detection limit and improve the analytical precision. Zircon U-Pb dating with laser beam spot of 24 渭 m and 16 渭 m was carried out by using the optimized LA-ICPMS analysis technique. Using NIST SRM 610 as standard sample to calibrate element content, zircon 91500 as international standard correction age value, Zr91 as internal standard element, The three zircon standard plesovicem Tank and Qinghu 206Pb/238U age weighted mean values of 337.0 卤3.1 Mai 732.0 卤6.8 Ma 158.2 卤1.6 Ma were obtained under the laser beam spot condition of 24 渭 m. The average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U were 339.6 卤4.1 Ma 73 2.9 卤8.1 Mai 159.8 卤1.8 Ma, respectively, for the laser beam spot of 16 渭 m. The results show that the average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U are 339.6 卤4.1 Ma, 732.9 卤8.1 Ma, 159.8 卤1.8 Ma, respectively. The results are in good agreement with the recommended values. The results show that the U-Pb dating method of small laser beam zircon developed in our laboratory is feasible, and the U-Pb dating method is suitable for zircon with small grain size and complex genesis, which is of great significance for obtaining a more precise age. The test of silicate main trace elements was also carried out in our laboratory. Under the condition of laser beam spot of 44 渭 m and frequency of 5 Hz, the melting glass of six international standard materials, BCR-2GN, BIR-1G, ATHO-G, GOR132-G, T1-G and St Hs6/80-G, was analyzed by using the optimized LA-ICPMS analysis technique. Ten major elements and 47 trace elements of LA-ICPMS were analyzed. For the same set of data, NIST SRM 610G and MPI-DING were used as external standard, Ca as normalized element, no internal standard method and Ca as internal standard method respectively. The results obtained from each sample were compared. The results show that the test method of silicate single mineral LA-ICPMS is feasible, and the differences between the results obtained by different correction strategies are compared, and the possible reasons are discussed. In addition, the main trace elements of carbonate were tested. Using NIST SRM 610G and MPI-DING as the external standard, using the laser frequency of 44 渭 m or 60 渭 m, the method of no internal standard and the correction strategy of Ca as the internal standard, the main quantity and trace element of MACS-3, the international standard material of carbonate, were analyzed and tested by using the laser frequency of 44 渭 m or 60 渭 m. The results show that the relative error between the test value and the recommended value of most elements is within 20%, and the relative standard deviation (RSD) is less than 10%. At the same time, we can accurately determine the main trace elements of carbonate by using no internal standard method. The results show that the in-situ test method of carbonate main trace element LA-ICPMS is feasible.
【学位授予单位】：合肥工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：P597.3;P575
本文编号：2153920
[Abstract]:Laser denudation-inductively coupled plasma mass spectrometry (ICP-MS) is a new type of instrument (abbreviated LA-ICPMS), which is used by laser denudation system and inductively coupled plasma mass spectrometer (LA-ICPMS). It has the advantages of in-situ, real-time, rapid analysis and high sensitivity. Good spatial resolution and other advantages. Although LA-ICPMS solid microanalysis is widely used in situ analysis, the accurate analysis of element content in geological samples is still restricted by many factors, such as instrumental conditions, fractionation effect and changes of sample matrix composition. The deficiency of matrix matching standard material, quantitative calculation strategy and effective sensitivity drift correction etc. Based on the normal operation of LA-ICPMS zircon U-Pb dating for several years, this paper optimizes and improves the LA-ICPMS analysis technology, including replacing the conventional denudation tank with the instrument into a rotary two-channel denudation pool, and increasing the signal leveller. A small amount of nitrogen (gas flow rate 2.5 ml/min) was added to the plasma central gas flow (Ar He) to improve the instrument sensitivity, reduce the detection limit and improve the analytical precision. Zircon U-Pb dating with laser beam spot of 24 渭 m and 16 渭 m was carried out by using the optimized LA-ICPMS analysis technique. Using NIST SRM 610 as standard sample to calibrate element content, zircon 91500 as international standard correction age value, Zr91 as internal standard element, The three zircon standard plesovicem Tank and Qinghu 206Pb/238U age weighted mean values of 337.0 卤3.1 Mai 732.0 卤6.8 Ma 158.2 卤1.6 Ma were obtained under the laser beam spot condition of 24 渭 m. The average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U were 339.6 卤4.1 Ma 73 2.9 卤8.1 Mai 159.8 卤1.8 Ma, respectively, for the laser beam spot of 16 渭 m. The results show that the average age weighted values of the three zircon standard plesovicege Mud Tank and Qinghu 206Pb/238U are 339.6 卤4.1 Ma, 732.9 卤8.1 Ma, 159.8 卤1.8 Ma, respectively. The results are in good agreement with the recommended values. The results show that the U-Pb dating method of small laser beam zircon developed in our laboratory is feasible, and the U-Pb dating method is suitable for zircon with small grain size and complex genesis, which is of great significance for obtaining a more precise age. The test of silicate main trace elements was also carried out in our laboratory. Under the condition of laser beam spot of 44 渭 m and frequency of 5 Hz, the melting glass of six international standard materials, BCR-2GN, BIR-1G, ATHO-G, GOR132-G, T1-G and St Hs6/80-G, was analyzed by using the optimized LA-ICPMS analysis technique. Ten major elements and 47 trace elements of LA-ICPMS were analyzed. For the same set of data, NIST SRM 610G and MPI-DING were used as external standard, Ca as normalized element, no internal standard method and Ca as internal standard method respectively. The results obtained from each sample were compared. The results show that the test method of silicate single mineral LA-ICPMS is feasible, and the differences between the results obtained by different correction strategies are compared, and the possible reasons are discussed. In addition, the main trace elements of carbonate were tested. Using NIST SRM 610G and MPI-DING as the external standard, using the laser frequency of 44 渭 m or 60 渭 m, the method of no internal standard and the correction strategy of Ca as the internal standard, the main quantity and trace element of MACS-3, the international standard material of carbonate, were analyzed and tested by using the laser frequency of 44 渭 m or 60 渭 m. The results show that the relative error between the test value and the recommended value of most elements is within 20%, and the relative standard deviation (RSD) is less than 10%. At the same time, we can accurately determine the main trace elements of carbonate by using no internal standard method. The results show that the in-situ test method of carbonate main trace element LA-ICPMS is feasible.
【学位授予单位】：合肥工业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：P597.3;P575
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