New Progresses in Analytical Methods of in situ S Isotope Measurement
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摘要: 综述了十余年来激光剥蚀等离子体质谱（LA-MC-ICP-MS）和二次离子质谱（SIMS）测定硫化物硫同位素的新进展，着重介绍了质谱干扰和同位素质量分馏效应的关键技术难点和校正方案.LA-MC-ICP-MS和SIMS都可实现黄铁矿、黄铜矿、闪锌矿、方铅矿、磁黄铁矿、镍黄铁矿、辉钼矿的微区δ34S准确测定，测试准确度和传统的整体分析测试技术相当，测试精密度（重现性）在0.17‰~0.45‰.目前硫化物硫同位素标准物质主要是黄铁矿、黄铜矿、磁黄铁矿、闪锌矿等矿物，缺乏其他硫化物类型的标准物质.改进仪器设备硬件或关键部件，系统深入调查仪器中的同位素质量分馏和基体效应，开发新的高质量硫化物硫同位素标准物质将是未来微区原位硫化物硫同位素测试主要发展方向.Abstract: The new progresses in analytical methods of in situ S isotope measurement by using laser ablation multi-collector inductively coupled plasma mass spectrometry (LA-MC-ICP-MS) and secondary ion mass spectrometry (SIMS) have been reviewed in this paper. The review is focused on the key technical difficulties, correction schemes of mass spectrum interference, and mass fractionation effects in the two instruments. As it suggested, both LA-MC-ICP-MS and SIMS can accurately determine the δ34S of various minerals, such as pyrite, chalcopyrite, sphalerite, galenite, pyrrhotite, pentlandite, molybdenite etc. The analytical accuracy is comparable to the traditional bulk analysis. The analytical precision (reproducibility) is ranges of from 0.17‰ to 0.45‰. There are a large number of reference materials of S isotope analysis in sulfides. However, the main reference materials are pyrite, chalcopyrite, pyrrhotite, and sphalerite. Other sulfides also lack the reference materials for microanalysis. It is suggested that improving the hardwares or key equipments, resolving the isotope fractionation and the matrix effect, developing the new sulfide reference materials will be the major development directions for the in situ S isotopic measurement by LA-MC-ICP-MS and SIMS.
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Key words:
- S /
- isotopes /
- LA⁃MC⁃ICP⁃MS /
- SIMS /
- microanalysis /
- reference materials /
- geochemistry
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图 1 不同微区技术（LA-MC-ICP-MS和SIMS）测定硫化物δ34S值与整体分析技术（IR-MS或者MC-ICP-MS）参考值之间的关系
Fig. 1. The relationship of determination of δ34S value in sulfide between micro-analysis (LA-MC-ICP-MS and SIMS) and bulk analysis (IR-MS and MC-ICP-MS)
图 2 LA-MC-ICP-MS和SIMS测定硫化物标准物质δ34S值的重现性（不确定度，‰）
Fig. 2. The reproducibility of δ34S value (uncertainty, ‰) in sulfide reference materials determined by LA-MC-ICP-MS and SIMS
表 1 硫同位素微区固体标准物质汇总
Table 1. Summary of solid reference materials for microanalysis of S isotope ratios
IRMS/SN⁃MC LA⁃MC⁃ICP⁃MS SIMS 参考文献 平均值 不确定度* 平均值 不确定度* 平均值 不确定度* Pyrite（黄铁矿） GAV-18 天然矿物 9.62 0.27 Craddock et al., 2008 10th-1 PSPT 5.33 0.27 5.22 0.22 Feng et al., 2018 PSPT-2 PSPT 32.48 0.29 32.65 0.26 Bao et al., 2017， GBW07267 RPP 3.46 0.18 3.56 0.43 Chen et al., 2022a PAS-Py600 PAS 18.22 0.07 18.06 0.25 Feng et al., 2022 RPPY RPP 3.65 0.29 3.58 0.31 Lv et al., 2022 Py1 天然矿物 ‒0.6 0.6 ‒1 1.2 Molnár et al., 2016 Py2 天然矿物 ‒0.4 1 ‒0.4 0.4 Molnár et al., 2016 IGGPy-1 天然矿物 17.09 0.09 17.05 0.15 17.01 0.15 Xie et al., 2024 PPP-1 天然矿物 5.1 0.6 5.3 0.3 Gilbert et al., 2014 UWPy-1 天然矿物 16.39 0.4 17.4 0.17 Kozdon et al., 2010 Py-1117 天然矿物 0.3 0.02 0.2 0.4 Zhang et al., 2014 CS01 天然矿物 4.6 0.08 4.3 0.4 Zhang et al., 2014 Balmat 天然矿物 15.1 0.2 Crowe and Vaughan, 1996 Ruttan 天然矿物 1.2 0.1 Crowe and Vaughan, 1996 CAR 123 天然矿物 1.4 0.4 Mojzsis et al., 2003 Sierra 天然矿物 2.17 0.28 0.25 LaFlamme et al., 2016 NWU-Py PAS 3.39 0.07 3.48 0.26 Peng et al., 2024 Chalcopyrite（黄铜矿） CCP 天然矿物 ‒0.7 1 ‒0.2 0.8 Molnár et al., 2016 PSPT-1 PSPT ‒0.73 0.09 ‒0.9 0.41 Bao et al., 2017 YN411-m Glass 0.37 0.24 0.6 0.3 Chen et al., 2017 GC 天然矿物 ‒0.79 0.24 ‒0.7 0.2 Chen et al., 2017 Cpy-1 天然矿物 4.12 0.23 4.4 0.3 Chen et al., 2017 TC1725 天然矿物 12.78 0.16 12.74 0.38 Bao et al., 2021 PAS-Cpy600 PAS 10.58 0.33 10.43 0.29 Feng et al., 2022 GBW07268 RPP ‒0.57 0.24 ‒0.38 0.43 Chen et al., 2022a HTS4-6 天然矿物 0.63 0.16 0.58 0.38 Li et al., 2020 CPY-1 天然矿物 1.4 0.4 1.4 0.93 Li et al., 2020 GC-1 RPP ‒0.65 0.28 ‒0.68 0.32 Lv et al., 2022 Norilsk 天然矿物 8 0.2 Crowe and Vaughan, 1996 Trout Lake 天然矿物 0.3 0.2 Crowe and Vaughan, 1996 IGSD 天然矿物 4.21 0.23 4.10 0.30 4.0 0.10 Chen, 2023 Nifty-b 天然矿物 ‒3.58 0.44 0.23 LaFlamme et al., 2016 Sphalerite（闪锌矿） NBS123 PPP 17.09 0.19 Pribil et al., 2015 PSPT-3 PSPT 26.4 0.21 26.23 0.23 Bao et al., 2017 PAS-GBW07270 PAS ‒5.44 0.15 ‒5.44 0.2 Nie et al., 2023 SPH-1 RPP ‒7.13 0.41 ‒7.22 0.47 Lv et al., 2022 BT-4 天然矿物 15.42 0.14 15.3 0.58 Kozdon et al., 2010 JC-14 天然矿物 4.9 0.08 5 0.6 Zhang et al., 2014 MY09-12 天然矿物 3.1 0.12 3.6 0.8 Zhang et al., 2014 Balmat 天然矿物 14.3 0.2 Crowe and Vaughan, 1996 Chisel 天然矿物 1.5 0.1 Crowe and Vaughan, 1996 Galena（方铅矿） RPP-Gn RPP ‒0.94 0.36 ‒0.82 0.39 Chen et al., 2022a NWU-GN RPP 28.27 0.17 28.44 0.45 Lv et al., 2022 UWGal-1 天然矿物 16.61 0.16 16.6 0.76 Kozdon et al., 2010 Pyrrhotite（磁黄铁矿） Po-10 天然矿物 6.1 0.6 5.9 0.3 Gilbert et al., 2014 Po 天然矿物 5.6 1.2 6.8 1 Molnár et al., 2016 Anderson 天然矿物 1.4 0.2 Crowe and Vaughan, 1996 Alexo 天然矿物 5.23 0.4 0.3 LaFlamme et al., 2016 YP136 天然矿物 1.5 0.1 1.5 0.3 Li et al., 2019 JC-Po 天然矿物 0.06 0.33 ‒0.09 0.27 Chen et al., 2021 Pentlandite（镍黄铁矿） Norilsk 天然矿物 7.9 0.2 Crowe and Vaughan, 1996 VMSo 天然矿物 3.22 0.51 0.33 LaFlamme et al., 2016 JC-Pn 天然矿物 ‒0.09 0.15 0.19 Chen et al., 2021 Arsenopyrite（毒砂） RPP-Apy RPP ‒1.05 0.15 ‒1.04 0.42 Chen et al., 2022a NWU-Apy PAS 18.17 0.16 18.19 0.32 Peng et al., 2024 Bornite（斑铜矿） N-11 天然矿物 ‒4.4 0.6 Gilbert et al., 2014 Barite（重晶石） NWU-Brt 天然矿物 14.17 0.42 14.27 0.23 Lv et al., 2024 Molybdenite（辉钼矿） Mo-H8 HTHP ‒0.22 0.1 Tian et al., 2024 Mo-P RHP ‒0.22 0.1 Tian et al., 2024 Stibnite（辉锑矿） BJ-Snt 天然矿物 ‒0.71 0.32 ‒0.78 0.36 Dai et al., 2024 Gypsum（石膏） NWU-Gy PAS ‒0.20 0.05 ‒0.19 0.32 Peng et al., 2024 
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