矿床地球化学国家重要实验室(2)

2021-09-24 13:26

单个流体包裹体主、微量元素的含量分析在中国科学院地球化学研究所矿床地球化学国家重点实验室利用LA-ICP-MS 完成。激光剥蚀系统为GeoLasPro 193nm ArF 准分子激光器,电感耦合等离子体质谱(ICP-MS)为Agilent 7900。

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激光剥蚀过程中采用氦气载气、氩气为补偿气,并加入少量氮气提高灵敏度,三者在进入ICP之前通过一个T型接头混合。样品仓为标配的剥蚀池,其中加入树脂制作的模具来获得一个较小体积的取样空间,以降低记忆效应,提高冲洗效率。单个样品的信号采集包括大约20s的空白信号、50s包裹体取样时间、20s左右信号衰减至背景值的时间。分析过程中,激光工作参数一般为频率9~10Hz, 能量10-11J/cm2,束斑24-44μm(根据包裹体大小调整)。在测试之前用SRM610对ICP-MS性能进行优化,使仪器达到最佳的灵敏度和电离效率(U/Th≈1)、尽可能小的氧化物产率(ThO/Th<0.3%)和低的背景值。数据校正使用NIST SRM610做外

wt.%)为内标(Heinrich et al., 2003)。氯标、氯化钠等效盐度(NaCl

equivalent

化钠等效盐度通过单独的流体包裹体测温获得。每分析10个包裹体分析两次NIST SRM610(NIST SRM610+10 流体包裹体 + NIST SRM610)。对分析数据的离线处理(包括对样品和空白信号的选择、仪器灵敏度漂移校正、元素含量计算)采用软件SILLS(Guillong et al., 2008)完成。为了排除基质石英的影响,信号选择同时有Na、K或其他阳离子信号的区间。对于以氯化物为主的流体包裹体,推荐选择电价平衡(charge-balance)的方式来计算(Allen et al., 2005)。使用含五种元素的人工合成流体包裹体来监控数据准确度,其所含元素理论值为Na=K=Ca=2.05 wt.%,Rb=300 ppm, Cs=200 ppm,准确度一般优于16%。

In English:

(1)Trace element analyses of magnetite by LA-ICP-MS

Major and trace element analyses were conducted by LA-ICP-MS at the State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry Chinese Academy of Sciences. Laser sampling was performed using the NWR UP-213 Nd:YAG laser. An Agilent 7500x ICP-MS instrument was used to acquire ion-signal intensities. Helium was applied as a carrier gas which was mixed with Argon via a T-connector before entering the ICP-MS. Each analysis incorporated a background acquisition of approximately 30 s (gas blank) followed by 50 s of data acquisition from the sample. Element contents were calibrated against multiple-reference materials (GSE-1G,

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BCR-2G, BIR-1G and BHVO-2G) combined with internal standardization (Dare et al., 2012). The preferred values of element concentrations for the USGS reference glasses are from the GeoReM database (http://georem.mp ch-mainz.gwdg.de/). Off-line selection and integration of background and analyte signals, and time-drift correction and quantitative calibration were performed by ICPMSDataCal (Liu et al., 2008a; Liu et al., 2010a).

(2)Trace element analyses of carbonate by LA-ICP-MS

Major and trace element analyses were conducted by LA-ICP-MS at the State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry Chinese Academy of Sciences. Laser sampling was performed using a GeoLas Pro193 nm ArF excimer laser. An Agilent 7500x ICP-MS instrument was used to acquire ion-signal intensities. Helium was applied as a carrier gas which was mixed with Argon via a T-connector before entering the ICP-MS. Each analysis incorporated a background acquisition of approximately 30 s (gas blank) followed by 50 s of data acquisition from the sample. Element contents were calibrated against multiple-reference materials (GOR128-G,ATHO-G, StHs6/80-G,T1-G) combined with internal standardization (Chen et al., 2011). The preferred values of element concentrations for the reference glasses are from the GeoReM database (http://georem.mp ch-mainz.gwdg.de/). Off-line selection and integration of background and analyte signals, and time-drift correction and quantitative calibration were performed by ICPMSDataCal (Liu et al., 2008a; Liu et al., 2010a).

(3)Trace element analyses of apatite by LA-ICP-MS

Major and trace element analyses were conducted by LA-ICP-MS at the State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry Chinese Academy of Sciences. Laser sampling was performed using a GeoLas

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Pro193 nm ArF excimer laser. An Agilent 7500x ICP-MS instrument was used to acquire ion-signal intensities. Helium was applied as a carrier gas which was mixed with Argon via a T-connector before entering the ICP-MS. Each analysis incorporated a background acquisition of approximately 30 s (gas blank) followed by 50 s of data acquisition from the sample. Element contents were calibrated against multiple-reference materials (NIST610、NIST612、NIST614) combined with internal standardization (Chew et al., 2016). The preferred values of element concentrations for the reference glasses are from the GeoReM database (http://georem.mp ch-mainz.gwdg.de/). Off-line selection and integration of background and analyte signals, and time-drift correction and quantitative calibration were performed by ICPMSDataCal (Liu et al., 2008a; Liu et al., 2010a).

(4)Trace element analyses of silicate by LA-ICP-MS

Major and trace element analyses of silicate were conducted by LA-ICP-MS at the State Key Laboratory of Ore Deposit Geochemistry, Institute of Geochemistry Chinese Academy of Sciences. Laser sampling was performed using a GeoLas Pro 193 nm ArF excimer laser. An Agilent 7500x ICP-MS instrument was used to acquire ion-signal intensities. Helium was applied as a carrier gas which was mixed with Argon via a T-connector before entering the ICP-MS. Each analysis incorporated a background acquisition of approximately 30 s (gas blank) followed by 50 s of data acquisition from the sample. Element contents were calibrated against multiple-reference materials (NIST 610,BCR-2G, BIR-1G and BHVO-2G) without applying internal standardization (Liu et al., 2008a). The preferred values of element concentrations for the reference glasses are from the GeoReM database (http://georem.mp ch-mainz.gwdg.de/). Off-line selection and integration of background and analyte signals, and time-drift correction and quantitative calibration were performed by

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