年 0 21, Nu Noblesse,, Nu Noblesse, Thermo ArgusVI Helix-SFT Helix-MC plus ArgusVI, 40 Ar/ 39 Ar 1 ArgusVI Argus 40 Ar/ 39 Ar ( 1) [1 4] Argus

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1 第 44 卷第 5 期 Vol.44, No.5, 年 9 月 GEOCHIMICA Sept., Ar/ 39 Ar 邱华宁 1,2*, 白秀娟 1, 刘文贵 3, 梅廉夫 1 (1. ( ), ; 2., ; 3. ( ), ) 摘要 :, ArgusVI, 40 Ar/ 39 Ar 40 Ar/ 39 Ar Qtegra Noble Gas PeriCon,,, Qtegra,, 40 Ar/ 39 Ar 40 Ar/ 36 Ar,, 40 Ar/ 39 Ar 关键词 : 40 Ar/ 39 Ar ; ; ; ; ArgusVI ; Qtegra 中图分类号 : P597 文献标识码 : A 文章编号 : (2015) Automatic 40 Ar/ 39 Ar dating technique using multicollector ArgusVI MS with home-made apparatus QIU Hua-ning 1,2*, BAI Xiu-juan 1, LIU Wen-gui 3 and MEI Lian-fu 1 1. MOE Key Laboratory of Tectonics and Petroleum Resources, China University of Geosciences, Wuhan , China; 2.State Key Laboratory of Isotope Geochemistry, Guangzhou Institute of Geochemistry, Chinese Academy of Sciences, Guangzhou , China; 3.State Key Laboratory of Geological Processes and Mineral Resources, China University of Geosciences, Wuhan , China Abstract: In this study we designed and developed an efficient preparation system of small volume, a CO 2 laser for heating samples, a crusher for extracting fluid inclusions and an air argon system for automatic 40 Ar/ 39 Ar dating. A new 40 Ar/ 39 Ar laboratory has thus been established by using these apparatus connected to an ArgusVI mass spectrometer in China University of Geosciences (Wuhan). The peripheral accessories of third party hardware, such as pneumatic valves, CO 2 laser and crusher, can be controlled by the Qtegra Noble Gas software through a PeriCon (peripheral controller). Therefore, the experimental precedures of air argon analyses, 40 Ar/ 39 Ar dating by laser stepwise heating and by crushing in vacuo could be fullly automatically performed. By two hundreds of air argon analyses, we have obtained well concordant atmospheric 40 Ar/ 36 Ar ratios with a weighted mean of ± 0.03 (1, MSWD = 0.74), indicating that all the devices made in-house are effective and reliable. This work serves as a pioneer example in China for establishment of a new noble gas laboratory with home-made peripheral accessories except for mass spectrometer. Key words: 40 Ar/ 39 Ar; CO 2 laser; preparation system; ArgusVI mass spectrometer; Qtegra noble gas software 收稿日期 (Received): ; 改回日期 (Revised): ; 接受日期 (Accepted): 基金项目 : (2012CB416706); ( ) 作者简介 : (1963 ),,, * 通讯作者 (Corresponding author): QIU Hua-ning, Huaning.Qiu@gmail.com; Tel: QIU Hua-ning et al.: Automatic 40 Ar/ 39 Ar dating technique using multicollector ArgusVI MS with home-made apparatus

478 2015 年 0 21, Nu Noblesse,, Nu Noblesse, Thermo ArgusVI Helix-SFT Helix-MC plus ArgusVI, 40 Ar/ 39 Ar 1 ArgusVI Argus 40 Ar/ 39 Ar ( 1) [1 4] ArgusVI 200, 678 ml (Hamilton, 2015, ) 5 1 CDD, H2 H1

2 年 0 21, Nu Noblesse,, Nu Noblesse, Thermo ArgusVI Helix-SFT Helix-MC plus ArgusVI, 40 Ar/ 39 Ar 1 ArgusVI Argus 40 Ar/ 39 Ar ( 1) [1 4] ArgusVI 200, 678 ml (Hamilton, 2015, ) 5 1 CDD, H2 H1 AX L1 L2 CDD ~ Ω, ~ fa, H Ω, H1 L Ω 1 NP10,, 20 L/s, Ar/ 39 Ar, 1 Zr-Ar 1 (Pfeiffer) HiCube Eco (Varian) StarCell 40 L/s (Swagelok) (5 ), CF16 1/4 VCR, 2 80 ml ( ), 18 ml, 62 ml, Thermo 340 ml (Hamilton, 2015, ) Thermo ArgusVI (678 ml) 1018 ml, ArgusVI 740 ml, Ar, ( ) 37% 2.2, 50 W, 10.6 μm, 1.8 mm, mm, 3.0 mm 2.5 mm 0.1%,, 2, CCD,, ArgusVI Fig.1 ArgusVI noble gas mass spectrometer, 5 Ar 40 Ar ~ 36 Ar H2 H1 AX L1 L2 5, H1 AX L1 L2 CDD 4 1 CDD,, CDD CF63, 63 mm, [5] 3.0 mm 2.5 mm,,, ;, 5~10 mm, Geochimica Vol. 44 No. 5 pp Sept., 2015

3 第 5 期邱华宁等 : 自动化 40 Ar/ 39 Ar 定年设备研制 479 碎样管激光器样品腔触发按扭 V4 LAV V5 V3 CRV TBV V7 冷阱隔离阀涡旋干泵分子泵 V2 AV1 AV2 IP2V V6 纯化泵离子泵 40L/s 空气瓶 ILV V1 手动阀门气动阀门离子泵 20L/s IP1V Argus VI 质谱仪真空指示 [mbar] Adc1 [V] 关开阀门 IP1V 位置指示气动阀门 4.32 Fig.2 2 ( ) 40 Ar/ 39 Ar A sketch of the 40 Ar/ 39 Ar dating laboratory in China University of Geosciences (Wuhan) 2.4 [6 10],, 40 Ar/ 39 Ar,,,, 空气瓶 31 L, 1/4VCR, 0.1 ml, 2 AV1 AV2 31,, d ( ), 40 L/s 3 d : (1), ; (2), 0.50 ml ( 1 ml 1/4 VCR ), 8 h, 31 L Ar 0.937% [11], Ar : Ar = (0.5 ml 76 Torr %) / ml = Torr Ar/ 39 Ar, Qtegra Noble Gas,, 40 Ar/ 39 Ar : (%) ( ) (s) XY (mm) csv, WPS Excel,,,, ( ), 3.2 Qtegra Noble Gas : Configurator, Instrument Control, Workflow Editor Experiment Editor 配置模块实验配置, ArgusVI ArgusControl NGPrepOnArgusVI, PeriCon ( 2 ) NGWorkflow 硬件面板配置 Graphics View 2, ArgusVI (PeriCon ) Preview 外部设备控制器 PeriCon Qtegra, 16, 1 PeriCon 16 QIU Hua-ning et al.: Automatic 40 Ar/ 39 Ar dating technique using multicollector ArgusVI MS with home-made apparatus

4 年实验室要求, 可以考虑购买第 2 个 PeriCon 对于未设备, 防止人为误操作购买 Thermo 公司纯化系统的用户, 可以利用 ArgusVI 质谱仪本身内置的控制电路 (实质上亦为工作流程模块工作流程模块 NGWorkflow 给用户提供了非常 PeriCon), 增加外设控制方便的编写工作流程的软件平台, 如图 3 所示, 展仪器控制软件仪器控制软件(Instrument Control)通常可分割示空气氩分析的工作流程该模块右上角的工作流为若干窗口, 为方便操作监视和仪器检漏, 我们通关闭 Close/Off 设定 Set 等待 Wait 设定时间零常设成 3 个窗口左窗口为质谱控制 (Argus 点 Set Time Zero 获得数据 Acquire Data (即质谱测 Controls) 右上窗口为质谱接收器信号输出(ArgusVI 量)和信息 Message (简要说明工作流程的内容, 如 Graph View), 右下窗口为实验室结构简图(图 2) 空气氩分析和激光加热分析等) 程命令(Workflow Commands)包括打开 Open/On 质谱控制窗口包括离子规真空指示与控制离工作流程编辑器左边就如记录本, 分为 3 列, 子泵阀门控制加速电压捕集电压电流磁场电依次为命令参数 1 和参数 2 点击右上压, 以及离子源各种参数设定角的命令 Open/On, 自动弹出仪器各种内置设备(显接收器信号输出窗口可同时显示 5 个接收器的示为设备名称)和外部设备(显示为 Pericon 1 和 2), 信号(以不同颜色表示), 也可以选择性输出某一个选择相应的设备, 即写入记录本 1 行前面 2 列, 在第接收器信号表达方式为信号强度随时间的变化曲 3 列参数 2 中可以输入相应的说明依此类推, 写线窗口显示时间跨度为 180 s, 实际信号显示的时完 1 个完整的工作流程后, 点击 Save 保存为 1 个纯间跨度为 130 s 文本文件(txt), 其中 3 列的内容之间以冒号分隔在实验室结构图(图 2, 即外部设备 PeriCon 窗图 3 给出了空气氩分析的工作流程, 并在参数口)进行鼠标点击, 可开/关离子规气动阀门和 2 中加了详细说明同样, 可以编写出本底测定流各种电器等外部设备, 方便操作和仪器检漏当启体包裹体定年和激光加热分析等实验的工作流程动实验流程时, 计算机控制仪器系统完成指定的实验, 这时 PeriCon 窗口变为灰色, 鼠标不能操控外部图3 本底空气氩和样品 40 Ar/39Ar 定年实验的工作流程是相似的, 通过设定各个气动阀门的开/关状工作流程编辑器 Fig.3 Noble Gas Workflow Editor 示例空气氩同位素测定工作流程, 附简要说明, 气动阀门缩写参见图 2 Geochimica Vol. 44 No. 5 pp Sept., 2015

5 第 5 期邱华宁等 : 自动化 40 Ar/ 39 Ar 定年设备研制 481 ( ),, 40 Ar/ 39 Ar : (1) ( 2, LAV IP2V IP1V, ), 2 30 s, ; (2) 60 s ; (3), 80 ~ 120, ; (4) Zr-Al, 400 s( ); (5) ILV,, 20 s, ; (6), IP2V ; (7), ILV 40 L/s 90 s, ; (8) ILV, IP1V, 20 L/s,,,, 实验编辑器与实验流程全自动化 1 1,, 40 Ar/ 39 Ar Templates Analysis Templates Analysis, ( ) ( ) 40 Ar/ 39 Ar,, ( 3.1 ), 1 (LabBook) ( imexp) 1, Run, Schedule, Run,,,,,, 1 ( ), 40 Ar/ 39 Ar 40 Ar 39 Ar, ; 38 Ar 37 Ar 36 Ar,,, ( 20 fa), 40 Ar/ 39 Ar,,,,, 6~ Ar/ 39 Ar,, 1 4 Koppers 40 Ar/ 39 Ar ArArCALC [12] V2.52b ArgusVI, J MDF, 40 Ar/ 39 Ar, ( ) Excel [13] Thermo Qtegra Noble Gas Analysis (.imexp), ArArCALC, Excel (.xls), Qtegra Noble Gas Excel ArArCALC ( csv ), ( D:\ArArRawDat\2014\06) L 0.1 ml,, 1/4VCR 0.50 ml ( 2, LAV V4, 1 ml ),, QIU Hua-ning et al.: Automatic 40 Ar/ 39 Ar dating technique using multicollector ArgusVI MS with home-made apparatus

6 年 8 h, AV2 AV1,, 1 h, AV1 AV2, 1, 3,, 10, 1 ArArCALC V2.52b, MDF ~12 4 7~9, 36 Ar 38 Ar 40 Ar L2 AX H2, fa fa (, ), Ar 38 Ar 40 Ar 0.052% 0.170% 0.031% ( 1 ), 20 fa, ; 100 fa, (50 V fa), 5~14, 38 Ar 40 Ar/ 36 Ar (1 ) 4 ( ), ± ± 0.03 ( %), MDF ± ± ( 40 Ar/ 36 Ar ) 40 Ar/ 36 Ar MDF, Ar-Ar, 5.2 ILV,,,,,,, s, 1 ( ), 80 ml, 18 ml, 1 1 5a, 30~35 s, 40 Ar 40 Ar/ 36 Ar,, 30 s, 47 ml ( 32 ml, 1/4 15 ml), 1/4 ( 3.8 mm), 1 5b, 40 s, 40 Ar, 40 s 4 Fig.4 Measurement of 40 Ar/ 36 Ar ratios of modern atmospheric argon in the laboratory (a) ~12 ; (b) ~9 40 Ar/ 36 Ar 1, Geochimica Vol. 44 No. 5 pp Sept., 2015

7 第 5 期邱华宁等 : 自动化 40 Ar/ 39 Ar 定年设备研制 Ar - Fig.5 Diagrams of 40 Ar intensity vs inlet time (a) ; (b) 表 1 40 Ar 强度 - 进气时间测定值 Table 1 Measurement of 40 Ar intensity and inlet time (s) 40 Ar (fa) 40 Ar/ 36 Ar :, ( ),, 40 Ar/ 36 Ar,, 40 Ar/ 36 Ar, 36 Ar 40 Ar,,, Ar/ 39 Ar 09PT20MS [14 15], 40 Ar/ 39 Ar ( 6a), (158.5±1.6) Ma ( 39 Ar 97%), MSWD 0.41 ( 97%) 36 Ar/ 40 Ar- 39 Ar/ 40 Ar ( 6b),, (158.5±1.8) Ma, 40 Ar/ 36 Ar 295.6±12.3, MSWD 0.44 ( 95%) Fig Ar/ 39 Ar 40 Ar/ 39 Ar age spectrum and inverse isochron for a muscovite sample from the Piaotang Tungsten Deposit QIU Hua-ning et al.: Automatic 40 Ar/ 39 Ar dating technique using multicollector ArgusVI MS with home-made apparatus

8 年 6 (1) 40 Ar/ 39 Ar, Ar, 40 Ar/ 39 Ar, (2) Thermo Qtegra Noble Gas, 40 Ar/ 39 Ar, (3), 40 Ar/ 36 Ar, ArgusVI 感谢贺怀宇研究员的建设性意见参考文献 (References): [1] Alexandre P, Hamilton D, Barfod D. The ARGUS multicollection noble gas mass spectrometer[j]. Geochim Cosmochim Acta, 2006, 70(18): A8. [2] Barfod D, Alexandre P, Hamilton D. The ARGUS multicollection noble gas mass spectrometer[j]. Geochim Cosmochim Acta, 2006, 70(18): A34. [3] Mark D F, Barfod D, Stuart F M, Imlach J. The ARGUS multicollector noble gas mass spectrometer: Performance for 40 Ar/ 39 Ar geochronology[j]. Geochem Geophys Geosyst, 2009, 10(2): Q0AA02. [4] Pfaender J A, Sperner B, Ratschbacher L, Fischer A, Meyer M, Leistner M, Schaeben H. High-resolution 40 Ar/ 39 Ar dating using a mechanical sample transfer system combined with a high-temperature cell for step heating experiments and a multicollector ARGUS noble gas mass spectrometer[j]. Geochemistry Geophysics Geosystems, 2014, 15(6): [5]. Ar-Ar : Ar-Ar [J]., 2006, 35(2): Qiu Hua-ning. Construction and development of new Ar-Ar laboratories in China: Insight from GV-5400 Ar-Ar laboratory in Guangzhou Institute of Geochemistry, Chinese Academy of Sciences[J]. Geochimica, 2006, 35(2): (in Chinese with English abstract). [6] Nier A O. A redetermination of the relative abundances of the isotopes of carbon, nitrogen, oxygen, argon and potassium[j]. Phys Rev, 1950, 77: [7] Lee J-Y, Marti K, Severinghaus J P, Kawamura K, Yoo H-S, Lee J B, Kim J S. A redetermination of the isotopic abundances of atmospheric Ar[J]. Geochim Cosmochim Acta, 2006, 70(17): [8] Renne P R, Cassata W S, Morgan L E. The isotopic composition of atmospheric argon and 40 Ar/ 39 Ar geochronology: Time for a change?[j] Quatern Geochronol, 2009, 4(4): [9] Valkiers S, Vendelbo D, Berglund M, de Podesta M. Preparation of argon Primary Measurement Standards for the calibration of ion current ratios measured in argon[j]. Int J Mass Spectrom, 2010, 291(1/2): [10] Mark D F, Stuart F M, de Podesta M. New high-precision measurements of the isotopic composition of atmospheric argon[j]. Geochim Cosmochim Acta, 2011, 75(23): [11] Kellas A. On the percentage of argon in atmospheric and in respired air[j]. Proc R Soc London, 1895, 59(1): [12] Koppers A A P. ArArCALC - software for 40 Ar/ 39 Ar age calculations[j]. Comput Geosci, 2002, 28(5): [13],,,,,,. 40 Ar/ 39 Ar ArArCALC [J]., 2009, 38(1): Zhang Fan, Qiu Hua-ning, He Huai-yu, Yang Lie-kun, Su Fei, Wang Ying, Wu Lin. Brief introduction to ArArCALC software for data reduction in 40 Ar/ 39 Ar geochronology[j]. Geochimica, 2009, 38(1): (in Chinese with English abstract). [14],,,,,. 40 Ar/ 39 Ar [J]., 2011, 56(23): Bai Xiujuan, Wang Min, Lu Kehao, Fang Jinlong, Pu Zhiping, Qiu Huaning. Direct dating of cassiterite by 40 Ar/ 39 Ar progressive crushing[j]. Chinese Sci Bull, 2011, 56(23): (in Chinese). [15] Bai X J, Wang M, Jiang Y D, Qiu H N. Direct dating of tin-tungsten mineralization of the Piaotang Tungsten deposit, South China, by 40 Ar/ 39 Ar progressive crushing[j]. Geochim Cosmochim Acta, 2013, 114: Geochimica Vol. 44 No. 5 pp Sept., 2015

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