Simultaneous Determination of U-Pb Age and Trace Elements of Zircon by Laser Ablation Sector Field Inductively Coupled Plasma-Mass Spectrometry
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摘要:
激光剥蚀-扇形磁场电感耦合等离子体质谱(LA-SF-ICP-MS)具有高灵敏度特征，被广泛应用于锆石等含U矿物原位微区U-Pb定年研究，但磁偏转式质量分析器的使用导致该质谱仪扫描速度相对较慢，可能影响U-Pb同位素与其他关键微量元素的同时采集。本文通过优化仪器信号稳定性和实验方法，对目前常用的7种锆石U-Pb标准样品进行U-Pb定年和Ti、REEs、Hf等关键元素同时定量分析，探讨了多元素同时分析方法的可行性及对于U-Pb定年结果的影响。实验结果表明，相对于LA-SF-ICP-MS仅检测U-Pb同位素方法，同时开展多元素含量检测可能会使U-Pb同位素信号强度稳定性下降，导致单点U-Pb年龄结果误差及离散程度增大。与仅测定U-Pb同位素年龄的测定结果相比较，根据不同锆石样品中U-Pb同位素含量高低，多元素同时检测获得分析点的206Pb/238U年龄和207Pb/235U年龄变化范围不同程度地增大，其中207Pb/235U年龄受影响明显，单点207Pb/235U年龄误差从～1.5%增大至～2.0%，单点年龄的相对标准偏差(RSD)从0.5%～1.3%增大至1.2%～3.3%。尽管如此，多元素同时检测方法对于各样品最终测定年龄没有明显的影响，相对于TIMS年龄，各样品的谐和年龄和206Pb/238U加权平均年龄偏差分别小于1.0%和0.7%，完全满足U-Pb同位素地质年代学测试要求。同时测定锆石样品中的关键微量元素含与其推荐值相对误差小于10%。因此，采用LA-SF-ICP-MS可以同时准确地测定锆石U-Pb年龄和微量元素含量，该方法亦可用于其他副矿物U-Pb年龄与关键微量元素同时测定。
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关键词:
- 激光剥蚀-扇形磁场电感耦合等离子体质谱(LA-SF-ICP-MS) /
- 锆石 /
- U-Pb定年 /
- 微量元素
Abstract:Laser ablation sector field inductively coupled plasma-mass spectrometry (LA-SF-ICP-MS) is widely applied in U-Pb dating of zircon due to its remarkable sensitivity. However, the utilization of a magnetic sector mass analyzer imposes constraints on its scanning speeds, potentially affecting the concurrent acquisition of U-Pb isotopes and other trace elements. Here a method for simultaneous zircon U-Pb dating and key trace elements quantifying by LA-SF-ICP-MS were developed. Seven zircon U-Pb standard samples were measured to assess the method's feasibility. Experimental data indicate that simultaneous collection of U-Pb isotopes and other trace elements may decrease signal stability, particularly for low-content isotopes like 207Pb, which in turn leads to an increased age uncertainty and dispersion for single analyses. However, the accuracy of the concordance age and weighted mean 206Pb/238U age of each sample, and the statistical results of all data points, are not affected significantly. Compared to TIMS ages, the discordance in these ages across all samples remains below 1.0% and 0.7%, respectively, meeting the requirements of U-Pb geological dating. Furthermore, the determination of key trace elements in zircon samples shows relative errors to recommended values of less than 10%. LA-SF-ICP-MS can accurately determine both zircon U-Pb ages and trace element contents simultaneously. The BRIEF REPORT is available for this paper at
http://www.ykcs.ac.cn/en/article/doi/10.15898/j.ykcs.202309110151 . -
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表 1 LA-SF-ICP-MS仪器工作条件
Table 1. Working conditions for LA-SF-ICP-MS instrument.
激光剥蚀系统(NWR 193UC) 高分辨电感耦合等离子体质谱仪(Element Ⅱ) 实验参数 工作条件 实验参数 工作条件 波长 193nm 射频功率 1200W 脉冲时间 15ns 冷却气(Ar)流速 16L/min 激光斑束 25μm 辅助气(Ar)流速 0.9L/min 激光频率 8Hz 样品气(Ar)流速 0.82L/min 能量密度 ～3.2J/cm2 分辨率 低 (M/ΔM=300) 载气流速(He) 0.8L/min 扫描模式 E-Scan 增敏气流速(N2) 1mL/min 扫描质量 29Si，49Ti，89Y，91Zr，139La，140Ce，141Pr，
146Nd，147Sm，151Eu，157Gd，159Tb，163Dy，
165Ho，166Er，169Tm，172Yb，175Lu，178Hf，
206Pb，207Pb，208Pb，232Th，238U剥蚀时间 40s 接收器模式 Both模式(Counting和Analog) 
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表 2 两种不同方法锆石U-Pb定年结果对比
Table 2. Zircon U-Pb dating results by LA-(SF)ICP-MS with two methods
标准
样品仅U-Pb定年方法 U-Pb定年+测定微量元素含量方法 206Pb/238U 207Pb/235U 谐和年龄
(Ma)206Pb/238U
加权平
均年龄
(Ma)206Pb/238U 207Pb/235U 谐和年龄
(Ma)206Pb/238U
加权平
均年龄
(Ma)年龄
(Ma)2σ RSD
(%)年龄
(Ma)2σ RSD
(%)年龄
(Ma)2σ RSD
(%)年龄
(Ma)2σ RSD
(%)91500 1045.3～1076.8 15.0～16.2 0.8 1047.7～1106.4 0.8～11.7 1.3 1065.9±2.4 1065.4±6.8 1045.7～1080.5 20.3～22.7 1.0 1044～1093 14.7～21.7 1.2 1063.3±2.4 1062.5±7.3 GJ-1 598.2～603.9 8.6～8.9 0.2 587.6～603.5 6.9～7.7 0.6 600.5±1.3 601.7±3.8 599～610 11.4～12.4 0.4 563～618 9.8～12.7 1.8 603.8±1.6 604.0±3.8 Tanz 556.3～568.1 8.3～8.6 0.5 554.6～569.4 6.9～7.3 0.8 563.2±1.3 564.6±3.7 550～570 10.9～11.9 0.8 546～577 9.1～11.5 1.6 559.5±1.7 562.7±4.2 SA01 525.0～539.6 7.9～9.6 0.6 527.8～537.5 7.8～9.3 0.5 532.9±1.5 533.2±3.8 526～542 10.1～12.1 0.8 519～548 10～17.2 1.4 533.8±2.0 534.5±4.7 Temora1 413.8～421.9 6.5～6.8 0.5 412.6～427.2 5.6～7.3 1.0 418.2±1.1 418.2±2.9 401～427 8.1～11.3 1.0 404～456 7～19.7 2.7 417.5±1.5 416.7±3.4 Plešovice 333.9～341.8 4.8～6.4 0.6 330.1～340.9 4.4～5.8 0.6 337.7±0.9 337.8±2.3 326～340 4.8～6.9 1.0 321～342 4.8～6.9 1.8 334.6±1.0 335.8±2.5 Qinghu 161.8～156.6 2.6～3.1 0.9 165.5～156.2 2.7～3.2 1.3 159.4±0.5 159.1±1.3 156.3～164.9 2.9～3.2 1.4 154.3～176.4 3.1～4.1 3.3 160.1±0.6 160.5±1.3
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表 3 LA-SF-ICP-MS锆石多元素同时分析微量元素定量结果
Table 3. Trace element results measured by LA-SF-ICP-MS, determining U-Pb and key trace elements simultaneously.
元素 检出限
(μg/g)NIST612 KL2-G 91500 SA01 GJ-1 Plešovice Qinghu Tanz Temora1 平均值
(μg/g)RSD
(%)SE
(%)平均值
(μg/g)RSD
(%)SE
(%)Si内标
(μg/g)Zr内标
(μg/g)文献值［48］
(μg/g)Si内标
(μg/g)Zr内标
(μg/g)文献值［35］
(μg/g)Ti 0.302 40.3 4.8 8.5 14053 1.0 8.4 5.9±2.5 5.1±2.8 6±1 12.1±3.49 11.2±1.08 12.1±0.3 3.6±1.57 87.8±21.4 17.2±3.78 15.1±2.68 12.4±1.97 Y 0.025 40.1 1.1 4.8 23.8 1.5 6.5 124±5.2 117±3 140±14 402±14.9 382±6.67 − 284±10.3 501±121 700±153 183±10.8 1063±307 La 0.020 36.8 1.4 2.2 12.1 1.2 8.0 0.03±0.03 0.03±0.04 0.006±0.003 0.104±0.02 0.096±0.03 0.108±0.02 ＜ 0.162±0.173 ＜ 0.02±0.006 0.072±0.027 Ce 0.017 38.3 1.1 0.3 30.0 1.4 7.3 2.3±0.08 2.1±0.14 2.6±0.3 16.8±0.566 15.4±0.464 17.8±1.1 14±0.6 2.99±1.35 10.3±1.77 7.27±0.429 3.67±0.687 Pr 0.013 38.1 1.1 0.7 4.3 1.6 6.9 0.03±0.02 0.02±0.01 0.024±0.015 0.615±0.043 0.586±0.037 0.67±0.04 0.034±0.008 0.251±0.203 0.245±0.112 0.05±0.01 0.184±0.076 Nd 0.056 36.8 1.7 3.6 19.7 1.9 8.9 0.23±0.05 0.2±0.09 0.24±0.04 7.89±0.482 7.94±0.328 8.94±0.51 0.655±0.19 2.5±1.21 1.59±0.691 0.963±0.118 2.64±1.04 Sm 0.045 38.9 1.6 3.2 5.4 2.6 2.6 0.44±0.06 0.41±0.1 0.5±0.08 8.39±0.307 9.31±0.436 10.1±0.47 1.61±0.29 4.05±1.32 3.73±1.4 2.76±0.383 4.38±1.71 Eu 0.024 36.4 0.8 2.4 1.8 2.7 7.2 0.25±0.02 0.23±0.04 0.24±0.03 5.04±0.171 5.34±0.136 6.04±0.36 1.16±0.129 1.08±0.418 0.389±0.177 1.52±0.197 0.951±0.315 Gd 0.073 38.6 2.6 3.4 5.6 4.8 5.9 2.2±0.08 2.1±0.19 2.2±0.3 23±1.06 23.7±0.777 25.1±1.5 7.48±0.53 14.4±4.42 14.8±4.66 11.6±1.33 20.8±7.31 Tb 0.017 38.1 1.0 1.4 0.8 4.1 9.0 0.74±0.04 0.74±0.05 0.86±0.07 5.34±0.271 5.4±0.15 5.94±0.36 2.15±0.153 5.24±1.46 5.5±1.51 2.91±0.333 7.32±2.56 Dy 0.062 37.3 1.7 5.0 4.7 3.4 9.6 10±0.42 10±0.48 12±1 49.4±0.869 50.4±1.5 53.3±3 22.2±0.936 58.3±15.6 65.8±16.7 25.2±2.23 89.1±30.5 Ho 0.011 39.5 1.3 3.1 0.9 3.2 4.2 4.1±0.14 4.1±0.14 4.8±0.4 14±0.421 13.7±0.244 14.9±0.9 7.55±0.245 15.6±3.87 23.1±5.42 6.17±0.382 34.4±10.7 Er 0.041 39.6 2.1 4.2 2.5 4.6 3.3 23±0.86 22±0.76 25±3 55.7±2.37 52.2±1.32 56.2±2.1 32.9±1.4 56.1±13.2 104±21.6 21.2±1.25 162±45 Tm 0.009 38.7 1.0 5.1 0.4 5.6 7.0 6.7±0.21 6±0.17 6.9±0.4 10.1±0.478 11±0.236 11.3±0.7 7.1±0.359 10.2±2.45 25±5.18 3.79±0.254 34.4±8.54 Yb 0.071 40.1 2.5 2.2 2.0 4.1 3.2 78±1.9 71±2.2 74±4 87.7±3.24 105±2.71 107±4.6 72.2±4.3 78.9±21.2 245±46.6 31.3±3.03 334±76.3 Lu 0.011 38.0 1.3 2.7 0.3 5.5 5.4 12±0.5 9.6±0.26 13±1 16.5±0.588 13.1±0.297 15.4±0.7 14.5±1.15 8.27±2.14 40.5±6.4 4.02±0.399 66.4±14 Hf 0.043 37.9 1.3 3.2 3.8 4.2 4.2 6027±325 5424±85 5900±300 9650±610 8647±151 10019±579 7220±297 10420±546 10027±359 10925±617 8252±538 Pb 0.015 38.9 1.2 0.8 1.9 3.0 6.5 15±0.41 13±0.36 15±2 13±0.4 11.2±0.591 22.5±9.7 43.7±2.28 53±18.2 20.7±5.23 35.2±2.18 13.2±6.16 Th 0.004 39.1 1.1 3.6 1.0 3.3 4.1 25±0.8 24±0.55 30±3 139±4.44 128±2.18 140±11 7.59±0.366 97.8±42.8 357±93 71.2±7.87 72.6±33.8 U 0.002 37.8 1.2 1.1 0.6 1.5 17.5 71±2.4 67±2.2 80±8 105±3.63 94.4±4.86 114±13 430±18 972±345 657±159 366±15.9 169±78.6 注：“—”表示文献未报道；“＜”表示测试数据低于方法检出限。
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