Effect of Gas Flow Rates in Laser Ablation System on Accuracy and Precision of Zircon U-Pb Dating Analysis by LA-ICP-MS
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摘要:
锆石U-Pb定年精度一直是激光剥蚀-电感耦合等离子体质谱(LA-ICP-MS)分析方法的研究重点,激光剥蚀系统气体流速变化影响ICP-MS信号稳定性而影响锆石U-Pb定年精度,但影响程度和机制尚不清楚。本文以锆石标样91500及Plešovice为研究对象,采用LA-ICP-MS开展了载气和补偿气流速变化对锆石U-Pb定年结果准确度和精密度影响的研究工作。实验结果表明:固定补偿气Ar流速为1.0L/min,而增大载气He流速(0.2~1.2L/min),锆石标样91500的206Pb/238U加权平均年龄增大(1002.0±10.4Ma~1083.0±6.8Ma,1σ),即样品气溶胶运输效率影响锆石U-Pb定年分析准确度,但He流速高于0.8L/min时由于大颗粒气溶胶引入使ICP-MS信号波动性和氧化物增加,导致锆石U-Pb定年分析精度降低。进一步以Plešovice锆石为例分析发现,Ar/He流速组合为0.95/0.8、0.8/0.8和0.8/0.6L/min时206Pb/238U加权平均年龄无显著性差异,但Ar/He流速均为0.8L/min时1σ单点分析相对偏差最小(1.4%),即通过控制载气和补偿气流速组合,优化样品气溶胶运输效率可提高LA-ICP-MS锆石U-Pb定年精度。在本实验条件下,0.8L/min为载气和补偿气流速最佳取值。
要点(1) 分析了载气(He)和补偿气(Ar)流速变化对LA-ICP-MS锆石U-Pb定年结果的影响。
(2) He和Ar流速比值为1时得到的206Pb/238U年龄谐和度值最高(91%~96%),本实验条件下He、Ar最佳流速为0.8L/min。
(3) 优化气溶胶运输效率可使锆石定年准确度提高6%及精确度提高3.4倍。
HIGHLIGHTS(1) The effect of carrier gas (He) and make-up gas (Ar) flow rate on zircon U-Pb dating analysis by LA-ICP-MS was studied.
(2) A ratio of 1 for He to Ar with the exact value of 0.8L/min yielded the highest 206Pb/238U age concordance values (91%-96%).
(3) Zircon dating analysis can be improved via optimizing sample aerosol transportation efficiency, with accuracy enhanced by 6% and precision increased by 3.4 times.
Abstract:BACKGROUNDDespite zircon U-Pb dating analysis by LA-ICP-MS receiving wide acceptance, it remains a challenge to obtain results with high accuracy and precision. It is known that gas flow rates of LA system can affect the signal stability of ICP-MS and thus result in impacts on analytical uncertainty of zircon U-Pb dating. However, the exact effects and mechanism of gas flow rates on zircon U-Pb dating analysis are still unclear.
OBJECTIVESTo thoroughly understand the influence of gas flow rates on the analytical uncertainty of zircon U-Pb dating, and to provide valuable information to propose a reliable and robust LA-ICP-MS approach for zircon U-Pb dating analysis.
METHODSBy applying zircon standard samples of Harvard 91500 and Plešovice as researching subjects, ICP-MS connected to a 193nm nanosecond laser ablation system was used to investigate the influence of gas flow rate settings on accuracy and precision of U-Pb dating analysis. RESULTS: With fixed make-up gas (Ar) of 1.0L/min, the average 206Pb/238U ages of Harvard 91500 were found to increase from 1002.0±10.4Ma (1σ) to 1083.0±6.8Ma (1σ) with increasing carrier gas (He) from 0.2 to 1.2L/min. Thus, it was clear that the sample aerosol transportation efficiency can greatly affect the analytical accuracy of zircon U-Pb dating. Furthermore, when the He flow rate was higher than 0.8L/min, the analytical accuracy and precision of zircon U-Pb dating decreased due to the increased signal intensity oscillations and formation of oxides from the introduction of large particles of sample aerosols. The comparison of the data of Plešovice obtained under 0.95/0.8, 0.80/0.8 and 0.8/0.6L/min for He/Ar gas flow rate patterns indicated that there were no significant differences in U/Pb weighted average age. However, the relative deviation of 1σ single-point analysis was the smallest (1.4%) when the Ar and He flow rates were both 0.8L/min.
CONCLUSIONSThe analytical accuracy and precision of zircon U-Pb dating by LA-ICP-MS can be improved by optimizing the gas flow rate setting of carrier gas and make-up gas, and highly recommending 0.8L/min of both Ar and He.
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激光拉曼光谱分析作为一种非破坏性的分析方法,可以快速方便地对单个包裹体进行定性、半定量分析,现已成为流体包裹体研究的基本工具之一[1, 2]。近年来随着仪器精度的提高以及科研的需要,激光拉曼针对包裹体的定量分析的研究发展迅速。定量分析主要涉及包裹体的气[3, 4, 5, 6, 7]、液相[8, 9, 10, 11, 12, 13, 14, 15]以及同位素[16, 17, 18, 19, 20]等化学组成分析以及包裹体的内压[21, 22, 23, 24]、密度[25, 26]、有机质热成熟度[27, 28]等物理参数的获取。而作为包裹体重要成分的各种无机和有机气相组分,由于其一般具有较强的拉曼活性,在拉曼谱图上表现出尖锐而特征的谱峰,因此被认为是进行拉曼定量分析的重要研究对象[29]。国内外学者对包裹体中常见的C-H-O-N-S体系的气相组分开展了比较广泛的定量研究[3, 4, 5, 6, 7],取得了显著的成果。由于气相组分的拉曼定量分析与分子性质、温度、压力、仪器性能等诸多因素有关[3, 4, 29],造成前人结果存在比较明显的差异,难以相互借用,如李维华等[5]与Wopenka等[30]测定的SO2的定量因子有近5倍的差别。因此在进行气相成分的定量分析之前,需要利用一系列混合气体标样对仪器进行标定。前人一般使用商用钢瓶装混合气进行仪器标定[3, 4, 5],虽然上述标样易于购置、配比准确,却存在气体组成单一无法调节、费用高、需要经常更换钢瓶等缺点。如按10%的梯度对10%~90%的两种气体的混合物进行标定,需要购置9瓶钢瓶气轮换使用,并且钢瓶气一定的使用期限,超过期限需要重新购置。针对上述不足,本文提出了一种在线配置不同浓度和压力条件下混合气体标样的方法,以实现快速准确地对激光拉曼探针进行标定及测定气体拉曼定量因子的研究目的。
1. 在线标样制备装置和在线标样的制备
为了实现混合气体标样的制备,本次研究搭建了一套在线标样制备装置(图 1)。该装置可以同时接入三路钢瓶气体,每路钢瓶气分别连接一个减压阀用于控制气体的输出压力;利用带有刻度和活塞的体积转移器量取实验所需体积的气体并将量取的气体注入高压容器中进行混合;增压泵用于对高压容器中的混合气体进行增压;真空泵用于对装置进行抽真空;装置的输出端与石英毛细管相连接;管路中安装有真空表以及压力表用于监控系统的真空度以及线路中气体的压力值;线路中还设有两个排气孔用于排气及管路清洗。
实验所用的钢瓶气为高纯气体,浓度≥99.999%;毛细管规格为内径0.1 mm,外径0.3 mm,表面涂有一层聚酰亚胺保护膜,厚度约0.025 mm(美国Polymicro Technologies公司)。激光拉曼分析的仪器为Renishaw Invia型激光拉曼光谱仪(英国Renishaw公司),使用Ar+激光器,波长为514 nm,光谱分辨率为2 cm-1。
在线混合气体标样制备的实验步骤如下。
(1) 打开阀门1~6、8、10,关闭阀门7、9、11,打开真空泵对管路、体积转移器及高压容器抽真空,待真空表读数≤10Pa时,关闭真空泵。
(2) 关闭阀门2~4、6、8、10,打开气瓶1的减压阀并调节至实验所需压力值,用体积转移器量取实验所需气体体积。
(3) 关闭阀门1、5、气瓶1的减压阀,打开阀门6、8,将体积转移器中的气体转移至高压容器中。
(4) 关闭阀门8,打开阀门1~6、8、10,对系统抽真空,待真空表读数≤10Pa时,关闭真空泵。
(5) 重复步骤(2)~(4),量取实验所需体积及压力条件下的气体2并注入到高压容器中,使气体1和2充分混合。
(6) 关闭阀门6,打开阀门8、11,利用高压容器中的混合气体对管路进行清洗。
(7) 关闭阀门11,打开阀门9,打开电动增压泵,对高压容器中的气体进行增压,待达到实验所需的气体压力时,停止增压并进行激光拉曼分析,然后继续增压至下一个压力点并进行拉曼分析。
2. 结果与讨论
2.1 在线样品准确性验证
为了验证制样方法的准确性及重复性,将本研究制备的70% N2+30% CO2的在线标样与购置于大连大特气体公司生产的同等浓度的商用标样,在10 MPa条件下分别进行了激光拉曼分析。结果表明,本次研究制备的混合气体与商用钢瓶装标样具有相似的峰形(图 2)。利用英国Renishaw公司出品的Wire3.0软件对上述拉曼谱图进行了分析,结果表明本方法制备的混合气体与商用标样具有相似的CO2与N2的相对峰高以及相对峰面积值,其相对误差小于4%,并具有较好的重现性,能够满足实验要求。
2.2 CH4及CO2相对拉曼定量因子的测定
在测定单个包裹体气体组成方面,国内外多沿用“相对拉曼定量因子”的方法,即通常将N2的定量因子定为1.00,其他气体与N2进行比较,得到相对拉曼定量因子[3, 4]。本次研究分别对拉曼峰面积及峰高计算了相对拉曼定量因子,具体公式如下:
式中,Ag为气体g的拉曼峰面积;AN2为N2的拉曼峰面积;Cg为气体g的摩尔分数;CN2为N2的摩尔分数;Hg为气体g的拉曼峰高;HN2为N2的拉曼峰高;Fgr代表以峰面积为参考值时气体g相对于N2的拉曼定量因子;Ggr代表以峰高为参考值时气体g相对于N2的拉曼定量因子。
为了测定CO2以及CH4的相对拉曼定量因子,在室温、5 MPa和10 MPa压力条件下,分别制备了N2摩尔分数为30%、50%和70%的N2-CO2混合气体标样以及N2-CH4混合气体标样。
在上述标样的激光拉曼谱图(图 3)中能清晰地辨识出N2、CO2以及CH4的拉曼特征峰。气体的拉曼峰强度随浓度以及压力的增加而增加,信噪比随着压力由5 MPa增加到10 MPa增大约一倍。
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虽然CO2在1286 cm-1附近以及1386 cm-1附近出现两个峰值,但是由于1286 cm-1附近的峰强度要小于1386 cm-1附近峰强度。因此本文仅针对CO2在1386 cm-1附近的峰计算了相对拉曼定量因子。
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求得CH4和CO2相对拉曼定量因子之后,便可以对包裹体中CH4和CO2的相对含量进行计算,具体计算公式如下:
3. 地质样品应用
选取四川金沙岩孔剖面,震旦系的藻云岩样品进行应用研究。该样品溶洞发育,被后期亮晶白云石充填。溶洞充填的亮晶白云石中发育气液两相盐水包裹体。选取个体较大并且靠近样品表面的包裹体,对其气泡进行激光拉曼分析,结果表明包裹体的气泡主要由CH4和CO2组成(图 6)。
利用wire3.0对图 6中两个包裹体的拉曼相关参数进行求解,并分别利用公式(3) 和(4) 对包裹体a和b中的CH4和CO2摩尔浓度进行了计算,得到包裹体中CH4的摩尔分数为27.60%~31.63%,CO2的摩尔分数为68.37%~72.40%(表 1)。上述结果表明,利用本文所求得的拉曼定量因子F和G所得到计算的结果基本一致(两者的绝对偏差在2.5%以内);包裹体a和b气相组成较接近,可能为同期捕获的产物。
表 1 包裹体样品分析结果Table 1. The analytical composition of gas in fluid inclusions包裹体 ACO2 HCO2 ACH4 HCH4 CCH4(%) CCO2(%) 据公式(3) 据公式(4) 据公式(3) 据公式(4) 包裹体a 3461.54 594.541 17891.2 4115.24 31.63 31.25 68.37 68.75 包裹体b 3137.87 732.481 14694.8 4251.27 29.54 27.60 70.46 72.40 4. 结语
本文利用自主搭建的在线标样制备装置,对N2-CH4以及N2-CO2进行在线混合增压,制备了N2摩尔浓度为30%、50%和70%,压力为5 MPa和10 MPa的N2-CH4以及N2-CO2混合气体在线标样。通过与商用混合钢瓶气体标样对比表明,该方法所使用的装置操作简单,制备的混合气体具有较高的准确性及重现性,能够方便、准确地对拉曼光谱仪进行标定,实现了不同压力和浓度条件下气体的相对拉曼定量因子的测定。通过对CH4及CO2的相对定量因子测定表明,气体压力在5~10 MPa的范围时,定量因子不受压力变化的影响,为固定值。地质样品应用表明,本方法可以方便、灵活、准确地按任意比例将两瓶及两瓶以上纯气体钢瓶样品进行混合及增压,弥补了商用钢瓶装混合气体标样费用高、气体组成单一固定等不足。
由于本次研究仅在5 MPa和10 MPa两个压力点进行了分析,因此对于相对定量因子在 < 5 MPa及 > 10 MPa压力条件下的变化规律还有待于进一步研究。另外由于缺乏已知气体组成的人工合成包裹体标样,对于本方法在包裹体应用中的误差范围还有待于进一步研究。
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图 1 不同气体流速条件下91500锆石U-Pb加权平均年龄分析结果
灰色实线、白色虚线、深灰色实线、黄色实线、灰色虚线、白色实线和黄色虚线分别为Ar//He流速组合为1.0/0.2、1.0/0.4、1.0/0.8、1.0/1.2、0.6/0.6、0.8/0.8和1.0/1.0L/min得到的年龄结果。
Figure 1. Weighted average U-Pb ages of zircon 91500 under different gas flow rates. The Ar/He gas flow rate settings for the gray-solid, white-dash, deep gray-solid, yellow-solid, gray-dash, white-dash and yellow-dash are 1.0/0.2, 1.0/0.4, 1.0/0.8, 1.0/1.2, 0.6/0.6, 0.8/0.8 and 1.0/1.0L/min, respectively
图 2 气体流速对91500锆石U-Pb加权平均年龄的单点分析误差影响
Figure 2. Effect of gas flow rate on the analytical deviation for U-Pb age of zircon 91500. The 1σ analytical deviations of each group are from a complete assay sequence, which includes 4-5 zircon 91500 as unknown samples bracketed by 2 zircon 91500 as the external calibration standards
表 1 LA-ICP-MS工作条件
Table 1 Working conditions for LA-ICP-MS
ICP-MS工作条件 LA工作条件 仪器型号 Agilent 7700x 仪器型号 Analyte Excite 193 RF功率 1450W 波长 193nm 等离子体气(Ar)流速 15L/min 脉冲宽度 5ns 辅助气(Ar)流速 1.0L/min 频率 5Hz 补偿气(Ar)流速 0.8L/min 激光能量密度 5.9J/cm2 检测器模式 双模式 束斑直径 35μm 采样锥/截取锥 镍锥,1.0/0.45mm 采样模式 单点剥蚀 采样深度 5.0mm 脉冲数/单点 200 积分时间 40s 载气(He) Main cell:0.6L/min 数据采集模式 TRA 流速 Inner cup:0.2L/min 注:载气和补偿气流速值为默认值,条件优化时可调整。 表 2 补偿气Ar和载气He不同流速条件下锆石91500年龄LA-ICP-MS分析结果
Table 2 Results of zircon 91500 by LA-ICP-MS under different flow rates of make-up gas Ar and carrier gas He
测点 Ar气流速(L/min) He气流速(L/min) 同位素比值 同位素年龄(Ma) 谐和度(%) 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ 91500-1 1.0 0.2 0.08354 0.00524 1.94219 0.12703 0.16736 0.00628 1283.34 122.22 1095.75 43.87 997.54 34.66 90 91500-2 0.08302 0.00489 1.95625 0.11654 0.17032 0.00623 1270.05 115.28 1100.60 40.05 1013.88 34.29 91 91500-3 0.07787 0.00486 1.81532 0.13351 0.16550 0.00628 1143.53 124.08 1051.00 48.19 987.26 34.73 93 91500-4 0.07936 0.00529 1.87112 0.12704 0.16947 0.00686 1181.17 133.33 1070.93 44.96 1009.21 37.84 94 91500-5 1.0 0.4 0.07405 0.00490 1.83186 0.12146 0.18207 0.00705 1042.60 134.42 1056.95 43.58 1078.27 38.43 98 91500-6 0.06808 0.00403 1.65237 0.10058 0.17523 0.00489 872.22 124.07 990.46 38.52 1040.86 26.84 95 91500-7 0.06937 0.00411 1.81117 0.11908 0.18546 0.00591 909.26 122.22 1049.50 43.04 1096.76 32.16 95 91500-8 0.06601 0.00440 1.59587 0.10133 0.17940 0.00600 805.56 139.65 968.60 39.66 1063.68 32.82 90 91500-9 1.0 0.8 0.07678 0.00369 1.87797 0.09634 0.17835 0.00451 1116.67 96.30 1073.35 34.00 1057.94 24.69 98 91500-10 0.07621 0.00372 1.92174 0.09133 0.18429 0.00442 1101.85 97.84 1088.67 31.75 1090.38 24.05 99 91500-11 0.07568 .00352 1.88231 0.09385 0.17939 0.00435 1087.04 93.06 1074.88 33.07 1063.67 23.80 98 91500-12 0.06916 0.00352 1.72129 0.08920 0.18076 0.00437 903.39 105.56 1016.51 33.29 1071.11 23.84 94 91500-26 1.0 1.2 0.06804 0.00370 1.72687 0.10170 0.18349 0.00602 870.05 117.59 1018.58 37.89 1086.02 32.79 93 91500-27 0.07337 0.00383 1.85591 0.10418 0.18368 0.00513 1033.34 106.64 1065.53 37.06 1087.03 27.95 98 91500-28 0.07600 0.00419 1.88984 0.10714 0.18083 0.00516 1094.45 143.06 1077.53 37.66 1071.53 28.19 99 91500-29 0.07631 0.00404 1.91539 0.09830 0.18400 0.00526 1103.39 105.56 1086.46 34.25 1088.81 28.66 99 91500-30 0.06574 0.00360 1.67245 0.09916 0.18323 0.00533 798.15 114.81 998.12 37.69 1084.62 29.06 91 表 3 补偿气Ar和载气He相同流速条件下锆石91500年龄LA-ICP-MS分析结果
Table 3 Results of zircon 91500 by LA-ICP-MS under equal flow rates of make-up Ar and carrier gas He
测点 Ar气流速(L/min) He气流速(L/min) 同位素比值 同位素年龄(Ma) 谐和度(%) 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ 91500-17 0.6 0.6 0.08128 0.00847 2.00782 0.20392 0.18118 0.00618 1227.78 205.56 1118.16 68.95 1073.43 33.74 95 91500-18 0.06985 0.00686 1.67127 0.16873 0.17916 0.00576 924.07 206.48 997.67 64.22 1062.36 31.50 93 91500-19 0.08061 0.00751 1.97547 0.19369 0.18117 0.00497 1212.96 184.11 1107.17 66.19 1073.35 27.15 96 91500-20 0.05234 0.00585 1.22046 0.14060 0.17705 0.00510 301.91 283.30 809.99 64.38 1050.84 27.92 74 91500-13 0.8 0.8 0.07169 0.00400 1.80023 0.10036 0.18115 0.00310 977.47 114.05 1045.54 36.41 1073.27 16.94 97 91500-14 0.07139 0.00371 1.78865 0.08726 0.18297 0.00374 968.52 106.64 1041.33 31.78 1083.18 20.41 96 91500-15 0.07282 0.00442 1.78181 0.09366 0.18039 0.00364 1009.26 124.08 1038.84 34.20 1069.09 19.87 97 91500-16 0.07160 0.00464 1.78184 0.10613 0.18258 0.00390 975.93 132.57 1038.85 38.76 1081.06 21.27 96 91500-21 1.0 1.0 0.07806 0.00412 1.89970 0.10648 0.17703 0.00655 1150.01 105.09 1080.99 37.30 1050.70 35.88 97 91500-22 0.07359 0.00397 1.92183 0.11762 0.19014 0.00823 1031.49 113.89 1088.70 40.90 1122.11 44.55 96 91500-23 0.07296 0.00362 1.76294 0.08237 0.17623 0.00554 1012.96 100.46 1031.93 30.28 1046.36 30.36 98 91500-24 0.06455 0.00350 1.67356 0.09517 0.18578 0.00648 761.12 113.72 998.54 36.16 1098.49 35.23 90 91500-25 0.07517 0.00432 1.82203 0.10655 0.17604 0.00674 1072.23 115.28 1053.41 38.35 1045.30 36.93 99 表 4 补偿气Ar和载气He不同流速组合条件下Plešovice锆石年龄LA-ICP-MS分析结果
Table 4 Results of Plešovice by LA-ICP-MS under different flow rate setings of make-up gas Ar and carrier gas He
测点 Ar气流速(L/min) He气流速(L/min) 同位素比值 同位素年龄(Ma) 谐和度(%) 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ 207Pb/206Pb 1σ 207Pb/235U 1σ 206Pb/238U 1σ PL-1 0.95 0.8 0.05495 0.00228 0.40140 0.01711 0.05284 0.00099 409.31 89.81 342.67 12.40 331.93 6.07 96 PL-2 0.05182 0.00189 0.38639 0.01529 0.05384 0.00104 275.99 87.95 331.73 11.20 338.06 6.38 98 PL-3 0.05536 0.00229 0.40526 0.01687 0.05312 0.00100 427.83 92.58 345.46 12.19 333.63 6.12 96 PL-4 0.06113 0.00219 0.47801 0.01731 0.05690 0.00112 642.61 77.77 396.71 11.89 356.77 6.83 89 PL-5 0.05457 0.00214 0.41876 0.01747 0.05560 0.00112 394.50 87.03 355.16 12.51 348.79 6.86 98 PL-6 0.8 0.8 0.05565 0.00257 0.41391 0.01841 0.05350 0.00075 438.94 103.69 351.69 13.22 335.95 4.56 95 PL-7 0.05852 0.00252 0.45879 0.01993 0.05630 0.00082 550.04 92.58 383.42 13.87 353.08 5.01 91 PL-8 0.05507 0.00234 0.40524 0.01615 0.05316 0.00071 416.72 94.44 345.44 11.67 333.88 4.33 96 PL-9 0.05542 0.00234 0.40653 0.01682 0.05283 0.00077 427.83 94.44 346.37 12.14 331.85 4.68 95 PL-10 0.8 0.6 0.06033 0.00260 0.46339 0.02002 0.05556 0.00095 616.69 92.58 386.61 13.89 348.55 5.82 89 PL-11 0.05084 0.00254 0.37078 0.01836 0.05296 0.00092 235.25 112.02 320.23 13.60 332.66 5.62 96 PL-12 0.04740 0.00259 0.35224 0.01939 0.05397 0.00092 77.87 116.66 306.41 14.56 338.83 5.64 89 PL-13 0.04869 0.00248 0.36907 0.01863 0.05526 0.00084 131.57 123.13 318.97 13.82 346.73 5.13 91 -
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