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。
Abstract:BACKGROUND Despite 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.
OBJECTIVES To 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.
METHODS By 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.
CONCLUSIONS The 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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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。 
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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
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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
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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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