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摘要:
氧同位素分析能够为岩石、热液及矿床形成演化提供重要的成因信息，是岩石学与矿床学研究的强有力工具。二次离子质谱仪(SIMS)以其独特的微区原位优势，广泛应用于锆石等矿物氧同位素分析，往代型号SHRIMP存在三维机械样品台在移动过程中发热甚至放气破坏样品腔真空的风险。为了维持样品腔稳定的高真空，保证氧同位素测试精度，本次研究首次利用升级压电陶瓷驱动高真空样品台的第五代高灵敏度、高分辨率二次离子质谱仪(SHRIMP Ⅴ)，建立了氧同位素微区原位分析测试方法。在一次离子强度为3nA，电子枪能量为−1.9keV，束斑大小为25μm，入射狭缝宽度为120μm，18O−和16O−两个接收器狭缝宽度均为300μm的条件下，用锆石标样Temora 2和Qinghu对系统进行调试，获得16O信号强度约为1.2×109cps，并对标样R33、FC1和Tanz进行了测试。结果表明，标样氧同位素δ18O分析结果与其参考值在误差范围内一致，δ18O单点内在分析精度优于0.30‰(2SE)，外在精度优于0.50‰(2SD)，测试精度整体与国内外原有SHRIMP相当，验证了仪器准确度、精密度和稳定性。升级高真空样品台后，SHRIMP Ⅴ样品腔真空度优于2.5×10−8torr(原有SHRIMP为4.0×10−8torr)，进一步提高了极限真空及重复定位能力和分辨力，更有利于氧等稳定同位素分析，并为今后传统无水矿物水含量的测试提供了可能。
Abstract:Oxygen isotope analysis can provide important genetic information for the formation and evolution of rocks, hydrothermal fluids, and mineral deposits. It is a powerful tool for petrology and mineral deposits research. Secondary ion mass spectrometry (SIMS) is widely used for oxygen isotopes analysis of accessory minerals such as zircon with its advantage of its unique in situ microanalysis. However, since the advent of SHRIMP, there has always been a problem of sample chamber vacuum damage caused by heating and deflation during the movement of the sample stage. In order to maintain a stable high level of vacuum in the sample chamber and ensure the accuracy of oxygen isotope testing, an in situ microanalytical method of oxygen isotopes in zircon was established by using the fifth generation of sensitive high resolution ion microprobe (SHRIMP Ⅴ) with an upgraded piezoceramics driven high vacuum sample stage. The instrument conditions include: the primary ion intensity of 3nA, electron gun energy of −1.9keV, beam spot size of 25μm, source slit width of 120μm, and slit widths of both 18O− and 16O− receivers of 300μm. The system was adjusted by using zircon standard samples Temora 2 and Qinghu, and the obtained signal intensity of 16O was 1.2×109cps. The standard samples R33, FC1 and Tanz were also tested. The results showed that the analysis values of δ18O for zircon standard samples were consistent with the reference values within the error range. Internal analysis accuracy was better than 0.30‰ (2SE), and the external accuracy was better than 0.50‰ (2SD). The overall testing accuracy of zircon oxygen isotope analysis by SHRIMP Ⅴ was comparable to that of existing SHRIMP series instruments in China and abroad, which verified the accuracy, precision and stability of SHRIMP Ⅴ. After upgrading the high vacuum platform, the sample chamber vacuum stability of the SHRIMP Ⅴ was maintained within 2.5×10−8torr (original SHRIMP is 4.0×10−8torr), which further improves the ultimate vacuum, repeat positioning ability and resolution. Besides, it is more conducive to the analysis of stable isotopes such as oxygen and provides the possibility for the future testing of water content in traditional anhydrous minerals.
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Key words:
- oxygen isotopes /
- SHRIMP Ⅴ /
- high vacuum sample stage /
- zircon /
- in situ microanalytical method
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表 1 SHRIMP Ⅴ样品腔真空统计
Table 1. The vacuum statistics of SHRIMP V sample chamber
SHRIMP Ⅴ
运行时间样品腔真空
(×10−8torr)SHRIMP Ⅴ
运行时间样品腔真空
(×10−8torr)202306 2.1～2.5 202401 1.5～1.7 202307 1.9～2.4 202402 1.5～2.1 202308 1.8～2.3 202403 1.2～2.5 202309 1.7～2.6 202404 1.2～2.7 202310 1.8～2.3 202405 1.5～2.1 202311 1.7～2.6 202406 1.6～2.2 202312 1.6～2.6 202407 1.2～2.6 202408 1.4～2.7 
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表 2 第1号靶和第2号靶SHRIMP Ⅴ 锆石氧同位素分析结果
Table 2. Results of zircon oxygen isotope analysis on target No.1 and No.2 by SHRIMP Ⅴ.
第1号靶第一组 测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)Temora 2-1 8.38 0.26 R33-1 5.78 0.27 FC1-1 5.51 0.18 Temora 2-2 8.21 0.31 R33-2 5.71 0.11 FC1-2 5.67 0.22 Temora 2-3 8.01 0.13 R33-3 5.39 0.12 FC1-3 5.71 0.26 Temora 2-4 7.83 0.32 R33-4 5.84 0.23 FC1-4 5.86 0.27 Temora 2-5 8.21 0.16 R33-5 5.48 0.09 FC1-5 5.65 0.32 Temora 2-6 8.48 0.20 R33-6 5.57 0.29 FC1-6 5.83 0.28 Temora 2-7 8.18 0.25 R33-7 5.61 0.14 FC1-7 5.61 0.17 Temora 2-8 8.39 0.29 R33-8 5.54 0.10 FC1-8 5.65 0.25 Temora 2-9 8.00 0.27 R33-9 4.74 0.26 FC1-9 5.77 0.20 Temora 2-10 8.12 0.20 R33-10 5.95 0.18 FC1-10 5.68 0.24 Temora 2-11 8.24 0.12 R33-11 5.87 0.20 FC1-11 5.61 0.18 Temora 2-12 8.51 0.18 R33-12 5.62 0.23 FC1-12 5.87 0.25 Temora 2-13 8.21 0.23 R33-13 5.37 0.24 FC1-13 5.78 0.24 Temora 2-14 8.01 0.24 R33-14 6.15 0.32 FC1-14 5.59 0.26 Temora 2-15 8.02 0.18 R33-15 5.63 0.26 FC1-15 5.81 0.32 第1号靶第二组 测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)Temora 2-1 8.09 0.22 R33-1 5.81 0.33 FC1-1 5.85 0.23 Temora 2-2 8.40 0.33 R33-2 5.29 0.22 FC1-2 5.73 0.26 Temora 2-3 8.08 0.22 R33-3 5.57 0.15 FC1-3 5.77 0.16 Temora 2-4 8.62 0.27 R33-4 5.31 0.20 FC1-4 6.21 0.41 Temora 2-5 8.30 0.19 R33-5 5.20 0.19 FC1-5 5.98 0.11 Temora 2-6 7.93 0.14 R33-6 5.22 0.23 FC1-6 5.94 0.19 Temora 2-7 8.19 0.17 R33-7 5.24 0.22 FC1-7 5.62 0.09 Temora 2-8 7.97 0.32 R33-8 5.40 0.26 FC1-8 5.48 0.14 Temora 2-9 8.31 0.13 R33-9 5.55 0.07 FC1-9 5.82 0.19 Temora 2-10 8.14 0.19 R33-10 5.09 0.17 FC1-10 5.86 0.14 Temora 2-11 8.00 0.32 R33-11 5.47 0.18 FC1-11 5.57 0.26 Temora 2-12 8.29 0.17 R33-12 5.68 0.26 FC1-12 5.72 0.17 Temora 2-13 8.65 0.35 R33-13 5.89 0.18 FC1-13 5.58 0.12 Temora 2-14 8.24 0.21 R33-14 5.74 0.10 FC1-14 5.65 0.25 Temora 2-15 8.40 0.18 R33-15 5.21 0.17 FC1-15 5.85 0.25 Temora 2-16 8.50 0.12 R33-16 6.02 0.20 FC1-16 5.92 0.25 Temora 2-17 8.41 0.14 R33-17 5.83 0.13 FC1-17 5.59 0.14 Temora 2-18 7.91 0.15 R33-18 5.83 0.31 FC1-18 5.88 0.22 Temora 2-19 7.81 0.07 R33-19 5.99 0.23 FC1-19 5.55 0.14 Temora 2-20 8.33 0.27 R33-20 5.64 0.10 FC1-20 5.53 0.23 第2号靶 测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)测试点号 δ18O
(‰)2SE
(‰)Qinghu-1 5.68 0.15 Qinghu-15 5.55 0.23 Tanz-9 6.37 0.11 Qinghu-2 5.20 0.08 Qinghu-16 5.52 0.25 Tanz-10 6.63 0.29 Qinghu-3 5.20 0.12 Qinghu-17 5.52 0.22 Tanz-11 6.37 0.08 Qinghu-4 5.77 0.28 Qinghu-18 5.62 0.32 Tanz-12 6.42 0.16 Qinghu-5 5.63 0.13 Qinghu-19 5.43 0.14 Tanz-13 6.47 0.17 Qinghu-6 5.15 0.24 Qinghu-20 5.26 0.07 Tanz-14 6.55 0.11 Qinghu-7 5.39 0.13 Tanz-1 6.63 0.11 Tanz-15 6.56 0.19 Qinghu-8 5.50 0.15 Tanz-2 6.49 0.23 Tanz-16 6.68 0.32 Qinghu-9 5.40 0.27 Tanz-3 6.60 0.16 Tanz-17 6.52 0.12 Qinghu-10 5.24 0.26 Tanz-4 6.38 0.21 Tanz-18 6.33 0.12 Qinghu-11 5.20 0.11 Tanz-5 6.18 0.12 Tanz-19 6.75 0.20 Qinghu-12 5.49 0.18 Tanz-6 6.32 0.50 Tanz-20 6.72 0.20 Qinghu-13 5.30 0.16 Tanz-7 6.56 0.29 Qinghu-14 5.69 0.15 Tanz-8 6.73 0.22 注：δ18O=[(18O/16OSample)/(18O/16OVSMOW)－1]×1000‰，18O/16OVSMOW＝0.0020052。
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