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摘要:
金红石电子探针微量元素分析一般以人工合成的氧化物来作为监测标样，尚较缺乏对金红石标样进行系统地测试分析。本文运用CAMECA SXFive电子探针对金红石标样R10进行微量元素分析，根据金红石中主要微量元素在地质学中的应用，本次共分析了Al、Si、Ti、Fe、Cr、Zr、V、Nb、Ta等9个元素，Ti、Si元素作为本次分析的监测元素。本文通过调整加速电压和电流、背景和峰值测试时长以及干扰谱峰处理等来提高微量元素分析精度和准确度。分析结果显示，其中，Zr（780±29×10-6）（1SD，n=25）、Nb（2799±66×10-6）、V（1276±33×10-6）、Fe（4309±34×10-6）、Cr（718±31×10-6）的分析结果与二次离子质谱（SIMS）和激光剥蚀电感耦合等离子体质谱（LA-ICP-MS）的推荐值在误差范围内一致。大部分元素数据波动范围在10%以内，V、Fe元素的数据波动范围仅在5%以内。V、Nb和Fe测试精度比前人电子探针分析结果有较大提高。金红石Zr测试误差传递给金红石Zr温度计给出的温度误差一般<22℃。本文还对金红石Zr温度计应用、提高Ta元素分析精度和准确度、金红石Fe3+分析等问题进行了探讨。
Abstract:Synthetic oxides are commonly used as the monitor standards for the trace element analysis of rutile by Electron Probe Microanalyzer (EPMA). Systematic analyses of rutile standards are still lacking. In this study we present a detailed EPMA analysis (CAMECA SXFive) on nine elements (Al, Si, Ti, Fe, Cr, Zr, V, Nb and Ta) in the rutile standard R10. Ti and Si are used as monitor elements. To improve the analytical precision and reduce the detection limit, we have critically adjusted the acceleration voltage, beam current and counting time, and have deducted the interference peak signals. Our results show that the concentrations of Zr (780±29×10-6) (1SD, n=25), Nb (2799±66×10-6), V (1276±33×10-6), Fe (4309±34×10-6) and Cr (718±31×10-6) are well consistent with those analyzed by Secondary Ion Mass Spectrum (SIMS) or Laser Ablation Inductively Coupled Plasma Mass Spectrometry (LA-ICP-MS) within the error range. EPMA analysis in this study exhibits good stability. From a one-month monitoring period, the variations of Nb, Zr, and Cr are within ±10%, whereas the variations of V and Fe are within ±5%. Our modified techniques improved the analytical precisions of V, Nb and Fe in rutile. The analytical precision of Zr in this study would not significantly affect the results yielded by the Zr-in-rutile thermometer. Therefore, EPMA trace element analysis is an effective approach to understand the formation mechanisms of rutile. The techniques that can potentially improve the analytical precisions of Ta and Fe3+ analyses in rutile are also discussed.
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Key words:
- Rutile /
- Trace element /
- Electron probe microanalyzer (EPMA) /
- Zr-in-rutile thermometers
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图 1
电子探针部分参数之间的联系
Figure 1.
The relationship between peak position and background value
图 2
微量元素Ta检测限和测试精度与测试时长的线性关系
Figure 2.
Influence of the counting time on the detection limit and analytical precision
图 9
标样R10各微量元素数据稳定度检测图
Figure 9.
Analytical stability testing for trace elements (V, Cr, Zr, Fe, Nb) of rutile R10
表 2
电子探针相关参数：X-ray、晶体、通道、特征X射线能量值
Table 2.
EPMA parameters including X-ray, analyzing crystals, channels, as well as the energy of characteristic X-ray
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表 3
金红石标样R10微量元素(×10-6)电子探针分析结果
Table 3.
Trace element concentrations (×10-6) of the standard rutile R10 obtained by Cameca SX Five
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