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Improved electron probe microanalysis of trace elements in quartz

机译:改进的电子探针微分析石英中痕量元素的方法

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摘要

Quartz occurs in a wide range of geologic environments throughout the Earth's crust. The concentration and distribution of trace elements in quartz provide information such as temperature and other physical conditions of formation. Trace element analyses with modern electron-probe microanalysis (EPMA) instruments can achieve 99% confidence detection of ~100 ppm with fairly minimal effort for many elements in samples of low to moderate average atomic number such as many common oxides and silicates. However, trace element measurements below 100 ppm in many materials are limited, not only by the precision of the background measurement, but also by the accuracy with which background levels are determined. A new "blank" correction algorithm has been developed and tested on both Cameca and JEOL instruments, which applies a quantitative correction to the emitted X-ray intensities during the iteration of the sample matrix correction based on a zero level (or known trace) abundance calibration standard. This iterated blank correction, when combined with improved background fit models, and an "aggregate" intensity calculation utilizing multiple spectrometer intensities in software for greater geometric efficiency, yields a detection limit of 2 to 3 ppm for Ti and 6 to 7 ppm for Al in quartz at 99% t-test confidence with similar levels for absolute accuracy.
机译:石英存在于整个地壳的各种地质​​环境中。石英中微量元素的浓度和分布提供了诸如温度和其他物理形成条件等信息。使用现代电子探针微分析(EPMA)仪器进行痕量元素分析,可以以最低的工作量实现低至中等平均原子序数样品中的许多元素(例如许多常见的氧化物和硅酸盐)的99%置信度检测,准确度约为100 ppm。但是,许多材料中的痕量元素测量值低于100 ppm不仅受到背景测量精度的限制,而且还受到确定背景水平的精度的限制。已经在Cameca和JEOL仪器上开发并测试了新的“空白”校正算法,该算法在样本矩阵校正的迭代过程中基于零水平(或已知的迹线)丰度对发射的X射线强度进行了定量校正。校准标准。这种迭代的空白校正与改进的背景拟合模型结合使用,并利用软件中的多个光谱仪强度进行“汇总”强度计算以提高几何效率时,Ti的检测限为2至3 ppm,Al中的检测限为6至7 ppm。石英在99%的t试验置信度下具有相似的绝对准确度。

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