Abstract Element distribution data in lake sediments are widely used to study environmental and climate change over geological time scales. Total reflection X-ray fluorescence (TXRF) seems to be well suited for fast multi-elemental analysis of small quantities of subsamples obtained by cutting a sediment core at different intervals. The TXRF technique based on the direct analysis of a suspension prepared by mixing 20 mg of powdered sample and 2 mL of an aqueous 1% Triton X-100 solution was applied to the various reference materials of sedimentary rocks and samples of lake sediments to determine Al, K, Ca, Ti, V, Cr, Mn, Fe, Ni, Cu, Zn, Rb, Sr, and Ba contents. It was shown that the element internal standard, as well the Compton scattered peak, can be used to compensate the error associated with the sample deposition process. Different quantitative approaches have been proposed and evaluated using the reference materials of the sedimentary rocks: (i) internal standardization, (ii) external calibration with correction by means of adding an internal standard, (iii) external calibration with the ‘fluorescent-to-Compton’ correction. It was shown that the external calibrations can compensate systematic overestimation or underestimation of the TXRF results obtained using the internal standard method, especially for Al, K, V, Cr, Zn, Rb, and Ba. The TXRF results for Ca, Ti, Mn, Fe, Ni, Cu, and Sr weakly depend on the quantitative procedure.

中文翻译：

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全反射X射线荧光法测定湖泊沉积物中元素的定量方法

摘要 湖泊沉积物中的元素分布数据被广泛用于研究地质时间尺度上的环境和气候变化。全反射 X 射线荧光 (TXRF) 似乎非常适合对通过以不同间隔切割沉积物核心获得的少量子样品进行快速多元素分析。TXRF 技术基于对通过混合 20 mg 粉末样品和 2 mL 1% Triton X-100 水溶液制备的悬浮液进行直接分析，应用于沉积岩的各种标准物质和湖泊沉积物样品中，以确定铝、K、Ca、Ti、V、Cr、Mn、Fe、Ni、Cu、Zn、Rb、Sr 和 Ba 含量。结果表明，元素内标以及康普顿散射峰可用于补偿与样品沉积过程相关的误差。已经提出并使用沉积岩的参考材料评估了不同的定量方法：（i）内部标准化，（ii）通过添加内部标准进行校正的外部校准，（iii）使用“荧光到-”的外部校准康普顿的修正。结果表明，外部校准可以补偿系统对使用内标法获得的 TXRF 结果的高估或低估，特别是对于 Al、K、V、Cr、Zn、Rb 和 Ba。Ca、Ti、Mn、Fe、Ni、Cu 和 Sr 的 TXRF 结果弱依赖于定量程序。(iii) 使用“荧光到康普顿”校正的外部校准。结果表明，外部校准可以补偿系统对使用内标法获得的 TXRF 结果的高估或低估，特别是对于 Al、K、V、Cr、Zn、Rb 和 Ba。Ca、Ti、Mn、Fe、Ni、Cu 和 Sr 的 TXRF 结果弱依赖于定量程序。(iii) 使用“荧光到康普顿”校正的外部校准。结果表明，外部校准可以补偿系统对使用内标法获得的 TXRF 结果的高估或低估，特别是对于 Al、K、V、Cr、Zn、Rb 和 Ba。Ca、Ti、Mn、Fe、Ni、Cu 和 Sr 的 TXRF 结果弱依赖于定量程序。