Abstract Total reflection X-ray fluorescence spectrometry (TXRF) is known as a state-of-the-art and fast-growing analytical technique. The spectral range of TXRF spectrometry encompasses elements from sodium to uranium. The object of this study was to develop, optimize, and validate the analytical method for fluorine in a form of calcium fluoride determination in fluoride fluxes by total reflection X-ray fluorescence spectrometry. The sample was lixiviated in acetic acid, then, the sample was filtered and the sediment and the filter were ignited at 650 °C. A portion of dried and ignited and weighed sample was placed in a plastic centrifuge tube. To this tube Triton X-100, Ga as internal standard and polyvinyl alcohol were added. The accuracy of the element determinations was estimated by comparison between obtained and certified values of the elements determined in the Certified Reference Materials of fluorite (fluorspar). The limit of detection for TXRF measurement is 4.26 μg F · dm−3 whereas the limit of quantification equals 12.78 μg F · dm−3. The variation coefficient that characterized the reproducibility of the measurement equals 16.94%. In addition to this, it was found that the uncertainty of results associated with the sample preparation process for TXRF measurement is negligible, compared to the measurement uncertainty at the measurement stage using TXRF spectrometry. The results of this work demonstrate the acceptable and fully satisfactory validation criteria such as limit of detection and quantification, accuracy, and precision.

中文翻译：

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用全反射 X 射线荧光法测定氟化物通量中的氟

摘要 全反射 X 射线荧光光谱法 (TXRF) 被认为是最先进且发展迅速的分析技术。TXRF 光谱的光谱范围涵盖从钠到铀的元素。本研究的目的是开发、优化和验证通过全反射 X 射线荧光光谱法测定氟化物通量中氟化钙形式的氟的分析方法。样品在乙酸中浸出，然后，样品被过滤，沉淀物和过滤器在650℃下点燃。将一部分干燥、点燃并称重的样品放入塑料离心管中。向该管 Triton X-100 中加入 Ga 作为内标和聚乙烯醇。元素测定的准确度是通过比较萤石（萤石）有证标准物质中测定的元素的获得值和标准值之间的比较来估计的。TXRF 测量的检测限为 4.26 μg F·dm-3，而定量限等于 12.78 μg F·dm-3。表征测量重现性的变异系数等于 16.94%。除此之外，与使用 TXRF 光谱法测量阶段的测量不确定度相比，与 TXRF 测量的样品制备过程相关的结果不确定度可以忽略不计。这项工作的结果证明了可接受且完全令人满意的验证标准，例如检测限和定量限、准确度和精密度。