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Validation of energy-dispersive X-ray fluorescence procedure for determination of major and trace elements present in the cement based composites
Spectrochimica Acta Part B: Atomic Spectroscopy ( IF 3.2 ) Pub Date : 2019-12-01 , DOI: 10.1016/j.sab.2019.105729
Nevenka Mijatović , Anja Terzić , Lato Pezo , Ljiljana Miličić , Dragana Živojinović

Abstract Adjustment and subsequent validation of energy-dispersive X-ray fluorescence (ED-XRF) method for cement based binders with addition of mineral raw materials (fly ash, zeolite and bentonite) was conducted. Eighteen chemical elements present in the material composition were analyzed: ten major elements (Si, Al, Fe, Ca, Mg, S, Na, K, Ti, P) and eight trace elements (Cr, Zn, Cu, As, Ni, Pb, Sr, Mn). Thirty-five samples of either certified reference materials or reference materials of cement, fly ash and clay were utilized during adjustment and optimization of the investigated ED-XRF procedure. The method was consecutively validated in terms of selectivity, precision, working range, linearity, accuracy, robustness, limits of detection and quantification. Thirty-two samples in total, i.e. three certified reference materials and twenty-nine reference materials, were simultaneously analyzed by ED-XRF and inductively coupled plasma optical emission spectrometry (ICP-OES). Comparison of the outputs of monitored methods showed infinitesimally small differences, as correlation coefficients were extremely good (≈1), which highlighted ED-XRF as highly satiable alternative for ICP-OES for the chemical analysis of cement binders.

中文翻译:

用于测定水泥基复合材料中存在的主要和痕量元素的能量色散 X 射线荧光程序的验证

摘要 对添加矿物原料(粉煤灰、沸石和膨润土)的水泥基粘合剂的能量色散 X 射线荧光 (ED-XRF) 方法进行了调整和后续验证。分析了材料成分中存在的十八种化学元素:十种主要元素(Si、Al、Fe、Ca、Mg、S、Na、K、Ti、P)和八种微量元素(Cr、Zn、Cu、As、Ni、铅、锶、锰)。在所研究的 ED-XRF 程序的调整和优化过程中,使用了 35 个认证参考材料或水泥、粉煤灰和粘土参考材料的样品。该方法在选择性、精密度、工作范围、线性、准确度、稳健性、检测限和定量方面得到了连续验证。总共三十二个样本,即 通过 ED-XRF 和电感耦合等离子体发射光谱法 (ICP-OES) 同时分析三种有证标准物质和 29 种标准物质。监测方法的输出比较显示出非常小的差异,因为相关系数非常好 (≈1),这突出了 ED-XRF 作为 ICP-OES 的高度令人满意的替代品,用于水泥粘合剂的化学分析。
更新日期:2019-12-01
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