Abstract This paper presents the assessment of a direct method to measure and analyse Pb in air particulate matter (PM) collected on polytetrafluoroethylene (PTFE) filtering membranes prepared by the SMART STORE® procedure. The suitability of grazing incidence X-ray fluorescence technique is verified on a set of continuous and conformal thin film samples created by atomic layer deposition. Different scans changing the angles of incidence are performed and the fluorescence intensity of thin films on PTFE substrate compared with that obtained by similar thin films deposited on Si wafer substrates. The effects of sample preparation, constraints, and limitations of the experimental setup are discussed. The results obtained by three commercial total reflection X-ray fluorescence spectrometers, equipped with Mo or Rh X-ray tubes, are compared. Reference samples with different Pb content are used to define the best measurement conditions, corresponding to the maximum fluorescence intensity. The precision is evaluated in terms of relative standard deviation of the net intensity, taking into account the homogeneity of the PM samples and hardware contributions to the errors. The calibration curves are built on the basis of mono- and multi-elemental Pb loaded PTFE reference samples. The analytical parameters, namely linear calibration and determination range, limits of detection, and quantification, are determined.

中文翻译：

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使用全反射 X 射线荧光光谱仪评估空气颗粒物中的测量和铅定量方法

摘要 本文介绍了测量和分析通过 SMART STORE® 程序制备的聚四氟乙烯 (PTFE) 过滤膜上收集的空气颗粒物 (PM) 中铅的直接方法的评估。掠入射 X 射线荧光技术的适用性在一组由原子层沉积产生的连续和保形薄膜样品上得到验证。执行不同的扫描改变入射角，并将 PTFE 基板上的薄膜的荧光强度与沉积在 Si 晶片基板上的类似薄膜所获得的荧光强度进行比较。讨论了样品制备的影响、约束和实验设置的限制。比较了三个配备 Mo 或 Rh X 射线管的商用全反射 X 射线荧光光谱仪获得的结果。使用不同铅含量的参考样品来定义最佳测量条件，对应于最大荧光强度。精度是根据净强度的相对标准偏差来评估的，同时考虑到 PM 样本的均匀性和硬件对误差的贡献。校准曲线建立在单元素和多元素铅负载 PTFE 参考样品的基础上。确定分析参数，即线性校准和测定范围、检测限和定量。考虑到 PM 样本的同质性和硬件对误差的贡献。校准曲线建立在单元素和多元素铅负载 PTFE 参考样品的基础上。确定分析参数，即线性校准和测定范围、检测限和定量。考虑到 PM 样本的同质性和硬件对误差的贡献。校准曲线建立在单元素和多元素铅负载 PTFE 参考样品的基础上。确定分析参数，即线性校准和测定范围、检测限和定量。