Evaluation of analysis volume in total reflection X‐ray fluorescence analysis
Evaluation of analysis volume in total reflection X‐ray fluorescence analysis
复制标题
全反射X射线荧光分析中分析体积的评价
DOI：
10.1002/xrs.3335
复制
发表时间：
2023
影响因子：
1.2
通讯作者：
Matsuyama Tsugufumi
中科院分区：
文献类型：
--
作者：
Tsuji Kouichi;Taniguchi Naoya;Yamaguchi Hiroki;Matsuyama Tsugufumi
全反射X射线荧光（TXRF）广泛用于痕量元素分析，其中单色薄X射线束通常应用于掠射角度。仪器测量样品的实际体积（分析体积）取决于X射线束的尺寸和掠射角度，这是TXRF分析样品制备的关键特征。在此，对分析体积进行了实验评估，包括分析区域和分析高度。利用真空蒸发装置在平板玻璃基板上的特定位置制备了厚度约为5nm、直径约为1mm的薄层。通过操纵带有小孔的掩模板来控制该金层的位置。在不同的金层位置制备9个样品，使用台式TXRF仪器在8个方位角上进行分析。最后，在玻璃基板上显示了Au的XRF强度分布。结果发现，使用台式TXRF仪器可以有效地检测到直径约为5mm的XRF。在直径为5mm，厚度为5nm的聚酰亚胺薄膜上沉积一层薄薄的金层，实验评估了分析高度。通过在金层和玻璃基板之间插入聚酰亚胺薄膜来调节金层的高度。随着Au层高度的增加，样品的XRF强度急剧下降，表明在<10 μm的高度下，使用所描述的设置可以有效地检测样品发射的XRF。
Total reflection X‐ray fluorescence (TXRF) is widely used for trace elemental analysis, wherein a thin monochromatic X‐ray beam is typically applied at glancing angles. The actual volume of the sample measured by the instrument (analysis volume) depends on the dimensions of the X‐ray beam and glancing angle, and it is a key feature in sample preparation for TXRF analysis. Herein, the analysis volume, including the analysis region and analysis height, was experimentally evaluated. A thin Au layer approximately 5 nm thick and 1 mm in diameter was prepared at a specific position on a flat glass substrate using a vacuum evaporation device. The position of this Au layer was controlled by manipulating a mask plate with a small hole. Nine samples were prepared at different Au layer positions and analyzed at 8 azimuth angles using a tabletop TXRF instrument. Finally, the Au XRF intensity distribution was visualized on a glass substrate. It was found that the XRF emitted over a diameter of approximately 5 mm was effectively detected using the tabletop TXRF instrument. The analysis height was experimentally evaluated using a thin Au layer deposited on a polyimide film 5 mm in diameter and 5 nm thick. The Au layer height was adjusted by inserting polyimide thin films between the Au layer and the glass substrate. The Au XRF intensity drastically decreased with increasing Au layer height, suggesting that the XRF emitted from the sample is effectively detected at heights of <10 μm by using the described setup.