TXRF intensity dependence on position of dried residue on sample carrier and TXRF determination of halogen in liquid samples
TXRF intensity dependence on position of dried residue on sample carrier and TXRF determination of halogen in liquid samples
复制标题
TXRF 强度对样品载体上干燥残留物位置的依赖性以及液体样品中卤素的 TXRF 测定
DOI：
10.1002/xrs.2688
复制
发表时间：
2016
影响因子：
1.2
通讯作者：
K. Tsuji
中科院分区：
文献类型：
--
作者：
Y. Tabuchi;K. Tsuji
全反射X射线荧光（TXRF）光谱是一种有效的技术，可同时对放置在平坦基底上的少量样品进行多元素痕量分析。内标法通常用于饮用水和环境样品等液体样品的TXRF定量分析。然而，很难测定Cl和Br，因为通过加入酸性内标溶液，它们会作为挥发性卤化氢化合物损失。因此，我们尝试将传统的校准曲线法应用于卤素的无内标测定。如果不采用内标法，TXRF强度会根据干燥残留物与检测器的相对位置发生剧烈变化。因此，我们研究了TXRF强度与干燥残留物相对于检测器的位置之间的关系。结果证实，TXRF强度严重依赖于样品载体上干燥残留物的位置。通过使用鼓风机仔细控制样品溶液液滴的位置，以将干燥的残留物置于样品载体上最有效的位置。在没有内标的情况下，我们可以成功地制作出具有良好相关性的Cl校准曲线。最后，使用台式TXRF仪器通过校准曲线法成功测定了NaCl溶液（0 - 5 ppm，10 µl）中的Cl。Cl的检出限为63 ppb（ng/ml）。版权所有© 2016约翰威利父子有限公司.
Total reflection X‐ray fluorescence (TXRF) spectroscopy is an effective technique for simultaneous multi‐elemental trace analysis of a small volume of a sample placed on a flat substrate. An internal standard method is usually applied for quantitative TXRF analysis of liquid samples such as drinking water and environmental samples. However, it was difficult to determine Cl and Br because they were lost as volatile hydrogen halide compounds by adding an acid internal standard solution. Thus, we attempted to apply the traditional calibration curve method for the determination of halogens without internal standard. If internal standard method is not applied, the TXRF intensity drastically changes depending on the relative position of the dried residue to the detector. Therefore, we investigated the relationship between TXRF intensity and the position of dried residue relative to the detector. As a result, it was confirmed that TXRF intensity critically depended on the position of the dried residue on the sample carrier. The position of the droplet of the sample solution was carefully controlled by using an air blower in order to place the dried residue at the most effective position on the sample carrier. We could successfully make a calibration curve for Cl with a good relationship without internal standard. Finally, Cl in the NaCl solutions (0 –5 ppm, 10 µl) was successfully determined by the calibration curve method using a table‐top TXRF instrument. The limit of detection of Cl was 63 ppb (ng/ml). Copyright © 2016 John Wiley & Sons, Ltd.