Analytical and Environmental Chemistry Laboratory, University Campus, Technical University of Crete, Chania, Greece.
Anal Chem. 2011 May 1;83(9):3386-91. doi: 10.1021/ac103295a. Epub 2011 Apr 4.
In the present work a method for the determination of perchlorate trace levels by total reflection X-ray fluorescence (TXRF) is introduced. Perchlorate anions were concentrated on anion-selective membranes that had been prepared on the surface of TXRF quartz reflectors. Various complexation substances were used in the membranes. The reflectors were immersed in water solutions containing nanogram per milliliter (ppb) concentrations of perchlorate. After this step, the reflectors were taken out of the solution and they were analyzed by TXRF, using a copper X-ray tube and helium flow on the target (to lower the argon peak which is present in the air). The effects of various experimental parameters were examined, and the possibility of discrimination between chloride and perchlorate anions was shown. Minimum detection limits lower than 1 ng/mL and good linearity at the concentration range of 1-50 ng/mL were achieved. The method is applicable for the analysis of perchlorate in drinking water samples.
本工作介绍了一种通过全反射 X 射线荧光（TXRF）测定痕量高氯酸盐的方法。高氯酸盐阴离子被浓缩在 TXRF 石英反射器表面制备的阴离子选择性膜上。在膜中使用了各种络合物物质。将反射器浸入含有纳克/毫升（ppb）浓度高氯酸盐的水溶液中。在这一步之后，将反射器从溶液中取出，并通过 TXRF 进行分析，在靶材上使用铜 X 射线管和氦气流（以降低空气中存在的氩峰）。研究了各种实验参数的影响，并显示了区分氯离子和高氯酸盐阴离子的可能性。在 1-50ng/mL 的浓度范围内，检测限低于 1ng/mL，线性良好。该方法适用于饮用水样品中高氯酸盐的分析。
