Evaluation of analysis volume in total reflection X‐ray fluorescence analysis

Abstract

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.

2023 atomic spectrometry update – a review of advances in X-ray fluorescence spectrometry and its special applications

“…The optimal dimensions of a TXRF spectrometry specimen were evaluated by Tsuji et al 54 Mask vacuum evaporation was used to prepare a thin circular gold layer at specific positions on a flat glass substrate. By visualising the Au intensity over the glass substrate, it was concluded that a diameter of 5 mm could be detected.…”

Empirical evaluation of the TXRF detector field of view – a coffee-ring case study

“…They determined the change of the FOV at four different excitation angles. 12 The picoliter approach applied here simplies the procedure for determining the detector FOV. It allows positioning the deposits more precisely using motorized stages, which allow for independent movement in the x-, y-and z-directions.…”

Evaluations of the optimal plasma treated area in total reflection X-ray fluorescence analysis and the retention period of superhydrophilic ability of the substrate

“…Various commercially available TXRF instruments have been developed; therefore, it is important to determine the analysis area for each TXRF instrument. We have previously determined the analytical area measured using a NANOHUNTER-II TXRF instrument (Rigaku Co., Japan) to be approximately 4 × 5 mm 2 ; 15 therefore, we believe that the optimal APPJ-treated area should be smaller than this value. In addition, it is important to evaluate the retention time of hydrophilicity after APPJ treatment.…”