A monochromatic confocal micro-x-ray fluorescence (μXRF) spectrometer for the lab

• Published in: Review of scientific instruments 2020-12, Vol.91 (12), p.123107-123107
• Main Authors: Ingerle, D., Swies, J., Iro, M., Wobrauschek, P., Streli, C., Hradil, K.
• Format: Article
• Language: English
• Subjects: Biological properties; Bremsstrahlung; Collimation; Excitation; Molybdenum; Parameters; Scientific apparatus & instruments; Spatial distribution; Spatial resolution; Standard reference materials; Trace elements; X ray fluorescence analysis
• ISSN: 0034-6748; 1089-7623
• DOI: 10.1063/5.0028830

Confocal micro-x-ray fluorescence (μXRF) is a powerful tool to analyze the spatial distribution of major, minor, and trace elements in three dimensions. Typical (confocal) μXRF measurements in the lab use polychromatic excitation, complicating quantification and fundamental parameter-based corrections and furthermore deteriorating peak-to-background ratios due to scattered bremsstrahlung. The goal for the new setup was to remedy these problems, without sacrificing spatial resolution, and keep it flexible for different excitation energies and transportation to other sources. The source assembly consists of a water-cooled fine-focus x-ray diffraction tube and a parallel beam-mirror, which produces a quasi-parallel, monochromatic beam. The presented results were obtained using a 2 kW molybdenum tube and a mirror for Mo-Kα. The confocal setup itself consists of two polycapillary half-lenses, one for the source side and the other for the detector side, where a 50 mm2 silicon drift detector is mounted. Both polycapillaries have a focus size of ∼15 μm for Mo-Kα. The second polycapillary can also be exchanged for a custom-designed collimator in order to perform non-confocal μXRF. Details of the technical setup and results from technical and biological samples are presented. Detection limits for selected elements from Ca to Pb in the confocal and non-confocal mode were established (e.g., 1 μg/g non-confocal and 20 μg/g confocal for As) using the NIST standard reference materials (SRMs) 621 and 1412. Furthermore, the results of the measurements of SRM 621 were evaluated using the fundamental parameter based quantification software ATI-QUANT. The results are compared with the certified values and generally are in good agreement.