Development and characterization of a high-sensitivity and high-throughput in-house multimodal TXRF/GIXRF mobile spectrometer

Total-reflection X-ray Fluorescence (TXRF) and Grazing Incidence X-ray Fluorescence (GIXRF) techniques are non-destructive methods widely applied across diverse research domains. These methodologies capitalize on constructive and destructive interferences between grazing incident and reflected X-rays to generate an X-ray standing wave (XSW) field, optimizing excitation conditions at interfaces and reflective surfaces and minimizing background noise thus enabling highly sensitive depth-resolved specific analysis at the nanometer regime. High precision tuning of the angle of incidence allows detection of thin layers down to the nanometer scale. While TXRF is established in global laboratories, advanced methods like GIXRF have predominantly remained confined to synchrotron radiation facilities due to the need of high flux monochromatic X-ray sources as well as high level of control in the beam direction and its divergence. Successful implementation of lab-based GIXRF instruments is furthermore constrained by data evaluation capabilities, critical for accurately modelling experimental datasets and determining the effective solid angles of detection, that vary in a not trivial fashion with the incident angles. This article showcases the development of a fully functional high sensitivity and high through-put mobile TXRF/GIXRF system assembled in-house, utilizing high-efficiency new-generation sources, high-efficiency silicon detectors and a high-precision motorized rotational stage. The system's capabilities have been tested on a range of well-characterized samples in both total reflection and grazing incidence geometries. This approach allows for the detection of contaminants in the parts per billion range and the extraction of the depth profile of a layered sample in the nanometer range. Future improvements could focus on adapting the developed system for application on imperfect samples surfaces in cultural heritage studies. • Development of a fully functional mobile TXRF/GIXRF system for in-house and in-situ applications. • Detection of target contaminants in the parts per billion range. • Extraction of the depth profile of a layered samples in the nanometer range. • Application to complex sample surfaces in cultural heritage studies.

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Publication Details

Journal
Spectrochimica Acta Part B Atomic Spectroscopy
Published
2025-07-16
DOI
https://doi.org/10.1016/j.sab.2025.107279
Citations
1
Primary Topic
X-ray Spectroscopy and Fluorescence Analysis
Type
article
Field-Weighted Citation Impact
1.88
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article

Development and characterization of a high-sensitivity and high-throughput in-house multimodal TXRF/GIXRF mobile spectrometer

Francesco Paolo Romano, Andreas Germanos Karydas, C. G. Fatuzzo, Giuliana Aquilanti et al.
1 citations
Spectrochimica Acta Part B Atomic Spectroscopy
X-ray Spectroscopy and Fluorescence Analysis
1.88
article

Development and characterization of a high-sensitivity and high-throughput in-house multimodal TXRF/GIXRF mobile spectrometer

Francesco Paolo Romano, Andreas Germanos Karydas, C. G. Fatuzzo, Giuliana Aquilanti, Michela Botticelli, Claudia Caliri, Eva Luna Ravan, G. Santagati
article en
1 citations

Abstract

Total-reflection X-ray Fluorescence (TXRF) and Grazing Incidence X-ray Fluorescence (GIXRF) techniques are non-destructive methods widely applied across diverse research domains. These methodologies capitalize on constructive and destructive interferences between grazing incident and reflected X-rays to generate an X-ray standing wave (XSW) field, optimizing excitation conditions at interfaces and reflective surfaces and minimizing background noise thus enabling highly sensitive depth-resolved specific analysis at the nanometer regime. High precision tuning of the angle of incidence allows detection of thin layers down to the nanometer scale. While TXRF is established in global laboratories, advanced methods like GIXRF have predominantly remained confined to synchrotron radiation facilities due to the need of high flux monochromatic X-ray sources as well as high level of control in the beam direction and its divergence. Successful implementation of lab-based GIXRF instruments is furthermore constrained by data evaluation capabilities, critical for accurately modelling experimental datasets and determining the effective solid angles of detection, that vary in a not trivial fashion with the incident angles. This article showcases the development of a fully functional high sensitivity and high through-put mobile TXRF/GIXRF system assembled in-house, utilizing high-efficiency new-generation sources, high-efficiency silicon detectors and a high-precision motorized rotational stage. The system's capabilities have been tested on a range of well-characterized samples in both total reflection and grazing incidence geometries. This approach allows for the detection of contaminants in the parts per billion range and the extraction of the depth profile of a layered sample in the nanometer range. Future improvements could focus on adapting the developed system for application on imperfect samples surfaces in cultural heritage studies. • Development of a fully functional mobile TXRF/GIXRF system for in-house and in-situ applications. • Detection of target contaminants in the parts per billion range. • Extraction of the depth profile of a layered samples in the nanometer range. • Application to complex sample surfaces in cultural heritage studies.

Spectrochimica Acta Part B Atomic SpectroscopyVol. 232
Istituto Nazionale di Fisica Nucleare (IT), National Centre of Scientific Research "Demokritos" (GR), Elettra-Sincrotrone Trieste S.C.p.A. (IT), Istituto di Fisiologia Clinica (IT), Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali del Sud (IT), Institute of Nuclear and Particle Physics (GR), Sapienza University of Rome (IT)
Openalex Percentile: Top 14%
X-ray Spectroscopy and Fluorescence Analysis
1.88
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