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. 2021 Nov 1;28(Pt 6):1811-1819.
doi: 10.1107/S1600577521008857. Epub 2021 Oct 18.

Trace-element XAFS sensitivity: a stress test for a new XRF multi-detector

Ilaria Carlomagno  1 , Matias Antonelli  2 , Giuliana Aquilanti  1 , Pierluigi Bellutti  3 , Giuseppe Bertuccio  4 , Giacomo Borghi  3 , Giuseppe Cautero  1 , Daniela Cirrincione  2 , Giovanni de Giudici  5 , Francesco Ficorella  3 , Massimo Gandola  4 , Dario Giuressi  1 , Daniela Medas  5 , Filippo Mele  4 , Ralf H Menk  1 , Luca Olivi  1 , Giulio Orzan  2 , Antonino Picciotto  3 , Francesca Podda  5 , Alexandre Rachevski  2 , Irina Rashevskaya  6 , Luigi Stebel  1 , Andrea Vacchi  2 , Gianluigi Zampa  2 , Nicola Zampa  2 , Nicola Zorzi  3 , Carlo Meneghini  7
Affiliations

Trace-element XAFS sensitivity: a stress test for a new XRF multi-detector

Ilaria Carlomagno et al. J Synchrotron Radiat. .

Abstract

X-ray absorption fine-structure (XAFS) spectroscopy can assess the chemical speciation of the elements providing their coordination and oxidation state, information generally hidden to other techniques. In the case of trace elements, achieving a good quality XAFS signal poses several challenges, as it requires high photon flux, counting statistics and detector linearity. Here, a new multi-element X-ray fluorescence detector is presented, specifically designed to probe the chemical speciation of trace 3d elements down to the p.p.m. range. The potentialities of the detector are presented through a case study: the speciation of ultra-diluted elements (Fe, Mn and Cr) in geological rocks from a calcareous formation related to the dispersal processes from Ontong (Java) volcanism (mid-Cretaceous). Trace-elements speciation is crucial in evaluating the impact of geogenic and anthropogenic harmful metals on the environment, and to evaluate the risks to human health and ecosystems. These results show that the new detector is suitable for collecting spectra of 3d elements in trace amounts in a calcareous matrix. The data quality is high enough that quantitative data analysis could be performed to determine their chemical speciation.

Keywords: X-ray absorption spectroscopy; X-ray fluorescence; fluorescence detector; geology.

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Figures

Figure 1
Figure 1
(a) One of the single modules of the detector described in the text. (b) Array of eight modules. (c) The detector mounted on the XAFS beamline.
Figure 2
Figure 2
Output count rate versus input count rate for different peaking times adapted from Bufon et al. (2019 ▸) for a single cell. Considering the entire detector has 64 cells, the system can handle more than 10 Mcounts s−1 within a linearity of 75%. The symbol τ indicated in the annotation is the fitted dead-time in the model of a paralyzed detector.
Figure 3
Figure 3
Energy resolution versus peaking time at room temperature (black line) and for the cooled detector (red line) with an average temperature of the sensors of 27°C and of 6°C, respectively.
Figure 4
Figure 4
XRF spectrum of the C20 sample: the fluorescence intensities are shown on a log-scale; the Fe, Mn and Cr K α fluorescence signals are emphasized in colour.
Figure 5
Figure 5
Normalized XANES spectra at the Fe, Mn and Cr K-edges. Spectra are vertically shifted for clarity.
Figure 6
Figure 6
Normalized XANES spectra at the Fe, Mn and Cr K-edge for the samples and for significant reference compounds.
Figure 7
Figure 7
LCA results for sample C13 (Fe concentration = 130 p.p.m.) at the Fe K-edge. The best fit (red line) to the experimental data (black dots) is obtained by a linear combination of the different phases, reported in the plot according to their multiplicative coefficients.
Figure 8
Figure 8
LCA results for sample C11 (Mn concentration = 13 p.p.m.) at the Mn K-edge. The best fit (red line) to the experimental data (black dots) is obtained by a linear combination of the different phases, reported in the plot according to their multiplicative coefficients.
Figure 9
Figure 9
LCA results for sample C9 (Cr concentration = 2.9 p.p.m.) at the Cr K-edge. The best fit (red line) to the experimental data (black dots) is obtained by a linear combination of the different phases, reported in the plot according to their multiplicative coefficients.
See this image and copyright information in PMC

References

    1. Bellotti, G., Butt, A., Carminati, M., Fiorini, C., Balerna, A., Piemonte, C., Zorzi, N. & Bombelli, L. (2016). 2016 IEEE Nuclear Science Symposium, Medical Imaging Conference and Room-Temperature Semiconductor Detector Workshop (NSS/MIC/RTSD), 29 October–6 November 2016, Strasbourg, France. IEEE.
    1. Benfatto, M. & Meneghini, C. (2015). In Synchrotron Radiation, edited by S. Mobilio, F. Boscherini and C. Meneghini. Heidelberg, Berlin: Springer.
    1. Bertuccio, G., Ahangarianabhari, M., Graziani, C., Macera, D., Shi, Y., Gandola, M., Rachevski, A., Rashevskaya, I., Vacchi, A., Zampa, G., Zampa, N., Bellutti, P., Giacomini, G., Picciotto, A., Piemonte, C. & Zorzi, N. (2016). IEEE Trans. Nucl. Sci. 63, 400–406.
    1. Bertuccio, G., Ahangarianabhari, M., Graziani, C., Macera, D., Shi, Y., Rachevski, A., Rashevskaya, I., Vacchi, A., Zampa, G., Zampa, N., Bellutti, P., Giacomini, G., Picciotto, A. & Piemonte, C. (2015). J. Instrum. 10, P01002.
    1. Bertuccio, G., Macera, D., Graziani, C. & Ahangarianabhari, M. (2014). 2014 IEEE Nuclear Science Symposium and Medical Imaging Conference (NSS/MIC), 8–15 November 2014, Seattle, WA, USA. IEEE.