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Main Author:	Santagati, Gianluca
Format:	Recurso digital
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Published:	Zenodo 2025
Online Access:	https://doi.org/10.5281/zenodo.19112916
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LAB-BASED XAS SPECTROSCOPY IN THE STUDY OF PIGMENT MATERIALS SERVING THE FIXLAB PLATFORM OF E-RIHS Gianluca Santagati,1,2 Tecla Arcidiacono,1,2 Michela Botticelli,1,2 Claudia Caliri,1,2 Francesca Falcone,1,2 Costanza Miliani,1 Eva Luna Ravan1,3 and Francesco Paolo Romano1,2 1Istituto di Scienze del Patrimonio Culturale, Consiglio Nazionale delle Ricerche (CNR-ISPC), Italy 2Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali del Sud (INFN-LNS), Italy 3Department of Science of Antiquities, University of Rome ‘Sapienza’, Italy X-ray Absorption Spectroscopy (XAS) is a well-established technique for chemical speciation, widely applied at synchrotron facilities for pigment analysis. Being highly sensitive to the local atomic structure, it provides unique insights into oxidation states, bond types, bond lengths, and coordination environments, even in amorphous or poorly crystalline phases.[1] In particular, the XANES (X-ray Absorption Near Edge Structure) region is especially sensitive to local coordination and oxidation states in transition metal ions.[2] The EXAFS (Extended X-ray Absorption Fine Structure) region, extending beyond the absorption edge, reveals interatomic distances, coordination numbers, and structural disorder.[2] When used together in painting investigation, XANES and EXAFS provide a comprehensive view of both the electronic and geometric factors influencing the pigment stability or its degradation due to aging, environmental factors or pigment-binder interaction. Recent improvements in X-ray sources and detectors now enable XAS measurements in laboratory environments, reducing reliance on large-scale facilities. In this work we present a novel lab-based XAS system recently installed at XRAYLab of ISPCCNR in Catania, accessible through the FIXLAB platform of E-RIHS. We demonstrate the feasibility of using this instrument to characterize ancient and modern pigments, both in the form of compressed pellets or thin paint fragments, typically obtained from the sampling often performed during the restoration procedures of real artworks. Specifically, we have developed a dedicated protocol for the instrument to analyze real samples, incorporating guidelines for sample preparation that include the minimum quantity of pigment required and the minimum detection time needed for obtaining reliable spectra. Preliminary results showcase the ability of lab-based XAS system to 1) reproduce XAS spectra obtained at synchrotron facilities for reference standards and specific pigment materials; 2) detect subtle spectral shifts and features indicative of phase transformations in pictorial pigments. Acknowledgements: PNRR projects: 1) H2IOSC “Humanities and Cultural Heritage Italian Open Science Cloud”, IR0000029, CUP B63C22000730005; 2) CHANGES, “Science and Technologies for Sustainable Diagnostics of Cultural Heritage”, PE0000020, CUP B53C22003890006; 3) SAMOTHRACE, “Sicilian MicronanoTech Research And Innovation Center”, ECS00000022, CUP B63C22000620005. E-RIHS European Infrastructure of Heritage Science (E-RIHS) [1] S. Mangold et al., J. Anal. At. Spectrom. 2003, 18, 723–729. [2] D. C. Koningsberger, R. Prins,” X-ray Absorption: Principles, Applications, Techniques of EXAFS, SEXAFS and XANES” 1988, Wiley, New York, 692.

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