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2025
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| Online Access: | https://doi.org/10.5281/zenodo.19112916 |
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| author | Santagati, Gianluca |
| author_facet | Santagati, Gianluca |
| contents | <p>LAB-BASED XAS SPECTROSCOPY IN THE STUDY OF PIGMENT<br>MATERIALS SERVING THE FIXLAB PLATFORM OF E-RIHS</p> <p><br>Gianluca Santagati,1,2 Tecla Arcidiacono,1,2 Michela Botticelli,1,2 Claudia Caliri,1,2<br>Francesca Falcone,1,2 Costanza Miliani,1 Eva Luna Ravan1,3 and Francesco Paolo<br>Romano1,2</p> <p><br>1Istituto di Scienze del Patrimonio Culturale, Consiglio Nazionale delle Ricerche (CNR-ISPC), Italy<br>2Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali del Sud (INFN-LNS), Italy<br>3Department of Science of Antiquities, University of Rome ‘Sapienza’, Italy<br><br>X-ray Absorption Spectroscopy (XAS) is a well-established technique for chemical speciation,<br>widely applied at synchrotron facilities for pigment analysis. Being highly sensitive to the local<br>atomic structure, it provides unique insights into oxidation states, bond types, bond lengths, and<br>coordination environments, even in amorphous or poorly crystalline phases.[1] In particular, the<br>XANES (X-ray Absorption Near Edge Structure) region is especially sensitive to local<br>coordination and oxidation states in transition metal ions.[2] The EXAFS (Extended X-ray<br>Absorption Fine Structure) region, extending beyond the absorption edge, reveals interatomic<br>distances, coordination numbers, and structural disorder.[2] When used together in painting<br>investigation, XANES and EXAFS provide a comprehensive view of both the electronic and<br>geometric factors influencing the pigment stability or its degradation due to aging, environmental<br>factors or pigment-binder interaction. Recent improvements in X-ray sources and detectors now<br>enable XAS measurements in laboratory environments, reducing reliance on large-scale facilities.<br>In this work we present a novel lab-based XAS system recently installed at XRAYLab of ISPCCNR<br>in Catania, accessible through the FIXLAB platform of E-RIHS. We demonstrate the feasibility of<br>using this instrument to characterize ancient and modern pigments, both in the form of compressed<br>pellets or thin paint fragments, typically obtained from the sampling often performed during the<br>restoration procedures of real artworks. Specifically, we have developed a dedicated protocol for<br>the instrument to analyze real samples, incorporating guidelines for sample preparation that include<br>the minimum quantity of pigment required and the minimum detection time needed for obtaining<br>reliable spectra.<br>Preliminary results showcase the ability of lab-based XAS system to 1) reproduce XAS spectra<br>obtained at synchrotron facilities for reference standards and specific pigment materials; 2) detect<br>subtle spectral shifts and features indicative of phase transformations in pictorial pigments.</p> <p><br>Acknowledgements: PNRR projects: 1) H2IOSC “Humanities and Cultural Heritage Italian Open Science Cloud”,<br>IR0000029, CUP B63C22000730005; 2) CHANGES, “Science and Technologies for Sustainable Diagnostics of<br>Cultural Heritage”, PE0000020, CUP B53C22003890006; 3) SAMOTHRACE, “Sicilian MicronanoTech Research<br>And Innovation Center”, ECS00000022, CUP B63C22000620005. E-RIHS European Infrastructure of Heritage<br>Science (E-RIHS)</p> <p><br>[1] S. Mangold et al., J. Anal. At. Spectrom. 2003, 18, 723–729.<br>[2] D. C. Koningsberger, R. Prins,” X-ray Absorption: Principles, Applications, Techniques of EXAFS, SEXAFS and<br>XANES” 1988, Wiley, New York, 692.</p> |
| format | Recurso digital |
| id | zenodo_https___doi_org_10_5281_zenodo_19112916 |
| institution | Zenodo |
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| publishDate | 2025 |
| publisher | Zenodo |
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| spellingShingle | Lab-based XAS spectroscopy in the study of pigment materials serving the FIXLAB platform of E-RIHS Santagati, Gianluca <p>LAB-BASED XAS SPECTROSCOPY IN THE STUDY OF PIGMENT<br>MATERIALS SERVING THE FIXLAB PLATFORM OF E-RIHS</p> <p><br>Gianluca Santagati,1,2 Tecla Arcidiacono,1,2 Michela Botticelli,1,2 Claudia Caliri,1,2<br>Francesca Falcone,1,2 Costanza Miliani,1 Eva Luna Ravan1,3 and Francesco Paolo<br>Romano1,2</p> <p><br>1Istituto di Scienze del Patrimonio Culturale, Consiglio Nazionale delle Ricerche (CNR-ISPC), Italy<br>2Istituto Nazionale di Fisica Nucleare, Laboratori Nazionali del Sud (INFN-LNS), Italy<br>3Department of Science of Antiquities, University of Rome ‘Sapienza’, Italy<br><br>X-ray Absorption Spectroscopy (XAS) is a well-established technique for chemical speciation,<br>widely applied at synchrotron facilities for pigment analysis. Being highly sensitive to the local<br>atomic structure, it provides unique insights into oxidation states, bond types, bond lengths, and<br>coordination environments, even in amorphous or poorly crystalline phases.[1] In particular, the<br>XANES (X-ray Absorption Near Edge Structure) region is especially sensitive to local<br>coordination and oxidation states in transition metal ions.[2] The EXAFS (Extended X-ray<br>Absorption Fine Structure) region, extending beyond the absorption edge, reveals interatomic<br>distances, coordination numbers, and structural disorder.[2] When used together in painting<br>investigation, XANES and EXAFS provide a comprehensive view of both the electronic and<br>geometric factors influencing the pigment stability or its degradation due to aging, environmental<br>factors or pigment-binder interaction. Recent improvements in X-ray sources and detectors now<br>enable XAS measurements in laboratory environments, reducing reliance on large-scale facilities.<br>In this work we present a novel lab-based XAS system recently installed at XRAYLab of ISPCCNR<br>in Catania, accessible through the FIXLAB platform of E-RIHS. We demonstrate the feasibility of<br>using this instrument to characterize ancient and modern pigments, both in the form of compressed<br>pellets or thin paint fragments, typically obtained from the sampling often performed during the<br>restoration procedures of real artworks. Specifically, we have developed a dedicated protocol for<br>the instrument to analyze real samples, incorporating guidelines for sample preparation that include<br>the minimum quantity of pigment required and the minimum detection time needed for obtaining<br>reliable spectra.<br>Preliminary results showcase the ability of lab-based XAS system to 1) reproduce XAS spectra<br>obtained at synchrotron facilities for reference standards and specific pigment materials; 2) detect<br>subtle spectral shifts and features indicative of phase transformations in pictorial pigments.</p> <p><br>Acknowledgements: PNRR projects: 1) H2IOSC “Humanities and Cultural Heritage Italian Open Science Cloud”,<br>IR0000029, CUP B63C22000730005; 2) CHANGES, “Science and Technologies for Sustainable Diagnostics of<br>Cultural Heritage”, PE0000020, CUP B53C22003890006; 3) SAMOTHRACE, “Sicilian MicronanoTech Research<br>And Innovation Center”, ECS00000022, CUP B63C22000620005. E-RIHS European Infrastructure of Heritage<br>Science (E-RIHS)</p> <p><br>[1] S. Mangold et al., J. Anal. At. Spectrom. 2003, 18, 723–729.<br>[2] D. C. Koningsberger, R. Prins,” X-ray Absorption: Principles, Applications, Techniques of EXAFS, SEXAFS and<br>XANES” 1988, Wiley, New York, 692.</p> |
| title | Lab-based XAS spectroscopy in the study of pigment materials serving the FIXLAB platform of E-RIHS |
| url | https://doi.org/10.5281/zenodo.19112916 |