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      Mass Spectrometric and Synchrotron Radiation based techniques for the identification and distribution of painting materials in samples from paints of Josep Maria Sert

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          Abstract

          Background

          Establishing the distribution of materials in paintings and that of their degradation products by imaging techniques is fundamental to understand the painting technique and can improve our knowledge on the conservation status of the painting. The combined use of chromatographic-mass spectrometric techniques, such as GC/MS or Py/GC/MS, and the chemical mapping of functional groups by imaging SR FTIR in transmission mode on thin sections and SR XRD line scans will be presented as a suitable approach to have a detailed characterisation of the materials in a paint sample, assuring their localisation in the sample build-up. This analytical approach has been used to study samples from Catalan paintings by Josep Maria Sert y Badía (20 th century), a muralist achieving international recognition whose canvases adorned international buildings.

          Results

          The pigments used by the painter as well as the organic materials used as binders and varnishes could be identified by means of conventional techniques. The distribution of these materials by means of Synchrotron Radiation based techniques allowed to establish the mixtures used by the painter depending on the purpose.

          Conclusions

          Results show the suitability of the combined use of SR μFTIR and SR μXRD mapping and conventional techniques to unequivocally identify all the materials present in the sample and their localization in the sample build-up. This kind of approach becomes indispensable to solve the challenge of micro heterogeneous samples. The complementary interpretation of the data obtained with all the different techniques allowed the characterization of both organic and inorganic materials in the samples layer by layer as well as to establish the painting techniques used by Sert in the works-of-art under study.

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          Most cited references20

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          Two-dimensional detector software: From real detector to idealised image or two-theta scan

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            Blackening of Pompeian cinnabar paintings: X-ray microspectroscopy analysis.

            Red Pompeian paintings, very famous for their deep intensity, are currently suffering from darkening. The origins of this darkening degradation are not clearly identified yet and remain a major issue for curators. In the specific case of cinnabar (HgS)-based red pigment, a photoinduced conversion into black metacinnabar is usually suspected. This work is focused on the blackening of red cinnabar paintings coated on a sparry calcite mortar. Different samples exhibiting different levels of degradation were selected upon visual observations and analyzed by synchrotron-based microanalytical techniques. Atomic and molecular compositions of the different debased regions revealed two possible degradation mechanisms. On one hand, micro X-ray fluorescence elemental maps show peculiar distributions of chlorine and sulfur. On the other hand, X-ray absorption spectroscopy performed at both Cl and S K-edges confirms the presence of characteristic degradation products: (i) Hg-Cl compounds (e.g., corderoite, calomel, and terlinguaite), which may result from the reaction with exogenous NaCl, in gray areas; (ii) gypsum, produced by the calcite sulfation, in black coatings. Metacinnabar is never detected. Finally, a cross section was analyzed to map the in-depth alteration gradient. Reduced and oxidized sulfur distributions reveal that the sulfated black coating consists of a approximately 5-mum-thick layer covering intact cinnabar.
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              Identification of reaction compounds in micrometric layers from gothic paintings using combined SR-XRD and SR-FTIR.

              Synchrotron radiation X-ray diffraction (micro-SR-XRD) and Fourier transform infrared spectroscopy (micro-SR-FTIR) are used in the non-destructive identification of reaction and aging compounds from micrometric ancient painting layers. The combination of the micrometer size and non-destructive nature of the techniques together with the high resolution and brilliance of the synchrotron radiation has proved to be a procedure most advantageous for the study of reaction, aging and degradation processes. Copper, lead and calcium carboxylates and oxalates are determined in the chromatic, preparation and alteration layers from 15th century egg tempera and oil paintings. Their nature and crystallinity have been assessed. Some hypothesis about the mechanisms of development of both carboxylates and oxalates are presented.
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                Author and article information

                Journal
                Chem Cent J
                Chem Cent J
                Chemistry Central Journal
                BioMed Central
                1752-153X
                2012
                22 May 2012
                : 6
                : 45
                Affiliations
                [1 ]Departament de Cristal.lografia, Mineralogia I Dipòsits Minerals, University of Barcelona, C/Marti i Franquès S/N, 08015, Barcelona, Spain
                [2 ]Dipartimento di Chimica e Chimica Industriale, University of Pisa, Via Risorgimento 35, 56126, Pisa, Italy
                [3 ]European Synchrotron Radiation Facility, 6 rue Jules Horowitz, F-38000, Grenoble, France
                [4 ]Centre de Recherche et de Restauration des Musées de France, CNRS UMR171, Palais du Louvre, Porte des Lions, 14 Quai François Mitterrand, F-75001, Paris, France
                [5 ]Science Division, Diamond Light Source Ltd, Harwell Science and Innovation Campus, Oxon, OX11 0DE, United Kingdom
                Article
                1752-153X-6-45
                10.1186/1752-153X-6-45
                3505478
                22616949
                823a5031-5d08-4deb-8a2f-8ab18859daa0
                Copyright ©2012 Lluveras-Tenorio et al.; licensee Chemistry Central Ltd.

                This is an Open Access article distributed under the terms of the Creative Commons Attribution License ( http://creativecommons.org/licenses/by/2.0), which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

                History
                : 2 February 2012
                : 27 April 2012
                Categories
                Research Article

                Chemistry
                xrd,synchrotron radiation,mapping,gc/ms,paintings,ftir
                Chemistry
                xrd, synchrotron radiation, mapping, gc/ms, paintings, ftir

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