L.K. Herrera

Advanced combined application of μ-X-ray diffraction/μ-X-ray fluorescence with conventional techniques for the identification of pictorial materials from Baroque Andalusia paintings

The process of investigating paintings includes the identification of materials to solve technical and historical art questions, to aid in the deduction of the original appearance, and in the establishment of the chemical and physical conditions for adequate restoration and conservation. In particular, we have focused on the identification of several samples taken from six famous canvases painted by Pedro Atanasio Bocanegra, who created a very special collection depicting the life of San Ignacio, which is located in the church of San Justo y Pastor of Granada, Spain. The characterization of the inorganic and organic compounds of the textiles, preparation layers, and pictorial layers have been carried out using an XRD diffractometer, SEM observations, EDX spectrometry, FT-IR spectrometry (both in reflection and transmission mode), pyrolysis/gas chromatography/mass spectrometry and synchrotron-based micro-X-ray techniques. In this work, the advantages over conventional X-ray diffraction of using combined synchrotron-based micro-X-ray diffraction and micro-X-ray fluorescence in the identification of multi-layer paintings is demonstrated.

Study by grazing incident diffraction and surface spectroscopy of amalgams from ancient mirrors

Characterization of four amalgam surfaces, with different alteration degrees from Andalusia historical mirrors, has been carried out by grazing-incidence X-ray diffraction (GIXRD), and other spectroscopic techniques (SEM/EDX, XPS, and REELS). The combination of all these techniques allows determining the corrosion state of the amalgams. The results show that the amalgams are composed in all cases of a binary alloy of tin and mercury. As mercury has high vapour pressure at RT, it slowly segregates and eventually evaporates, it leaves finely divided particles of tin that easily can be oxidize, forming tin monoxide (SnO) and tin dioxide (SnO2). In one of the samples, most of the amalgam remains unoxidized, since Hg0.1Sn0.9 and metallic Sn phases are the major components; in two other samples, Hg0.1Sn0.9 and Sn phases are not detected while SnO2 and SnO phases appear. Finally, in the last studied sample, only SnO2 phase is detected. The surface analyses of these samples by XPS show that, for most of them an unique chemical species (Sn4+) is found.

Non-destructive analysis of cultural heritage artefacts from Andalusia, Spain, by X-ray diffraction with Göbel mirrors

The characterization of the phases present in artefacts has been normally carried out using XRD (Bragg-Brentano geometry) that requires sampling from artworks, being a destructive technique. However, X-ray diffraction with Göbel mirrors permits directly to study rough artefacts without sampling. Grazing incidence attachments can be used to characterize as much the superficial layer as the underlying ones in flat samples to obtain information about the depth profile of some samples. The combination of Göbel mirrors and measure at low fixed incidence angles allow to obtain information about the depth profile of bent samples. This work reports the alteration processes on the surface of the following cultural heritage artefacts: a rivet and a nail extracted from Pardon Gateway, located in the North façade of Mosque-Cathedral of Cordoba; a Roman arrow and a button from a Roman jacket obtained from an excavation in Baena (Cordoba); organ pipe from Cathedral of Zaragoza; lead seals from Seville City Hall collection. The main objective of this paper is the study through a totally non-destructive analytical method, X-ray diffraction with Göbel mirrors, of the superficial alteration of some metallic artefacts from cultural heritage. This knowledge allows us the election of appropriate methods to carry out the restoration of these artefacts.