[1] The Cretaceous paleogeography and the kinematic evolution of the Iberian plate are poorly constrained. Especially problematic is to reconcile Iberian paleomagnetic data with paleomagnetic data of the neighboring plates and with Euler poles derived from seafloor magnetic anomalies. The first limitation arises from the Cretaceous Normal Polarity Superchron where paleogeographic reconstruction using marine magnetic anomalies is handicapped. The second arises from the paucity of reliable paleomagnetic poles with satisfactory statistical criteria and age. In order to address these shortcomings and provide new high quality paleomagnetic poles for Iberia, we conducted a detailed rock magnetic and paleomagnetic study of two Cretaceous magmatic sills, the Paço de Ilhas (PI) and Foz da Fonte (FF) sills, from the Lusitanian Basin, Portugal, recently dated at about 88 and 94 Ma, respectively. Our results show that the magnetic mineralogy of the sills is primary, i.e., acquired during magma cooling, and essentially represented by titanomagnetite. The corresponding paleomagnetic poles match the synthetic APWP from the African plate at 80 and 100 Ma. On the basis of a rigorous selection of Iberian Cretaceous poles, we then calculated mean paleomagnetic poles for different time intervals and found that Iberian paleomagnetic data fit well the global APWP between 70 and 120 Ma, but move far away from the APWP at pre-rift times. Our approach shows that new and better constrained paleomagnetic poles can aide in solving part of the contradiction between Iberian and African APWPs.
The Roman town of Ammaia (in Marvão Region) is considered one of the most important recent findings of the Roman presence in Portuguese territory. It was settled in Republican times and abandoned in the seventh century. In this research, 17 masonry mortars and renders from the West Tower (South Gate), the residential area near the West Tower, the macellum, the peristylium, the public bath building, the podium of the temple and the portico of the forum were analysed. The methodology of chemical, mineralogical and microstructural characterization has involved several complementary techniques, including stereomicroscopy, X‐ray diffraction, thermal analysis and scanning electron microscopy coupled with energy‐dispersive X‐ray spectroscopy. The results indicate that the mortars from the beginning of the town's edification were mainly composed of soil (clays). Later, during the main Roman building period, mortars were composed using a calcitic binder and the mortar composition varied according to their use and function. The samples from a period subsequent to the Roman occupation are based on a dolomitic binder. From the present study, relevant information has been acquired about the technological evolution of Roman construction in Ammaia, the historical context of the archaeological structures and guidelines for the conservation and restoration of mortars.
Historical mortars from sixteenth to seventeenth century military forts located at the mouth of the Tagus River in Lisbon have been characterized by polarized light microscopy (PLM), thermal analysis (TG/DTA), X-ray diffractometry (XRD) and scanning electron microscopy ? energy dispersive spectroscopy (SEM ? EDS). The results indicate that the mortars used were all hydraulic lime-based. The presence of well-rounded lime lumps indicates a limited use of water during the lime hydration process. The detection of hydrated calcium chloroaluminate and carboaluminate compounds mostly at binder-aggregate interfaces provides evidence for the onset of pozzolanic reactions during mortar production as further confirmed by the presence of ceramic fragments in the aggregate fractions intentionally added by the fort builders to increase the hydraulic properties of the mortars. The higher mechanical strength and greater resistance to degradation processes imparted by these pozzolanic compounds could explain why, despite the extreme proximity of the investigated sites to the sea, salt weathering processes do not appear to have significantly affected the studied mortars.
Seventeen Portuguese miniature portraits on copper support from the Évora Museum collection (Portugal) were analyzed in situ and nondestructively by Raman microscopy (RM), SEM-EDS, and stereomicroscopy. This work constitutes a great breakthrough in the study of miniature paintings from the 17 th and 18 th centuries, since the chemical information known about this unique kind of paintings are still scarce, and in particular, this exclusive collection was never been subjected to any physicochemical study. In this work, each portrait was examined in detail in order to characterize the pigments palette used by the miniaturists. The μ-Raman analysis, in particular, guaranteed an exceptional visualization and good individual identification of small grains of pigments and other constituents of the pictorial layer. Using this technique, 19 compounds were identified, including bluish black covellite, a pigment rarely found in oil paintings. SEM-EDS was used as an important complementary technique to confirm the chemical nature of some pigments and to identify shell gold (gold dust) in some portraits. Overall, the pigments identified in this large set of old paintings are broadly consistent with those mentioned in the painting treatises of that time or reported in other more modern bibliographic sources.
Energy dispersive X-ray fluorescence (EDXRF) is a well-known technique for non-destructive and in situ analysis of archaeological artifacts both in terms of the qualitative and quantitative elemental composition because of its rapidity and non-destructiveness. In this study EDXRF and realistic Monte Carlo simulation using the X-ray Monte Carlo (XRMC) code package have been combined to characterize a Cu-based bowl from the Iron Age burial from Fareleira 3 (Southern Portugal). The artifact displays a multilayered structure made up of three distinct layers: a) alloy substrate; b) green oxidized corrosion patina; and c) brownish carbonate soil-derived crust. To assess the reliability of Monte Carlo simulation in reproducing the composition of the bulk metal of the objects without recurring to potentially damaging patina's and crust's removal, portable EDXRF analysis was performed on cleaned and patina/crust coated areas of the artifact. Patina has been characterized by micro X-ray Diffractometry (μXRD) and Back-Scattered Scanning Electron Microscopy + Energy Dispersive Spectroscopy (BSEM + EDS). Results indicate that the EDXRF/Monte Carlo protocol is well suited when a two-layered model is considered, whereas in areas where the patina + crust surface coating is too thick, X-rays from the alloy substrate are not able to exit the sample.
This work is part of a broader research line that aims to develop and implement a nondestructive methodology for the chemical characterization of archaeological metals based on a protocol that combines energy dispersive X-ray fluorescence spectrometry (ED-XRF) with a Monte Carlo (MC) simulation algorithm. In this paper, the ED-XRF/MC protocol has been applied to estimate the chemical composition
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