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- Alluvial nodular monazite in Monfortinho (Idanha-a-Nova, Portugal): Regional distribution and genesisPublication . Salgueiro, Rute; Inverno, Carlos; de Oliveira, Daniel Pipa Soares; Guimarães, Fernanda; Lencastre, José; Rosa, DiogoABSTRACT: This work constitutes a contribution to the knowledge on the occurrence of nodular monazite in the Monfortinho (Idanha-a-Nova) alluviums and its genesis. A new edition of the alluvial nodular monazite regional distribution map is presented, underlining its wide occurrence and preferential concentration in the north-western and central zones of this region. The assessment of the geological and environmental evolution during Neoproterozoic-Palaeozoic and Caenozoic times and alluvial nodular monazite accumulation seems to provide a direct association between the presence of the Ordovician rocks, in particular the radioactive (carrying radioactive heavy minerals) quartzite (one of the most probable original sources) and Caenozoic sedimentary rocks (most probably the secondary source). Nevertheless, the Slate-Greywacke Complex cannot be excluded as a host rock for nodular monazite as well. Alluvial heavy mineral concentrates include: iron oxide/hydroxide, ilmenite, tourmaline, nodular monazite, monazite, xenotime, zircon, rutile, anatase, brookite, apatite, andalusite, gold, cassiterite and topaz. There is a significant REE enrichment in these concentrates (up to> 32,000 mg/kg), mainly in LREE-MREE. The contents in Ce and Th, Th and REE and Ce and La showed good correlation (0.97, 0.96 and 0.99, respectively), reflecting mainly the striking presence of nodular monazite, as can be proved by the similarity among NASCN patterns of this mineral and concentrates. In Monfortinho there are two distinct alluvial nodular monazite populations: 1) distal pre-deformation nodules generation, from the central western area, mostly ellipsoidal to discoidal, with irregular not orientated probable detrital mineral inclusions; and 2) proximal generation, in the northern area near the Ordovician rocks, with smaller grains, with mostly irregular surfaces. Diagenetic/low metamorphic pre-deformation distal Monfortinho nodules population growth can be recognised and characterised by the encompassing of irregular unoriented mineral inclusions of the host matrix rock; preferential incorporation of MREE over other REE in the core nodules, consistent with diagenetic MREE-rich environmental/mineralized fluids supplied by the dehydration of Variscan sedimentary marine sequences with phosphatic rocks, at the start of nodule formation. The slight increase in Ca towards the nodule rims denotes a relative increase in fluid salinity during nodule growth, consistent with the ineffectiveness of metamorphic dewatering in dissolving the significant salt content of those marine sequence(s); Th increment in nodule rims points to the temperature increment at this stage; its moderately to pronouncedly negative Eu anomalies and the general involvement of the cheralitic substitution mechanism are characteristic of metamorphic monazites. Monfortinho and other published data suggest that in the beginning of nodular monazite formation the fractionation (La/Sm) N tended to be lower than that of the original source (detrital relic mineral/seawater), very similar to primary synsedimentary apatite or to monazite nodules interpreted to have precipitated directly from seawater. At the end the fractionation values can be substantially higher than those and may be dependent on the conditions established during the different geologic environments.
- Alluvial xenotime and heavy minerals assemblage from the northern edge of Nisa-Albuquerque Batholith, eastern Portugal : provenance and geochemical implicationsPublication . Salgueiro, Rute; Rosa, Diogo; Inverno, Carlos; de Oliveira, Daniel Pipa Soares; Solá, A. Rita; Guimarães, FernandaAlluvial xenotime and heavy minerals assemblage from the northern edge of Nisa-Albuquerque Batholith, eastern Portugal : provenance and geochemical implications / Rute Salgueiro... [et al.]. - Amsterdam : Elsevier, 2014. - [18] p. : il., 13 figuras e 8 tabelas ; 30 cm The xenotime-bearing heavy mineral assemblages present in the alluvial samples from Vila Velha de Ródão, Nisa, Póvoa e Meadas and Sto. António das Areias, localized in the northern edge of Nisa-Albuquerque Batholith, Eastern Portugal, were studied in detail. The insights for mineral provenance came from the analysis of the drainage network and from the composition of the regional alluvial samples and outcropping lithologies. Since xenotime is a mineral with economic interest, the motivation of the current work is its contribution for exploration studies, considering the potential information contained in the alluvial samples. In the study region, the alluvial heavy minerals and their morphology reflect clearly the mineralogy and relative distance to their source, respectively. In alluvial samples with direct provenance from the Nisa granite (late Carboniferous), the increase in xenotime concentration and decrease in monazite, apatite, zircon, ilmenite and iron oxide concentration, from W (Nisa) to E (Sto. António das Areias), matches the increase in P2O5 and decrease in REE, CaO, Zr, TiO2, and Fe2O3 contents in granite rocks. The geochemical signature of xenotime studied reveals an igneous source, characterized by the characteristic strong Eu negative anomaly in REE patterns. Their YPO4 values (72–78 mol%) are similar to xenotime from Erzgebirge (Germany) granites. The high values of Y/Ho (50–71) and, in some cases, downward kinks at Ho in REE plots, suggest generation in late stages of crystallization and association with a siliceous evolved magmatic system. The slight decrease in HREE contents in xenotime, from W to E, and Ho anomalies in the normalized REE pattern are similar to those identified in the Nisa granite, which supports the sourcing of xenotime from these granitic rocks. The genetic development of the batholith chemical zonation (more evolved to E) seems to have favoured the generation of xenotime instead of apatite, monazite and zircon, in the eastern end area (Sto. António das Areias). Supporting the geochemical signature, the alluvial zircons also display morphological typologies that are compatible with provenance from peraluminous granites formed at temperatures of 600–700 °C, possibly from the Nisa granite. Since all xenotime grains show the same magmatic affinity, this leads to the hypothesis that the xenotime from the Vila Velha de Ródão sample, with provenance from Cenozoic sedimentary rocks, has been transported to this northern area, after been disaggregated from Nisa batholith granites, most probably by braided anastomosing and erratically sandy channels, that explains its actual position in the opposite bank of the Tagus river. This phosphate has been deposited with other sediments in tectonic depressions and subsequently included in the formation of sedimentary rocks. The greater development of Ca, Th and U phosphate inclusions/substitutions in these xenotime grains can be explained by the chemical mobility provided during all the geological processes.
- An insight into the firing conditions of Chinese blue-and-white porcelain through XANESPublication . Coutinho, ML; Veiga, JP; Ruivo, Andreia; Silva, Teresa; Salas-Colera, Eduardo; Bottura Scardina, Silvia; Lima, Augusta; Figueiredo, Elin; Cotte, Marine; Lima, M.M.R.A.ABSTRACT: Chinese blue-and-white porcelain is found in archaeological excavations worldwide, being significant evidence of global trade routes and cultural exchange. Synchrotron radiation-based techniques have been applied for studying cobalt speciation to establish a correlation between the cobalt and iron oxidation state and local coordination environment in the rich blue shades of Chinese blue-and-white porcelain. However, the relationship between the firing atmosphere conditions and the speciation of cobalt has not been established yet. In this study, underglaze blue models were produced and fired in air or under reducing atmospheres to ascertain the effect of the firing atmosphere in cobalt and iron speciation. The experimental results were compared with data obtained on historical samples of ancient porcelain shards. The microstructure and colour of the produced underglaze blue models were investigated by variable pressure scanning electron microscopy (VP-SEM-EDS), using a hyperspectral imaging camera (Vis-SWIR reflectance spectroscopy) and colorimetry. The formal valence and coordination of cobalt and iron ions of the glaze were determined by X-ray absorption spectroscopy (XAS), particularly X-ray absorption near edge structure (XANES), using synchrotron radiation. Spectral features demonstrated that both cobalt and iron speciation were affected by the firing atmosphere and therefore could be used to ascertain the firing atmosphere.
- Ascertaining the degradation state of ceramic tiles : a preliminary non-destructive step in view of conservation treatmentsPublication . Silva, Teresa; Figueiredo, M. Ondina; Prudêncio, Maria IsabelConserving the cultural heritage is a general concern and the use of non-destructive techniques to characterize ancient materials is important. Serious deterioration effects in environmentally exposed ancient glazed ceramic tiles arise from the development of micro-organisms (algae/fungi) within the pore system. Subsequent biodegradation processes are particularly harmful once the decorated glaze is damaged by exfoliation/detachment. Three case studies will be addressed: Portuguese polychrome decorated tiles from the interior of two churches (16th–17th century) and from the outdoor of a Palace (18th century). Small tile fragments were directly irradiated in a wavelength-dispersive X-ray fluorescence spectrometer for glaze chemical characterization and subsequently irradiated in a powder diffractometer to assess the phase constitution of both glaze and ceramic body. Cleaning and conserving these ancient cultural artifacts involve a decontamination process applying innovative non-destructive techniques. The present work is intended as a contribution to diagnose the actual degradation state of ancient tiles in view of future decontamination actions using gamma radiation.
- Assessment of potential contamination and acid drainage generation in uranium mining zones of Peña Blanca, Chihuahua, MexicoPublication . Guzmán-Martínez, Fredy; Arranz‑González, Julio César; Tapia‑Téllez, Alfredo; Prazeres, Cátia; García‑Martínez, María Jesús; Jiménez‑Oyola, SamanthaABSTRACT: Potential pollution of mining environmental liabilities' locations can be preliminarily and efficiently assessed by the potential generation of acid mine drainage and indices of contamination. This research evaluates the potential pollution by potentially toxic elements at locations with uranium mining liability evidence, using the net acid generation test and determining the background values to estimate acid mine drainage and indices of contamination. Sixty soil samples were collected, and the mineralogy and potentially toxic elements' total contents were determined by x-ray diffraction and optical spectrometry. The findings suggest that the soils related to a specific lithology might not present potential acid mine drainage generation but potential soil and sediment contamination. Future research is recommended on applying leaching tests to identify which potentially toxic elements are effectively being solubilized. Finally, it can be concluded that the study area's potential contamination is relatively low overall.
- Biostratigraphic and structural research in the Guedelhinha–Lançadoiras–Algaré sector in the context of the geology of the Neves–Corvo mine region, Iberian Pyrite BeltPublication . Pereira, Zélia; Matos, João Xavier; Mendes, Márcia; Solá, A. Rita; Albardeiro, Luís; Araújo, Vítor; Pacheco, Nelson; Oliveira, José TomásABSTRACT: Based on drill hole sampling and sedimentary rock dating by palynology, the present research focuses on the palynostratigraphic events established in the key geological section of Guedelhinha–Lançadoiras–Algaré located in the Portuguese Neves–Corvo mine region, Iberian Pyrite Belt. The age data allow detailing the lithostratigraphic sequence and further understanding the complex structural setting, representing an important contribution to the geological knowledge of this sector located to the immediate WNW of the Neves–Corvo VMS deposit. The combination of the studied events allows the reconstruction of the Devonian-Carboniferous sedimentation and paleoenvironments along the Iberian Pyrite Belt. Several stratigraphic hiatuses identified in the Neves–Corvo region by the palynological record are confirmed, mainly occurring from the mid Frasnian to mid Famennian, from the early and mid Strunian, and from the early to late Tournaisian, which were mainly coincident with the worldwide extinction events, in particular during Frasnian–Famennian and Late Devonian times. Extensional tectonics and related gravitational faults, local uplift mechanisms and intense volcanic activity could also explain the lack of palynological data and sedimentary hiatus. In this research, the importance of the late Strunian times in the Iberian Pyrite Belt (Miospore Biozone LN of the Neves Formation) is highlighted, confirming the contemporaneity of felsic volcanism, hydrothermalism, sulphide mineralization precipitation and black shale anoxic sedimentation.
- CdTe detector based PIXE mapping of geological samplesPublication . Chaves, P. C.; Taborda, A:; de Oliveira, Daniel Pipa Soares; Reis, M. A.A sample collected from a borehole drilled approximately 10 km ESE of Bragança, Trás-os-Montes, was analysed by standard and high energy PIXE at both CTN (previous ITN) PIXE setups. The sample is a fine-grained metapyroxenite grading to coarse-grained in the base with disseminated sulphides and fine veinlets of pyrrhotite and pyrite. Matrix composition was obtained at the standard PIXE setup using a 1.25 MeV H+ beam at three different spots. Medium and high Z elemental concentrations were then determined using the DT2fit and DT2simul codes (Reis et al., 2008, 2013 [1] and [2]), on the spectra obtained in the High Resolution and High Energy (HRHE)-PIXE setup (Chaves et al., 2013 [3]) by irradiation of the sample with a 3.8 MeV proton beam provided by the CTN 3 MV Tandetron accelerator. In this paper we present results, discuss detection limits of the method and the added value of the use of the CdTe detector in this context.
- Characterization of Tableware from Fábrica de Loiça de Sacavém : Linking Analytical and Documental ResearchPublication . Coutinho, ML; Veiga, JP; Ruivo, Andreia; Silva, Teresa; Bottura Scardina, Silvia; Lima, M.M.R.A.; Pereira, Carlos; Dias, Ana Carvalho; Dias, Luis; Vandenabeele, Peter; Roseiro, J. CarlosABSTRACT: Fabrica de Loica de Sacavem (ca. 1858-1994) was among the first to produce white earthenware in Portugal, becoming one of the country's leading ceramic manufacturers during the late 19th to early 20th centuries. Research on white earthenware has accompanied the growing interest in post-industrial archaeology but is still poorly explored compared to more ancient ceramic productions. This study focused on the ceramic body, glazes, and colourants of tableware produced by Fabrica de Loica de Sacavem during the first 50 years of its activity (1859-1910). A multi-analytical approach was selected to investigate the chemical and mineralogical composition of the ceramic body, glaze, and pigments using optical microscopy, variable-pressure scanning electron microscope energy-dispersive X-ray spectroscopy (VP-SEM-EDS), mu-Raman spectroscopy, mu-X-ray Diffraction (mu-XRD), and reflectance spectroscopy (hyperspectral image analysis). The studied tableware was produced with a Ca-poor siliceous-aluminous white earthenware ceramic body covered with transparent alkali lead or lead borosilicate glaze, and most colourants were complex Cr-based pigments. These results are in agreement with the little documental evidence from this period found in the manufacturer's archives.
- Chemical and Mineralogical Characterization ofWaste from Abandoned Copper and Manganese Mines in the Iberian Pyrite Belt, Portugal: A First Step Towards the Waste-to-Value Recycling ProcessPublication . de Oliveira, Daniel Pipa Soares; Silva, Teresa; Morais, Igor; Fernandes, JoãoABSTRACT: This study examines the chemical and mineralogical composition of waste materials from abandoned copper and manganese mines in the Iberian Pyrite Belt, Portugal, as a first step toward their potential recycling for critical and strategic raw materials (CRM and SRM). Using portable X-ray fluorescence (pXRF) and other analytical techniques, this research highlights the presence of valuable elements, including copper, manganese, and rare earth elements, in concentrations significantly above their crustal abundance. The findings underscore the dual potential of these wastes: as sources of secondary raw materials and for mitigating environmental hazards such as acid mine drainage (AMD). Recovered materials include chalcopyrite, pyrolusite, and rhodochrosite, with critical elements like cobalt, lithium, and tungsten identified. pXRF proved to be a reliable, cost effective tool for rapid field and laboratory analyses, demonstrating high precision and good correlation with standard laboratory methods. The study emphasizes the importance of characterizing historical mining waste to support a circular economy, reduce reliance on foreign material imports, and address environmental challenges. This approach aligns with the European Union’s Critical Raw Materials Act, promoting sustainable resource use and the recovery of strategic resources from historical mining sites.
- Comparability of heavy mineral data - The first interlaboratory round robin testPublication . Dunkla, István; von Eynatten, Hilmar; Andòb, Sergio; Lünsdorf, Keno; Morton, Andrew; Alexander, Bruce; Aradi, László; Augustsson, Carita; Bahlburg, Heinrich; Barbarano, Marta; Benedictus, Aukje; Berndt, Jasper; Bitz, Irene; Boekhout, Flora; Breitfeld, Tim; Cascalho, João; Costa, Pedro J.M.; Ekwenye, Ogechi; Fehér, Kristóf; Flores-Aqueveque, Valentina; Führing, Philipp; Giannini, Paulo; Goetz, Walter; Guedes, Carlos; Gyurica, György; Hennig-Breitfeld, Juliane; Hülscher, Julian; Jafarzadeh, Mahdi; Jagodziński, Robert; Józsa, Sándor; Kelemen, Péter; Keulen, Nynke; Kovacic, Marijan; Liebermann, Christof; Limonta, Mara; Lužar-Oberiter, Borna; Markovic, Frane; Melcher, Frank; Miklós, Dóra Georgina; Moghalu, Ogechukwu; Mounteney, Ian; Nascimento, Daniel; Novaković, Tea; Obbágy, Gabriella; Oehlke, Mathias; Omma, Jenny; Onuk, Peter; Passchier, Sandra; Pfaff, Katharina; Lincoñir, Luisa Pinto; Power, Matthew; Razum, Ivan; Resentini, Alberto; Sági, Tamás; Salata, Dorota; Salgueiro, Rute; Schönig, Jan; Sitnikova, Maria; Sternal, Beata; Szakmány, György; Szokaluk, Monika; Thamó-Bozsó, Edit; Tóth, Ágoston; Tremblay, Jonathan; Verhaegen, Jasper; Villaseñor, Tania; Wagreich, Michael; Wolf, Anna; Yoshida, KohkiABSTRACT: Heavy minerals are typically rare but important components of siliciclastic sediments and rocks. Their abundance, proportions, and variability carry valuable information on source rocks, climatic, environmental and transport conditions between source to sink, and diagenetic processes. They are important for practical purposes such as prospecting for mineral resources or the correlation and interpretation of geologic reservoirs. Despite the extensive use of heavy mineral analysis in sedimentary petrography and quite diverse methods for quantifying heavy mineral assemblages, there has never been a systematic comparison of results obtained by different methods and/or operators. This study provides the first interlaboratory test of heavy mineral analysis. Two synthetic heavy mineral samples were prepared with considerably contrasting compositions intended to resemble natural samples. The contributors were requested to provide (i) metadata describing methods, measurement conditions and experience of the operators and (ii) results tables with mineral species and grain counts. One hundred thirty analyses of the two samples were performed by 67 contributors, encompassing both classical microscopic analyses and data obtained by emerging automated techniques based on electron-beam chemical analysis or Raman spectroscopy. Because relatively low numbers of mineral counts (N) are typical for optical analyses while automated techniques allow for high N, the results vary considerably with respect to the Poisson uncertainty of the counting statistics. Therefore, standard methods used in evaluation of round robin tests are not feasible. In our case the 'true' compositions of the test samples are not known. Three methods have been applied to determine possible reference values: (i) the initially measured weight percentages, (ii) calculation of grain percentages using estimates of grain volumes and densities, and (iii) the best-match average calculated from the most reliable analyses following multiple, pragmatic and robust criteria. The range of these three values is taken as best approximation of the 'true' composition. The reported grain percentages were evaluated according to (i) their overall scatter relative to the most likely composition, (ii) the number of identified components that were part of the test samples, (iii) the total amount of mistakenly identified mineral grains that were actually not added to the samples, and (iv) the number of major components, which match the reference values with 95% confidence. Results indicate that the overall comparability of the analyses is reasonable. However, there are several issues with respect to methods and/or operators. Optical methods yield the poorest results with respect to the scatter of the data. This, however, is not considered inherent to the method as demonstrated by a significant number of optical analyses fulfilling the criteria for the best-match average. Training of the operators is thus considered paramount for optical analyses. Electron-beam methods yield satisfactory results, but problems in the identification of polymorphs and the discrimination of chain silicates are evident. Labs refining their electron-beam results by optical analysis practically tackle this issue. Raman methods yield the best results as indicated by the highest number of major components correctly quantified with 95% confidence and the fact that all laboratories and operators fulfil the criteria for the best-match average. However, a number of problems must be solved before the full potential of the automated high-throughput techniques in heavy mineral analysis can be achieved.