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The fabrication of low-electrical-percolation-threshold polymer composites aims to reduce the weight fraction of the conductive nanomaterial necessary to achieve a given level of electrical resistivity of the composite. The present work aimed at preparing composites based on multiwalled carbon nanotubes (MWCNTs) and magnetite particles in a polyurethane (PU) matrix to study the effect on the electrical resistance of electrodes produced under magnetic fields. Composites with 1 wt.% of MWCNT, 1 wt.% of magnetite and combinations of both were prepared and analysed. The hybrid composites combined MWCNTs and magnetite at the weight ratios of 1:1; 1:1/6; 1:1/12; and 1:1/24. The results showed that MWCNTs were responsible for the electrical conductivity of the composites since the composites with 1 wt.% magnetite were non-conductive. Combining magnetite particles with MWCNTs reduces the electrical resistance of the composite. SQUID analysis showed that MWCNTs simultaneously exhibit ferromagnetism and diamagnetism, ferromagnetism being dominant at lower magnetic fields and diamagnetism being dominant at higher fields. Conversely, magnetite particles present a ferromagnetic response much stronger than MWCNTs. Finally, optical microscopy (OM) and X-ray micro computed tomography (micro CT) identified the interaction between particles and their location inside the composite. In conclusion, the combination of magnetite and MWCNTs in a polymer composite allows for the control of the location of these particles using an external magnetic field, decreasing the electrical resistance of the electrodes produced. By adding 1 wt.% of magnetite to 1 wt.% of MWCNT (1:1), the electric resistance of the composites decreased from 9 × 104 to 5 × 103 Ω. This approach significantly improved the reproducibility of the electrode’s fabrication process, enabling the development of a triboelectric sensor using a polyurethane (PU) composite and silicone rubber (SR). Finally, the method’s bearing was demonstrated by developing an automated robotic soft grip with tendon-driven actuation controlled by the triboelectric sensor. The results indicate that magnetic patterning is a versatile and low-cost approach to manufacturing sensors for soft robotics.

A detailed archaeometric study of Phoenician ceramics found in an excavation inside the medieval walls of Sao Jorge's Castle in Lisbon is described here. Thirty ceramic sherds were studied, grouped into six categories, namely amphorae, containers for domestic use, red slip wares, grey wares, cooking wares and also some indigenous tradition handmade wares. Micro-Raman, X-Ray Fluorescence Emission, X-Ray Diffraction and ground state diffuse reflectance absorption measurements were correlated and used as our main analytical techniques to perform this study. At least three totally different local clay sources were used to produce the here studied pottery, one of alluvial origin using clays collected along the river banks, and another one using clays probably extracted in the oriental part of the Castle's hill. Cooking-ware was made with the use of raw materials with sandy detrital origin. Evidence was also found showing that part of the amphorae, common containers, and grey wares were made with the same raw materials as used in the Phoenician kilns of Almaraz, located in the left margin of the Tagus River, roughly facing Lisbon's Castle hill. The temperatures of the kilns used to fire the amphorae and common containers was in most cases higher than the one used for firing red slip and grey tableware. A detailed laboratorial study of the alluvial clays fired at different temperatures and collected in the Tagus River banks, allowed us, in most cases, to establish the origin of the sources used to produce the Phoenician pottery found in Lisbon.

No envelhecimento acelerado de rochas ornamentais em câmara saturada em SO2, as interações físico-químicas têm o objetivo de simular a exposição das mesmas às chuvas ácidas. As presenças de SO2, de H2O, somadas à incidência de radiação solar (externa) permitem a formação fotoquímica do ácido sulfúrico (H2SO4) e a correlação entre as digitalizações das superfícies dos corpos de prova, antes e após as exposições ao H2SO4, propicia a análise da evolução das alterações causadas. A estimativa do tempo gasto, em anos, para que as alterações descaracterizem totalmente a aparência estética da superfície das amostras é feita com a progressão aritmética do coeficiente de correlação linear de Pearson (r) que permite, quando igual a 0 (zero), afirmar a inexistência de correlação entre imagens de amostras submetidas ao ensaio e suas imagens originais ao natural. Os resultados apontam o Butterfly Gold como o mais susceptível à descaracterização estética superficial (3,08 anos), seguido do Butterfly Green (3,91 anos) e do Butterfly Beige (16,03 anos). Ressalta-se que a descaracterização não implica, necessariamente, em alteração ou comprometimento estrutural ou físico-mecânico da rocha. A concentração do gás na câmara (25 ppm) foi superelevada propositalmente para acelerar o processo de deterioração. É importante lembrar que a câmara simula as condições climáticas em fluxo praticamente contínuo necessitando o pesquisador, para as interpretações, considerar a concentração de SO2 na atmosfera, a duração das estações chuvosas, a incidência de chuvas ácidas e suas intensidades ao longo de um ano nos diferentes territórios. As previsões aqui realizadas não são impeditivos para aplicação destes materiais em ambientes externos nem tampouco internos, pois procedimentos usuais de limpeza podem ser perfeitamente aplicados para conservação dos mesmos.

This work was funded by the Leverhulme Trust (RPG-2015-071). Dr. C. Cousins also wishes to acknowledge funding from the Royal Society of Edinburgh. This work was financed by FEDER - Fundo Europeu de Desenvolvimento Regional funds through the COMPETE 2020 - Operacional Programme for Competitiveness and Internationalisation (POCI), and by Portuguese funds through FCT - Fundação para a Ciência e a Tecnologia in the framework of the project POCI-01-0145-FEDER-029932 (PTDC/FIS-AST/29932/2017). Exogenous organic molecules are delivered to the surface of Mars annually, yet their fate is largely unknown. Likewise, the survivability of putative organic biomarkers directly implicates current Mars surface exploration ambitions. Among these, amino acids are valuable target molecules due to their abiogenic and biological origins. We present the fundamental, but not previously considered, factors that affect the fate of amino acids embedded in Mars mineral analogues when exposed to ionising radiation. Using existing experimental datasets, we show that the attenuation coefficient at 200 nm for amino acids is an effective parameter for quantifying organic survivability, especially when mineral shielding is limited or absent. Conversely, the dielectric constant of a material is a potential key parameter regarding mineral shielding, as it accounts for iron content, and the physical properties of the material (pore size, surface area or water content). Finally, we combine Martian climatic parameters (surface temperature and atmospheric opacity) to show that the relative UV environment varies significantly on Mars as a function of latitude, providing a reference point for future Mars simulation studies. Postprint

In this study, low-carbon recycled cement (RC) was produced from thermally activated concrete and cement paste wastes and its incorporation in mortars, as cement replacement, was investigated. The calcination temperatures were defined based on thermogravimetric and X-ray diffraction analysis. Mortars were characterized in terms of their main fresh and mechanical properties (compressive and flexural strength, ultrasonic pulse velocity and dynamic modulus of elasticity). The influence of RC replacement ratio (20%, 50%, 75% and 100%), RC treatment temperature and RC fineness were analyzed. In all tested properties, RC from concrete waste showed significant lower efficiency than that from cement paste waste. The RC rehydration capacity was improved by increasing its fineness and pre-heating temperature. Mortars produced with 100% of 650 °C pre-heated RC were able to attain as high as 8.3 MPa of compressive strength at 28 days, corresponding to about 20% of that found in reference mortars without RC. In addition, mechanical properties were little affected by RC replacement ratios up to 20%. This study shows the efficient rehydration capacity of thermal activated RC and suggests its high potential for the construction industry.

The fraction of organic matter present affects the fragmentation behavior of sialoliths; thus, pretherapeutic information on the degree of mineralization is relevant for a correct selection of lithotripsy procedures. This work proposes a methodology for in vivo characterization of salivary calculi in the pretherapeutic context. Sialoliths were characterized in detail by X-ray computed microtomography (μCT) in combination with atomic emission spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Correlative analysis of the same specimens was performed by in vivo and ex vivo helical computed tomography (HCT) and ex vivo μCT. The mineral matter in the sialoliths consisted essentially of apatite (89 vol%) and whitlockite (11 vol%) with average density of 1.8 g/cm3. In hydrated conditions, the mineral mass prevailed with 53 ± 13 wt%, whereas the organic matter, with a density of 1.2 g/cm3, occupied 65 ± 10% of the sialoliths’ volume. A quantitative relation between sialoliths mineral density and X-ray attenuation is proposed for both HCT and μCT.

Findings of Iron Age metallurgical activities related to tin metal and mining are very rare. In the present work, we present a detailed study of the Outeiro de Baltar hillfort, dated to the Late Iron Age/Early Roman period, located in a place where 20th century tin mining work took place. Elemental and microstructural analysis by portable, micro and wavelength dispersive X-ray fluorescence spectrometry (pXRF, micro-XRF and WDXRF) and scanning electron microscopy with energy dispersion spectrometer (SEM-EDS) showed that metallurgical debris found at the archaeological site is related to tin smelting and binary and ternary bronze productions. Analysis of the artefacts of diverse typologies found at the site showed that a variety of metals and alloys were in circulation and use. Samples of tin ores (cassiterite) from the region were analyzed for comparison with an archaeological tin slag from the site. The analytical results point to the production of tin metal using local cassiterite and the production of bronze by directly adding cassiterite into a smelting process. Furthermore, data of remote sensing (airborne Light Detection and Ranging (LiDAR) and historical aerial imagery) and Geographical Information System (GIS) mapping were combined with archival mining documentation and maps to retrieve a landscape context for the site. The study showed that the place of the Outeiro de Baltar hillfort (NW Iberia) was mined periodically over time. publishersversion published

The use of vegetable oils to produce biodiesel raises several sustainability issues, namely the fuel/food conflict. The high cost of vegetable oils and an expensive homogeneous base catalyzed process encourages the search for alternative raw materials and more efficient production processes. Biodiesel from beef tallow, a non-edible fat, was produced by methanolysis over calcium based heterogeneous catalyst. The catalyst was prepared by calcination of scallop shells at 800 ​°C. To overcome the undesired effect of the tallow acidity (3.9 mgKOH/gfat), mixtures of tallow and soybean oil (SBO) (0.6 mgKOH/gfat) were processed and alcohol co-solvents (isopropanol, 1-propanol, and isobutanol) and biodiesel itself, as a solvent, were used to improve the miscibility of the reaction mixture. Processing of neat tallow promotes an important decay of the catalytic activity due to the partial neutralization of the basic catalyst. Co-processing mixtures of tallow/SBO allowed minimizing the acidity effect. Alcohol co-solvents harmed the biodiesel yield due to competitive adsorption of alcohols with methanol on catalyst active sites but protected the catalyst against adsorption of the reaction mixture species. Biodiesel used as a solvent had an almost null effect on the esterification reaction yield, thus showing the absence of mass transfer limitation. Co-processing low-grade fat with vegetable oil seems to be a feasible strategy to process low-grade fats using basic heterogeneous catalysts, thus contributing to improving the sustainability of biodiesel production.

The on-board identification of ore minerals during a cruise is often postponed until long after the cruise is over. During the M127 cruise, 21 cores with deep-seafloor sediments were recovered in the Trans-Atlantic Geotraverse (TAG) field along the Mid Atlantic Ridge (MAR). Sediments were analyzed on-board for physicochemical properties such as lightness (L*), pH and Eh. Selected samples were studied for mineral composition by X-ray powder diffraction (XRD). Based on XRD data, sediment samples were separated into high-, low- and non-carbonated. Removal of carbonates is a common technique in mineralogical studies in which HCl is used as the extraction agent. In the present study, sequential extraction was performed with sodium acetate buffer (pH 5.0) to remove carbonates. The ratio between the highest calcite XRD reflection in the original samples (Iorig) vs its XRD-reflection in samples after their treatment with the buffer (Itreat) was used as a quantitative parameter of calcite removal, as well as to identify minor minerals in carbonated samples (when Iorig/Itreat &gt, 24). It was found that the lightness parameter (L*) showed a positive correlation with calcite XRD reflection in selected TAG samples, and this could be applied to the preliminary on-board determination of extraction steps with acetate buffer (pH 5.0) in carbonated sediment samples. The most abundant minerals detected in carbonated samples were quartz and Al- and Fe-rich clays. Other silicates were also detected (e.g., calcic plagioclase, montmorillonite, nontronite). In non-carbonated samples, Fe oxides and hydroxides (goethite and hematite, respectively) were detected. Pyrite was the dominant hydrothermal mineral and Cu sulfides (chalcopyrite, covellite) and hydrothermal Mn oxides (birnessite and todorokite) were mineral phases identified in few samples, whereas paratacamite was detected in the top 20 cm of the core. The present study demonstrates that portable XRD analysis makes it possible to characterize mineralogy at cored sites, in particular in both low- and high-carbonated samples, before the end of most cruises, thus enabling the quick modification of exploration strategies in light of new information as it becomes available in near-real time.

22 páginas.-- 6 figuras.-- 115 referencias.-- Additional Supporting Information may be found in the online version of this article: http://dx.doi.org/10.1111/sed.12431, Subsurface granitic environments are scarce and poorly investigated. A multi‐disciplinary approach was used to characterize the abundant moonmilk deposits and associated microbial communities coating the granite walls of the 16th Century Paranhos spring water tunnel in Porto city (north‐west Portugal). It is possible that this study is the first record of moonmilk in an urban subsurface granitic environment. The morphology and texture, mineralogical composition, stable isotope composition and microbial diversity of moonmilk deposits have been studied to infer the processes of moonmilk formation. These whitish secondary mineral deposits are composed of very fine needle‐fibre calcite crystals with different morphologies and density. Calcified filaments of fungal hyphae or bacteria were distinguished by field emission scanning electron microscopy. Stable isotope analysis revealed a meteoric origin of the needle‐fibre calcite, with an important contribution of atmospheric CO2, soil respiration and urn:x-wiley:00370746:media:sed12431:sed12431-math-0001 from weathering of Ca‐bearing minerals. The DNA‐based analyses revealed the presence of micro‐organisms related to urban contamination, including Actinobacteria, mainly represented by Pseudonocardia hispaniensis, Thaumarchaeota and Ascomycota, dominated by Cladosporium. This microbial composition is consistent with groundwater pollution and contamination sources of the overlying urban area, including garages, petrol stations and wastewater pipeline leakage, showing that the Paranhos tunnel is greatly perturbed by anthropogenic activities. Whether the identified micro‐organisms are involved in the formation of the needle‐fibre calcite or not is difficult to demonstrate, but this study evidenced both abiotic and biogenic genesis for the calcite moonmilk in this subsurface granitic environment., The authors acknowledge the Spanish Ministry of Economy, Industry and Competitiveness (MINEICO, project CGL2011-2569) and the Portuguese Foundation for Science and Technology, FCT (UID/GEO/04035/2013, UID/ECI/04028/2013, PEst-OE/CTE/UI0098/2011) and the LABCARGA| ISEP re-equipment program (IPP-ISEP|PAD’2007/ 08) for financial support. AZM thanks MINEICO for the ‘Juan de la Cierva – Incorporación’ postdoctoral contract (IJCI-2014-20443). PMMS thanks the Spanish Ministry of Science and Innovation for his contract associated with the ‘Research Programme in Technologies for the Assessment and Conservation of Cultural Heritage’ (TCP CSD2007-0005

São estudadas as rochas ornamentais Butterfly Beige, Butterfly Gold e Butterfly Green correspondentes a quartzo sienitos com hiperstênio que são exploradas em Barra de São Francisco-Espírito Santo, Brasil. O objetivo é analisar os efeitos estéticos, bem como quantificá-los, depois de submetidas à exposição de temperaturas elevadas a partir de análises comparativas das imagens, das cores e das respectivas características petrográficas. Os valores para os coeficientes de correlação (r) entre as rochas, já nos primeiros 200ºC, mostram descaracterizações moderadas, sendo as rochas bastante afetadas pela temperatura. As alterações causadas pela ciclagem térmica somada à umidade aceleram o processo de oxidação do Fe. Além disso, por histerese, a ciclagem implica a geração de microfissuras e o alargamento dos planos de clivagem dos minerais, bem como ofusca os contatos entre eles, facilitando a percolação de fluidos (água) e aumentando o grau de oxidação do Fe ao mesmo tempo em que facilita a disseminação do Fe(OH)2. Frente aos resultados obtidos, sugere-se que as rochas estudadas (principalmente a variedade Green) sejam utilizadas em revestimentos de ambientes internos e que fontes de calor, como o sol, em revestimentos externos, podem acelerar o processo de modificação das cores em função da presença de minerais ferro-magnesianos e, principalmente, do Fe (OH)2 passíveis de oxidação

The recovery of lithium from hard rock minerals has received increased attention given the high demand for this element. Therefore, this study optimized an innovative process, which does not require a high-temperature calcination step, for lithium extraction from lepidolite. Mechanical activation and acid digestion were suggested as crucial process parameters, and experimental design and response-surface methodology were applied to model and optimize the proposed lithium extraction process. The promoting effect of amorphization and the formation of lithium sulfate hydrate on lithium extraction yield were assessed. Several factor combinations led to extraction yields that exceeded 90%, indicating that the proposed process is an effective approach for lithium recovery. info:eu-repo/semantics/publishedVersion

Separation is a fundamental step for concrete recycling, enabling not only the achievement of reliable and cleaner recycled aggregates but also the better re-use of the remaining concrete constituents. Recently, a new hydraulic binder produced from the hydrated cement paste contained in waste concrete, which is associated with lower processing temperatures and carbon dioxide emissions, has gained momentum in the history of concrete recycling. However, a decisive turning point for its application lies in the successful individualisation of the cement paste and aggregate initially contained in concrete debris. This paper describes a new patented method involving a mechanical comminution stage and a high-intensity magnetic separation process to obtain the cementitious fraction in concrete and retrieve cleaner fine aggregate. The efficiency of the proposed method was assessed through image analysis, thermogravimetry, X-ray diffraction and acid attack. In addition, cement pastes produced with the obtained recycled cement after thermal activation were characterised in terms of mechanical strength. Findings suggest that the proposed method effectively separated the main concrete constituents, especially when the waste material was reduced to the size range 150–500 μm. It was possible to obtain a recycled binder at the current laboratory scale with up to about 80% cement content by weight (nearly 90% in volume). Furthermore, a cleaner recycled fine aggregate, with minimal cement paste contamination, as low as less than 3 wt%, was also obtained. The mechanical strength of pastes with recycled cement retrieved from waste concrete was about 70% of that of reference pastes of equal water/binder produced with recycled cement from non-contaminated waste cement pastes.

Lithotripsy methods show relatively low efficiency in the fragmentation of sialoliths compared with the success rates achieved in the destruction of renal calculi. However, the information available on the mechanical behavior of sialoliths is limited and their apparently tougher response is not fully understood. This work evaluates the hardness and Young’s modulus of sialoliths at different scales and analyzes specific damage patterns induced in these calcified structures by ultrasonic vibrations, pneumoballistic impacts, shock waves, and laser ablation. A clear correlation between local mechanical properties and ultrastructure/chemistry has been established: sialoliths are composite materials consisting of hard and soft components of mineralized and organic nature, respectively. Ultrasonic and pneumoballistic reverberations damage preferentially highly mineralized regions, leaving relatively unaffected the surrounding organic matter. In contrast, shock waves leach the organic component and lead to erosion of the overall structure. Laser ablation destroys homogeneously the irradiated zones regardless of the mineralized/organic nature of the underlying ultrastructure; however, damage is less extensive than with mechanical methods. Overall, the present results show that composition and internal structure are key features behind sialoliths’ comminution behavior and that the organic matter contributes to reduce the therapeutic efficiency of lithotripsy methods.

The consumption of edible pine seeds of stone pine by the invasive Leptoglossus occidentalis represents a major concern for producers in Mediterranean countries but, to date, little knowledge is available about its feeding process on these seeds. In the present study, we tested whether L. occidentalis is capable of feeding upon mature pine seeds and also estimated the impact that they may induce. Sound pine seeds were offered to bugs under laboratory conditions. Seed content was analyzed via a multitechnique approach using a stereomicroscope, X-rays and microcomputed tomography, which was expected to better characterize the damage caused by this bug. Adults of L. occidentalis were capable of feeding on mature seeds by piercing the hard and thick coat. However, the consumption was low and demonstrated a slow start, presumably as a result of the time and effort taken to drill a feeding hole. A collaborative feeding process was suggested because all bugs in the same box appeared to have fed through the same hole in most cases. Consumption was estimated to be approximately one-fifth of a seed kernel per bug per month. Consumed kernels appeared skunked and wrinkled.

15 páginas.- 5 figuras.- 85 referencias.- The following are available online at http://www.mdpi.com/2079-6412/10/11/1134/s1 .- This article belongs to the Special Issue Biofilms on Cultural Heritage, The Galapagos Islands (Ecuador) have a unique ecosystem on Earth due to their outstanding biodiversity and geological features. This also extends to their subterranean heritage, such as volcanic caves, with plenty of secondary mineral deposits, including coralloid-type speleothems and moonmilk deposits. In this study, the bacterial communities associated with speleothems from two lava tubes of Santa Cruz Island were investigated. Field emission scanning electron microscopy (FESEM) was carried out for the morphological characterization and detection of microbial features associated with moonmilk and coralloid speleothems from Bellavista and Royal Palm Caves. Microbial cells, especially filamentous bacteria in close association with extracellular polymeric substances (EPS), were abundant in both types of speleothems. Furthermore, reticulated filaments and Actinobacteria-like cells were observed by FESEM. The analysis of 16S rDNA revealed the presence of different bacterial phylotypes, many of them associated with the carbon, nitrogen, iron and sulfur cycles, and some others with pollutants. This study gives insights into subsurface microbial diversity of the Galapagos Islands and further shows the interest of the conservation of these subterranean geoheritage sites used as show caves, This research was funded by the Ecuadorian Ministry of Environment (Project PC-65-14 National Park Galapagos), by the Spanish project MINECO CGL2016-75590-P with European Regional Development Fund and the Portuguese Foundation for Science and Technology (Fundação para a Ciência e a Tecnologia-FCT) under the project UID/Multi/04449/2019 for HERCULES/UE. AMGS was supported by a FPU fellowship of the Spanish Ministry of Education, Culture and Sport (AP2010-2052). AZM was supported by a Marie Curie Intra-European Fellowship of the European Commission’s 7th Framework Programme (PIEF-GA-2012-328689-DECAVE) and a CEECIND/01147/2017 contract from FCT. MLC was supported by a CEECIND/00349/2017 contract from FCT. FG was financially supported by the “HIPATIA” research program of the University of Almeria.

11 páginas.- 7 figuras.- 1 tabla.- 73 referencias.- Supplementary data to this article can be found online a https://doi.org/10.1016/j.scitotenv.2019.134321, Siliceous speleothems frequently reported in volcanic caves have been traditionally interpreted as resulting from basalt weathering combined with the activity of microbial communities. A characteristic feature in lava tubes from Hawaii, Azores and Canary Islands is the occurrence of black jelly-like speleothems. Here we describe the formation process of siliceous black speleothems found in a lava tube from La Palma, Canary Islands, Spain, based on mineralogy, microscopy, light stable isotopes, analytical pyrolysis, NMR spectroscopy and chemometric analyses. The data indicate that the black speleothems are composed of a hydrated gel matrix of amorphous aluminum silicate materials containing charred vegetation and thermally degraded resins from pines or triterpenoids from Erica arborea, characteristic of the overlying laurel forest. This is the first observation of a connection between fire and speleothem chemistry from volcanic caves. We conclude that wildfires and organic matter from the surface area overlying caves may play an important role in the formation of speleothems found in La Palma and demonstrate that siliceous speleothems are potential archives for past fires., A.Z. Miller acknowledges the support from the Marie Curie Intra-European Fellowship of the European Commission seventh Framework Fig. 6. Contour van Krevelen density plots displaying cumulative abundances of pyrolysis compounds identified in Table S2 for: A) Erica arboreabiomass, B) Andosol topsoil, C) Black jelly-like speleothem 1 (BS1), and D) Black jelly-like speleothem 2 (BS2).9A.Z. Miller et al. / Science of the Total Environment 698 (2020) 134321 Programme (grant PIEF-GA-2012-328689) and the CEECIND/01147/2017 contract funded by Fundação para a Ciência e a Tecnologia (Portugal). The authors acknowledge the Spanish Ministry of Economy and Competitiveness (project CGL2013-41674-P) and ERDF funds forfi-nancial support. The authors are grateful to the speleologist OctavioFernández (GE Tebexcorade–La Palma) for the assistance during thefield trip and photographic documentation in the lava tubes from LaPalma Island

Calcium diglyceroxide (CaD) was used as the catalyst for biodiesel production through oil methanolysis. It was evaluated its catalytic behavior, its air expo- sure tolerance, and the Ca leaching. CaD catalyst was synthesized from food waste scallop shell derived CaO (obtained by calcination at 900 °C) by contacting with a mixture of equal volumes of glycerin and methanol at 65 °C for 2 h. The CaO obtained by calcination of scallop shell was used as reference catalyst. In standard reaction conditions (2.5 h, methanol reflux temperature, 5 wt% (oil basis) catalyst loading, and methanol:oil = 12:1 moral ratio), CaD presented lower catalytic activity than CaO (FAME yield of 92% against 99%, respectively). 24 h repined CaD presented improved catalytic behavior probably due to the formation of surface Ca −OH groups, achieving 96% of FAME yield. Thermogravimetry (TG) data showed that inorganic residue was larger for biodiesel than for glycerin, being CaD catalyst more soluble than CaO. Data showed that CaD is unstable under reaction conditions, suffering leaching, but the absence of Matter Organic Non-Glycerol (MONG) in the glycerin phase allows to neglect the homogeneous contribution of the leached catalyst. CaD formation during reaction contributes to FAME contamination with Ca and promotes catalyst deactivation thus being an undesired occurrence.

The present study aims at evaluating the impact of anobiid damage on pine timber elements. Anobiid attack produces a diffuse damage of the elements with a set of tunnels in random directions and sizes, thus confusing quantification. Therefore, a method was developed based on X-ray micro-computed tomography (μ-XCT) to obtain, for naturally infested timber samples, an empirical correlation between lost material percentage (consumed by beetles) and timber apparent density (original, before degradation—OTD and residual, after degradation—RTD). The quantified density loss can then be used in further assessment of the structure. The results of the tests performed showed high correlation between original apparent density and lost material percentage (r2 = 0.60) and between residual apparent density and lost material percentage (r2 = 0.83), which confirms μ-XCT as a valuable tool to the required quantification. The loss of density results can be further applied on the definition of an assessment method for the evaluation of the residual strength of anobiids infested timber, thus contributing to reducing unnecessary replacement. The optimized procedure of the μ-XCT study for infested Maritime pine (Pinus pinaster) is presented and discussed in this article., The authors acknowledge the support given by Portuguese Foundation for Science and Technology (FCT) within research projects: PTDC/EPH-PAT/4684/2014 (DB-HERITAGE), PTDC/ECM-EST/1072/2014 (Pro-Timber), Pest-OE/CTE/UI4028/2011 (CERENA) and UIDB/ 04625/2020 (CERIS).

Considerable amounts of municipal solid waste incinerator bottom ashes are produced yearly without an adequate outlet. Given the established reactivity of the ash when subjected to an alkali medium, there is considerable scope to valorize it within the Construction industry in an alkali-activated material, thereby reducing the significant environmental pressure of the cement industry. This study assesses the optimization of alkali-activated mortars, using milled municipal solid waste incinerator bottom ash as a precursor, from mechanical and durability behaviour perspectives, many properties of which have never been analysed. The alkaline solution is comprised of either NaOH or Na2SiO3 (Na2O/precursor ratio varying between 9.1% and 24.2% and SiO2/Na2O ratios of 0 or 1.0); fly ash from a coal-fired power plant was also used as control precursor. X-ray fluorescence and powder X-ray diffraction analyses of cement, fly ash, bottom ash and of the resulting pastes were carried out. All specimens were evaluated in terms of their mechanical and durability-related performance (i.e. flexural and compressive strength, carbonation, water absorption by capillary action, and shrinkage). Considerable generation of H2 gas was observed during production, resulting from the reaction between the bottom ashes’ metallic aluminium fraction and the NaOH solution, leading to significant expansion and an overall increase in porosity and thus a strong decline in performance. Alkali-activated bottom ash specimens presented fast carbonation, resulting in a considerable strength increase. Despite the low performance of most of these mixes, the strength enhancement of specimens subjected to some conditions infers that there is significant scope for further mix design optimization (e.g. aluminium reduction, mixing time, Na2O/precursor and SiO2/Na2O ratios) that can lead to the manufacture of fit-for-industry construction materials.

Milled municipal solid waste incinerator bottom ash was used as a precursor in the production of alkali-activated mortars with recycled concrete aggregates as a sand substitute. Fly ash was used as control precursor and sodium hydroxide as an alkaline activator. Different thermal curing regimens were used: 24 h in ambient conditions; 24 h/70 °C; 48 h/70 °C; and 24 h/90 °C. Mechanical and durability-related performances were evaluated (i.e. flexural and compressive strength, modulus of elasticity, ultrasonic pulse velocity, carbonation, capillary water absorption, and shrinkage). The reaction between metallic aluminium from municipal solid waste incinerator bottom ash and OH− ions produced hydrogen gas, causing expansion, porosity increase and thus decline in performance. Low stability in high relative humidity settings due to leaching of highly soluble compounds was also observed. A further decline in performance was observed in mixes containing recycled aggregates. Alkali activated municipal solid waste incinerator bottom ash presented fast carbonation but also a considerable strength enhancement.

São Domingos sulfide mine was shut down more than 50 years ago leaving behind eroded and depositional surfaces due to acid mine drainage (AMD). The aim of this study was to assess six selected sites subjected to AMD, considered phytotoxic regions characterized by vegetation scarcity. Two main criteria, nature and composition of soluble fractions and total chemistry of surficial products related to jarosites presence, enabled to set up an overall dichotomy between superficial proximal/discharge and distal/sedimentation areas. Wet and dry sieving results comparison revealed that samples have a predominant sandy texture and lithic (phyllite, quartzite and volcanic country rocks) composition. Quartz, and subordinate feldspar enrichment is also detected in the coarse silt fraction. The results also suggest that the materials under study, when subjected to the local torrential hydrologic regime, have a high mechanical vulnerability, facilitating erosion and mud transport, both critical for vegetation support, and triggering contamination transfer and dispersion. The vicinity and ground-level surfaces of discharging areas are enriched in the jarosite group minerals whereas the sedimentation ones present hypersaline aluminous tendency. The formation of jarosite is considered as an efficient positive environmental contribution to metals and metalloids sequestration/immobilization. The remediation/revegetation solutions to be adopted in each location must have into consideration these differentiating aspects.

Stone coatings, biological colonization, efflorescence and detachments are frequent on granitic surfaces of our cultural heritage infrastructure. In order to find the different origins for each deterioration form, this paper studies and compares several coatings, efflorescence and flakes found on granitic surfaces of bridges from different ages built in the same area (Ourense in NW Iberian Peninsula at 90 km from the sea) under the same environmental and traffic conditions. The most recent bridge was the New Bridge built in the beginning of 20th century and the oldest one was the Roman Bridge with the 1st century AD foundations but its current structure was built in 17th century. The New Bridge has exhibited a greater variety of deterioration forms such as black crusts, carbonate crusts, efflorescence and biological colonization. On the Roman Bridge, black crusts, efflorescence to a greater extent, and flakes associated with salt crystallization processes have been identified. Scanning electron microscopy with energy dispersive X-ray spectroscopy, X-ray diffraction and Fourier transform infrared (FTIR) spectroscopy studies were carried out in order to establish their composition, and optical and electronic microscopies and X-ray microtomography were used to study their morphologies. As a result, anthropogenic factors (industrial activities, traffic pollution and fertilizers) are considered to be the main contributors to crusts, efflorescence and flake formation on both studied substrates (granite ashlars and mortars). To a lesser extent, natural factors (marine influence and bird droppings) should be taken into account.

A Cu 12 Sb 3.6 Bi 0.4 S 10 Se 3 glass was prepared by melt spinning and crystallized by heat treatments at selected temperatures, the total preparation procedure taking less than one day. The sample characterization by powder X-ray diffraction, scanning and transmission electron microscopy complemented with EDS indicate the formation of compact materials, with a tetrahedrite relative weight fraction higher than 90% when treated at temperatures close to the crystallization peaks (∼200° C). Selenium enters the tetrahedrite structure, while bismuth precipitates in submicron and nanosized spherical shape phases depleted in copper and enriched in antimony, sulfur and selenium (when compared with the matrix composition). The characterization of electrical transport properties (electrical resistivity and Seebeck coefficient) indicate a behavior similar to that obtained by other methods on Cu 12 Sb 4 S 13 , with a maximum power factor of ∼400 μW/K 2 m at room temperature.

Tissue engineering is responsible for developing biological substitutes that restore, maintain or improve tissue function. A solution to achieve this is to implant scaffolds on the affected tissue. These support structures will be responsible for cell protection, oxygenation and nutrition, while supporting mechanical loads during the regeneration process. They should also be biodegradable in order to be gradually replaced by healthy tissue. From the available scaffolds manufacturing techniques, fused filament fabrication has been used recently. This technique does not use organic solvents and has the ability to produce complex geometries. In this paper the influence of manufacturing parameters was assessed. Different temperatures, extrusion speeds, filament offset distances and layer thicknesses were tested and their effect analyzed regarding scaffold morphology and mechanical properties. By decreasing the filament offset distance, three different scaffolds porosities were obtained, increasing the mechanical properties. Combining higher printing temperatures with slow extrusion speeds and low layer thickness, a maximum yield stress of 28 ​MPa and apparent compressive modulus of 942 ​MPa were obtained. With these preferred parameters, two different manufacturing schemes and geometries were tested. While using a double layer printing scheme one obtains an average of 70% increase in mechanical properties, using a staggered configuration can decrease mechanical properties up to 84%.

A detailed archaeometric study of pottery was made of a fifteenth-to-sixteenth-century kiln located inside the walls of the Castle of Alenquer. The locally collected sherds are lead glazed, and mostly exhibit a green or dark yellow decoration. Only in one case, a fragment of a bowl, tin oxide was detected in the white glaze. Pastes from the ceramics of the Alenquer kiln were spectroscopically characterized in terms of their mineralogical and elemental composition. This pottery was fired twice, the first time at high temperatures to produce the biscotto, and the second time at lower temperatures to glaze the ceramics. Although only one type of raw material collected locally was used, two types of ceramic pastes were detected and organized into two groups: one produced at about 850 °C and another at about 950 °C. Pastes from Group 1 were converted into Group 2 pastes whenever the temperature of the kiln was raised from 850 to 950 °C, as confirmed by firing Group 1 pastes in an oven. These results were compared with those obtained for coeval ceramics, namely at Santo Antonio da Charneca and Mata da Machada. Both kilns were located on the south shore of the river Tagus (Lisbon), as previously reported. The first archaeometric study of ceramics produced in the kiln of Alenquer, (Portugal, fifteenth to sixteenth centuries) is reported, with the use of surface spectroscopies techniques, namely micro-Raman. Significant differences were found from two coeval kilns also located at the Tagus basin, Santo Antonio da Charneca and Mata da Machada.

In this work, the initial results of the type testing of the LiF:Mg,Cu,P (TLD-100H) whole-body personal dosemeters are presented. An assessment of reproducibility, linearity of the response, the residual signal as a function of the dose, energy and angular dependence of the response was performed. In general, the dosemeters show good reproducibility for different dose values and a linear behaviour for a range between 0.1 and 300 mSv. The detection limits obtained are lower than 50 μSv. The system presents a good energy and angular response for different radiation qualities.

The oldest kilns producing tin glaze wares discovered in the region of Lisbon were located in the south shore of Tagus river at Santo Antonio da Charneca (SAC) and Mata da Machada (MM). Firing this type of pottery from the fourth quarter of the 15th century to mid-16th century, they were located about 20 km away from central Lisbon. Many other examples of ceramics produced in Lisbon workshops from that period are also known and exist in museums or archaeological collections, in spite of the fact that only one kiln dated from that period was found in Lisbon until now. Therefore, the spectroscopic characterization of ceramics found in Lisbon archaeological contexts (attributed to Lisbon workshops) – and also from SAC or MM – was needed and was performed here. Sherds representative of these faience production centres in the Lisbon region dated from the 16th/17th centuries were studied with the use of non-invasive spectroscopies, namely micro-Raman, Ground State Diffuse Reflectance Absorption (GSDR) and X-ray fluorescence emission (XRF). X-ray diffraction (XRD) experiments were also performed. Also clays were collected both in the North and South shores of the river Tagus, as much as possible from the same clay sources as used in the initial workshops. The obtained results evidence a clear similarity in the pastes of the pottery of the Lisbon region, quartz, gehlenite and diopside (or augite) being the major components. Clays are from Miocene origin, but differences between the ceramic pastes were detected pointing to the use of several clay sources. The spectroscopic trend exhibited at SAC and MM pottery is remarkably different, quartz being the major component of those pastes, and clays are from Pliocene origin.

11 páginas.-- 6 figuras.-- 1 tablas- 67 referencias.-- Supplementary information accompanies this paper at https://doi.org/10.1038/s41598-018-20393-2, Microbial diversity in lava tubes from Canary Islands (Spain) has never been explored thus far offering a unique opportunity to study subsurface microbiology. Abundant yellow coloured mats developing on coralloid speleothems in a lava tube from La Palma Islands were studied by next-generation sequencing and DNA/RNA clone library analyses for investigating both total and metabolically active bacteria. In addition, morphological and mineralogical characterization was performed by field emission scanning electron microscopy (FESEM), micro-computed tomography, X-ray diffraction and infrared spectroscopy to contextualize sequence data. This approach showed that the coralloid speleothems consist of banded siliceous stalactites composed of opal-A and hydrated halloysite. Analytical pyrolysis was also conducted to infer the possible origin of cave wall pigmentation, revealing that lignin degradation compounds can contribute to speleothem colour. Our RNA-based study showed for the first time that members of the phylum Actinobacteria, with 55% of the clones belonging to Euzebyales order, were metabolically active components of yellow mats. In contrast, the DNA clone library revealed that around 45% of clones were affiliated to Proteobacteria. Composition of microbial phyla obtained by NGS reinforced the DNA clone library data at the phylum level, in which Proteobacteria was the most abundant phylum followed by Actinobacteria., Tis research was supported by the Spanish Ministry of Economy, Industry and Competitiveness (MINEICO), project CGL2013–41674-P. J.L.G-P. and A.Z.M. were supported by a PhD fellowship (BES-2014–069587) and a “Juan de la Cierva – Incorporación” post-doctoral contract (IJCI-2014–20443) from the MINEICO, respectively. Te Portuguese Foundation for Science and Technology (Strategic project UID/ECI/04028/2013) are also thanked for fnancial support. Te authors would like to thank the assistance during the feld work and photographic contributions in La Palma lava tubes of the speleologist Octavio Fernandez. We gratefully acknowledge the collecting permissions granted by the staf of Caldera del Taburiente National Park (La Palma Island, Spain).

The main factors that affect the extraction of metals from spent lithium-ion batteries by acid leaching using H2SO4, and sodium metabisulphite, were evaluated and optimized through a set of experiments, framed by a techno-economic approach. The maximum value of the profit response was obtained with the highest possible values of acid concentration (2.5 M) and time (2 h), a liquid/solid ratio of 5 L/kg, and the lowest possible value of temperature (40 degrees C). After leaching, the electrodes active material contained in the metals decreased, while it was still significant in the graphite, as observed by scanning electron microscopy-energy dispersive spectrometry and x-ray powder diffraction. Even though the performed economic evaluation was a summarized outline it can be considered suitable to compare different leaching conditions and to determine the possible best combinations of factors that can optimize the profit response. info:eu-repo/semantics/publishedVersion

Lithium extraction from hard-rock ores has regained importance due to the increased demand for this metal to supply the growing battery market. Therefore, several studies have been focused on the lithium extraction from ores, however, leaching and purification steps are sparsely studied. Thus, the objective of this study was to evaluate the main factors affecting the water leaching step and the subsequent purification operations for lithium recovery from a lepidolite concentrate, which was processed by mechanical activation and sulphuric acid digestion. In the leaching step, among the variables studied, only one, the leaching temperature, showed a significant effect on the lithium extraction, taking into account the range of values tested. Thus, the recommended operating value for the leaching time and the L/S ratio is the minimum, while for the leaching temperature is 50°C. After optimizing the leaching operation, the purification of the leachate, by neutralization, was thoroughly performed by efficient removal of impurities (Fe, Al, Mn and Ca), allowing to obtain lithium carbonate as final product, as well as other relevant by-products, such as rubidium and potassium alums. info:eu-repo/semantics/publishedVersion

The hydrometallurgical extraction of metals from spent lithium-ion batteries (LIBs) was investigated. LIBs were first dismantled and a fraction rich in the active material was obtained by physical separation, containing 95% of the initial electrode, 2% of the initial steel and 22% of plastic materials. Several reducers were tested to improve metals dissolution in the leaching step using sulphuric acid. Sodium metabisulphite led to the best results and was studied in more detail. The best concentration of Na2S2O5 was 0.1 M. The metals dissolution increased with acid concentration, however, concentrations higher than 1.25 M are unnecessary. Best results were reached using a stirring speed of 400 min(-1). The metals leaching efficiency from the active material (Li, Mn, Ni, Co) increased with the temperature and was above 80% for temperatures higher than 60 degrees C. The dissolution of metals also rose with the increase in the liquid/solid ratio (LAS), however, extractions above 85% can be reached at LAS as lower as 4.5 L/kg, which is favourable for further purification and recovery operations. About 90% of metals extraction can be achieved after only 0.5 h of leaching. Sodium metabisulphite can be an alternative reducer to increase the leaching of Li, Mn, Co, and Ni from spent LIBs. info:eu-repo/semantics/publishedVersion

Materials with a cellular structure are common in nature and an example of natural solid foam is trabecular bone. As for other materials, the microstructural features of cellular solids affect their mechanical response. The aim of this work is to study how the trabecular bone microarchitecture affects the mechanical properties of two types of bone and compare the results with models existing on the literature for solid cellular materials. In spite of several works which make a more medical analysis, this type of materials-science approach is rare. Two types of trabecular bone were studied, namely from male and female patients with osteoporotic (fragility) fractures and patients with coxarthrosis, that were submitted to total hip arthroplasty. Each sample was first analyzed with micro-computed tomography, micro‑CT, for structural assessment. Several parameters used to characterize the three-dimensional structure of trabecular bone were obtained, including the bone volume fraction. Cylinder samples were also tested under uniaxial compression and the Young’s modulus and the ultimate stress were determined. No statistical differences between the two bone groups in respect to the structural and mechanical properties were found. The structural parameters that correlate better with the mechanical properties are different for each bone assembly, being the trabecular separation on the coxarthrosis group and the trabecular number on the osteoporotic group. However, both trabecular separation and trabecular number are strongly correlated with the bone volume fraction, i.e., to the bone relative density. The existing models of Gibson and Ashby were adapted to the relationship between stiffness and strength with the bone volume fraction. In both bone groups, the Young’s modulus is reduced with the decrease of the bone volume fraction following a quadratic law as happens in bending dominated open-cell foams. The ultimate strength is related to the bone volume fraction by a relationship with an exponent between 1 and 2, which indicates that during cell collapse, there is a mixture of two mechanisms: elastic buckling and brittle crushing.

Egg shells, shellfish shells and cuttlefish bones, high calcium content alimentary wastes, were used to prepare CaO sorbents for CO 2 capture. The materials were prepared by a simple procedure including two steps: crushing and calcination at 900 °C. Fine powders displaying chalky-white to pale grey-green shades were obtained depending on the starting material. All the prepared sorbents were microcrystalline limes containing various trace elements. The CO 2 sorption ability of the obtained lime materials was assessed using cycle carbonation/calcination tests by thermogravimetry. The CO 2 sorption profiles showed two regions: an initial region controlled by chemical reaction and a second region with diffusional control. The rate of chemical reaction of carbonation was almost invariant with the nature of the biomaterial used to produces the sorbent. The decarbonation (calcination step) was much faster than the carbonation for all the examined sorbents and also almost invariant with the sample. The diffusion rate depends on the calcite film thickness formed during chemical reaction controlled region. Results showed that alimentary wastes with high calcium content can be used to produces CO 2 sorbents thus contributing to mitigate the anthropogenic carbon and the environment contamination with alimentary wastes.

The aim of this study was to identify three-dimensional microstructural changes of trabecular bone with age and gender, using micro-computed tomography. Human trabecular bone from two disease groups, osteoporosis and osteoarthritis was analyzed. A prior analysis of the effects of some procedure variables on the micro-CT results was performed. Preliminary micro-CT scans were performed with three voxel resolutions and two acquisition conditions. On the reconstruction step, the image segmentation was performed with three different threshold values. Samples were collected from patients, with coxarthrosis (osteoarthritis) or fragility fracture (osteoporosis). The specimens of the coxarthrosis group include twenty females and fifteen males, while the fragility fracture group was composed by twenty three females and seven males. The mean age of the population was 69 ± 11 (females) and 67 ± 10 years (males), in the coxarthrosis group, while in the fragility fracture group was 81 ± 6 (females) and 78 ± 6 (males) years. The 30 μm voxel size provided lower percentage difference for the microarchitecture parameters. Acquisition conditions with 160 μA and 60 kV permit the evaluation of all the volume’s sample, with low average values of the coefficients of variation of the microstructural parameters. No statistically significant differences were found between the two diseases groups, neither between genders. However, with aging, there is a decrease of bone volume fraction, trabecular number and fractal dimension, and an increase of structural model index and trabecular separation, for both disease groups and genders. The parameters bone specific surface, trabecular thickness and degree of anisotropy have different behaviors with age, depending on the type of disease. While in coxarthrosis patients, trabecular thickness increases with age, in the fragility fracture group, there is a decrease of trabecular thickness with increasing age. Our findings indicate that disease, age and gender do not provide significant differences in trabecular microstructure. With aging, some parameters exhibit different trends which are possibly related to different mechanisms for different diseases.

This article presents a detailed study of the microstructure of Iberian expanded clay lightweight aggregates (LWA). Other than more commonly used mercury porosimetry (MP) and water absorption methods, the experimental study involves optical microscopy, scanning electron microscopy (SEM), and microtomography (μ-CT). Pore connectivity and how it is deployed are shown to some degree, and the pore size spectrum is estimated. LWA are in general characterized by a dense outer shell up to 200 μm thick, encasing an inner cellular structure of 10–100 times bigger pore size. Aggregate pore sizes may span from some hundreds of nanometers up to over 1 mm, though the range of 1–25 μm is more typical. A noteworthy fraction of these pores is closed, and they are mainly up to 1 μm. It is also shown that macropore spatial arrangement is affected by the manufacturing process. A step forward is given to understanding how the outer shell and the inner pore network influence the mechanical and physical LWA properties, particularly the density and water absorption. The joint consideration of μ-CT and SEM seems to be the most appropriate methodology to study LWA microstructure. MP analysis is likely to distort LWA pore spectrum assessment.

The wear evolution of railway wheels is a very important issue in railway engineering. In the past, the reprofiling intervals of railway vehicle steel wheels have been scheduled according to designers’ experience. Today, more reliable and accurate tools in predicting wheel wear evolution and wheelset lifetime can be used in order to achieve economical and safety benefits. In this work, a computational tool that is able to predict the evolution of the wheel profiles for a given railway system, as a function of the distance run, is presented. The strategy adopted consists of using a commercial multibody software to study the railway dynamic problem and a purpose-built code for managing its pre- and post-processing data in order to compute the wear. The tool is applied here to realistic operation scenarios in order to assess the effect of some service conditions on the wheel wear progression.

9 páginas.-- 3 figuras.-- 2 tablas.-- 83 referencias.-- Selected paper from the XVI Latin-American Congress on Chromatography (XVICOLACRO) and the 9th National Meeting on Chromatography (9ENC), 5–9 January 2016, Lisbon, Portugal., This study comprises an innovative approach based on the combination of chromatography (analytical pyrolysis and pyrolysis compound-specific isotope analysis (Py-CSIA)), light stable isotopes, microscopy and mineralogy analyses to characterize the internal layering of coralloid speleothems from the Ana Heva lava tube in Easter Island (Chile). This multidisciplinary proxy showed that the speleothems consist of banded siliceous materials of low crystallinity with different mineralogical compositions and a significant contribution of organic carbon. Opal-A constitutes the outermost grey layer of the coralloids, whereas calcite and amorphous Mg hydrate silicate are the major components of the inner whitish and honey-brown layers, respectively. The differences found in the mineralogical, elemental, molecular and isotopic composition of these distinct coloured layers are related to environmental changes during speleothem development. Stable isotopes and analytical pyrolysis suggested alterations in the water regime, pointing to wetter conditions during the formation of the Ca-rich layer and a possible increase in the amount of water dripping into the cave. The trend observed for δN values suggested an increase in the average temperature over time, which is consistent with the so-called climate warming during the Holocene. The pyrolysis compound-specific isotope analysis of each speleothem layer showed a similar trend with the bulk δC values pointing to the appropriateness of direct Py-CSIA in paleoenvironmental studies. The δC values for n-alkanes reinforced the occurrence of a drastic environmental change, indicating that the outermost Opal layer was developed under drier and more arid environmental conditions., A.Z. Miller acknowledges the support from the Marie Curie Intra-European Fellowship of the European Commission’s 7th Framework Programme (PIEF-GA-2012-328689). The Spanish Ministry of Economy and Competitiveness (MINECO, project CGL2013-41674-P) and the FEDER Funds are acknowledged for the financial support. N.T. Jiménez-Morillo thanks the MINECO for funding his pre-doctoral FPI fellowship (BES-2013-062573).

An excavation in a 14th c. church at Torres Novas, named Santa Maria do Castelo, provided some green glazed ceramic sherds, archaeologically dated from 14th c. to the 16th c. The town of Torres Novas is located at the center of Portugal, about 100 km north of Lisbon. The obtained results evidence three types of pastes of the pottery: type 1 with Quartz, Illite, Muscovite and Microcline as the main constituents, type 2 with Quartz, Calcite and Gehlenite; and finally type 3 with Quartz, Calcite and Diopside being the major components. Type 1 pastes are related to clay sources of Pliocene origin, and all this pottery was most probably made in Portuguese kilns. However, types 2 and 3 spectroscopic trends are remarkably different, indicating that those ceramics were produced in Seville. All the studied ceramics are lead glazed, and green glazed. In one of the samples from the Seville kiln, Cerusite was the main pigment used to obtain the greenish colouration. In what regards the origin of all samples produced with Pliocene clays, the 16th c. ones were most likely produced in the Santo Antonio da Charneca or Mata da Machada kilns, both located in the south shore of the Tagus river, region of Lisbon. In what regards the green glazed jug rim (14th c.) and the jug spout (15th c.) they could also have been produced in the two mentioned kilns south of Lisbon city, but another interesting hypothesis - due to richness of the decoration - is the production in Lisbon workshops, with the use of Pliocene clays imported by Lisbon potters, now documented both in Lisbon archaeological findings and also in documental sources.

Different in situ and laboratory tests are commonly used to determine the nature of salts and to improve the comprehension of degradation mechanisms. Although laboratory tests are more accurate, in situ tests yield faster results and require a significantly lower budget. This study aimed at collecting data on nine case studies of buildings (26 sample’s analysis) showing salt induced damage and assessing the potential of diagnosis techniques. Two in situ (test strips and a spectrophotometer-field kit) and three laboratory techniques [X-ray diffraction (XRD), X-ray fluorescence (XRF) and infrared spectroscopy (FTIR)] were carried out. The results showed the importance of collecting samples from different materials and locations. It is concluded that the combination of a thorough description of the areas affected by salt damage, a survey of the building’s history, the consideration of its surrounding environmental conditions, and simple in situ tests is a useful and straightforward diagnostic tool. A...

2 páginas.-- 2 figuras, Coralloid-type speleothems were found in Ana Heva lava tube from Easter Island (Chile). The ceiling of the lava tube presents light to dark brown speleothems with globular coral-like shape. To appraise their internal structure and composition, optical microscopy (OM) of cross-sections, field emission scanning electron microscopy with energy dispersive X-ray spectroscopy (FESEM-EDS) and X-Ray micro-computed tomography ( CT) were performed. The latter is a non-destructive method (NDM), performed to assess physical and compositional heterogeneities of the coralloids. The internal structure of these speleothems comprises a succession of thin layers, ranging from white to brown, with vitreous to resinous luster (Fig. 1A). According to their color and texture, four major layers are easily distinguishable, from the surface to their inner part: a superficial dark brown to black coating, with approximately 0.1 mm thick (L1); a 0.1-1 mm thick semi-transparent grayish layer (L2); a 0.1-1 mm thick white layer (L3), and a heterogeneous honey brown layer, with 1-5 mm thick and shades ranging from yellowish to honey brown (L4). FESEM-EDS microanalyses performed on the internal layers of longitudinally cut coralloid samples (Fig. 1B) showed systematic differences in chemical composition of the different color inner layers. In general, they contain variable proportions of Si, Mg and Ca (Fig. 1C-G). According to a previous study [1], the thin dark brown to black coating of the coralloid surfaces is probably derived from the weathering of the overlying volcanic rock and microbial activity [1]. The semi-transparent grayish layer (L2) is composed of low crystalline silica (opal-A), whereas the whitish layers (L3) are calcium carbonate (calcite). In contrast, the honey-brown layers (L4) present an unusual composition characterized by high levels of Mg, corresponding to an amorphous Mg hydrate silicate. Significant content of organic carbon was also found in these layers [1]. The CT study allowed us to confirm the existence of internal zoning in the studied coralloids (Fig. 2), and between them and the basaltic substrate. The brighter domains in the reconstructed images (Fig. 2D,E) correspond to the vacuolar basaltic. The other opaque domains, comprising thin spheroidal precipitates or dispersed spots within the coralloids (Fig. 2F-I), are calcium rich phases. According to mineralogical data and FESEM-EDS analysis, the inner/older spots correspond to apatite and the outer/more recent spots correspond to calcite. In contrast, the Si, Mg and C enriched domains are more transparent to X-ray radiation, combining at least two main phases (siliceous and magnesium silicate compounds). The proposed methodology was considered adequate for studying coralloid samples, by combining a NDM (μCT) with other microanalytical techniques. Investigations of speleothems using the potentialities of μCT provide general morphological and compositional information, suggesting the best approach for selecting and sectioning the samples. The FESEM-EDS provides characteristic information on the morphological, mineral and chemical composition., The authors acknowledge FCT for PEst-OE/CTE/UI0098/2011, AZM (SFRH/BPD/63836/2009) grant, and Spanish Ministry of Science and Innovation (Project CGL2011-2569) and CSIC 210230E125.

This paper assesses the physical, chemical and mineralogical characteristics of fine recycled aggregates obtained from crushed concrete waste, comparing them with two types of natural fine aggregates from different origins. A commercial concrete was jaw crushed, and the effect of different aperture sizes on the particle size distribution of the resulting aggregates was evaluated. The density and water absorption of the recycled aggregates was determined and a model for predicting water absorption over time is proposed. Both natural and recycled aggregates were characterized regarding bulk density and fines content. Recycled aggregates were additionally characterized by XRD, SEM/EDS and DTA/TG of individual size fractions. The results show that natural and recycled fine aggregates have very different characteristics. This should be considered in potential applications, both in terms of the limits for replacing amounts and of the rules and design criteria of the manufactured products.

Cellulose acetate (CA)–silver (Ag) nanocomposite asymmetric membranes were prepared via the wet-phase inversion method by dispersing polyvinylpirrolydone-protected Ag nanoparticles in the membrane casting solutions of different compositions. Silver nanoparticles were synthesized ex situ and added to the casting solution as a concentrated aqueous colloidal dispersion. The effects of the dispersion addition on the structure and on the selective permeation properties of the membranes were studied by comparing the nanocomposites with the silver-free materials. The casting solution composition played an important role in the adequate dispersion of the silver nanoparticles in the membrane. Incorporation of nanoscale silver and the final silver content resulted in structural changes leading to an increase in the hydraulic permeability and molecular weight cut-off of the nanocomposite membranes. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015, 132, 41796.

11 páginas.-- 8 figuras.-- 1 tabla.-- 33 referencias, Coralloid-type speleothems were recorded on the ceiling of the Ana Heva lava tube in Easter Island (Chile). These speleothems were morphologically, geochemically and mineralogically characterized using a wide variety of microscopy and analytical techniques. They consist dominantly of amorphous Mg silicate and opal-A. Field emission scanning electron microscopy revealed a variety of filamentous and bacillary bacteria on the surface of the Ana Heva coralloid speleothems, including silicified filamentous microorganisms. Among them, intriguing reticulated filaments resemble those filaments documented earlier in limestone caves and lava tubes. The identification of silicified microorganisms on the coralloid speleothems from the Ana Heva lava tube suggests a possible role of these microorganisms in silica deposition. © 2014 Copyright Taylor and Francis Group, LLC., This research was partially financed by Portuguese Funds through FCT- Fundaçao para a Ciencia e a Tecnologia (PEst-OE/CTE/UI0098/2011) and also by the Spanish Ministry of Science and Innovation (Project CGL2011–2569). This work was supported by FCT grant to AZM (SFRH/BPD/63836/2009).