Areas such as Douro Demarcated Region (Portugal), where vineyards are frequently located on steep slopes of narrow valleys, can be particularly sensitive to runoff and erosion processes. These particular conditions are expected to enhance the transport of pollutants, acting as a potential source of contamination to freshwater systems. The intense vine cultivation in this region includes decades of pesticides application, that have resulted in the accumulation of these chemicals and its degradation products in the vineyards soils and sediments. Residues of several pesticides related to agricultural activities were found in soils, with older vineyards showing higher levels of Cu and banned insecticides (such as DDT). The metabolite 4,4-DDE was the compound found at higher levels in soils and in sediments. The relatively high levels in more recent sediments suggest that soils are still a source of contamination. Levels of currently used pesticides were low, which is related with their physicochemical properties, the application period, and climacteric conditions.

This study was directed towards investigating suitable compounds to be used as stable isotope reference materials for gas chromatography combustion isotope ratio mass spectrometry (GC-C-IRMS) calibration. Several compounds were selected from those used in the 'Grob-test' mixture. Oxygen- and nitrogen-containing substances were added to these compounds to allow the mixture to be used as a possible multi-isotopic calibration tool for 2H/1H, 13C/12C, 15N/14N and 18O/16O ratio determinations. In this paper we present the results of delta13C measurements performed by the consortium of the five laboratories taking part in this inter-calibration exercise. All the compounds were individually assessed for homogeneity, short-term stability and long-term stability by means of EA-IRMS, as required by the bureau communitaire de reference (BCR) Guide for Production of Certified Reference Materials. The results were compared then with the GC-C-IRMS measurements using both polar and non-polar columns, and the final mixture of selected compounds underwent a further certification exercise assessing limits of accuracy and reproducibility under specified GC-C-IRMS conditions.

Draining through industrial areas of the Minas Gerais mining state (Brazil), some tributaries of the São Francisco River constitute a potential environmental hazard for this great river and threaten the quality of the regional soils for agriculture and other activities. Extensive geochemistry and mineralogy of sediments, soils and alluvial plains from six selected areas within the Consciência drainage basin close to an important Zn-extraction plant, have been carried out. In this report, detailed mineralogy of those samples and supporting geochemical data are discussed, taking into account their specific climactic and environmental context. Petrographic and electron microprobe characterization of the sand-grained fraction of these materials was complemented by XRD on their finer fraction: the main contaminant minerals are willemite (one of the Zn ores used in the industrial plant) and jarosite, though their contents are quite variable in the studied areas and also with depth; minor amounts of Zn-, Pb-, Cd-, and Mn-bearing mineral phases are also frequent, usually as inclusions in willemite or in polycrystalline clasts, or adsorbed on the finer materials, such as clay minerals and associated Fe-hydroxides. Mineralogical contamination is responsible for high metal contents in the soils and sediments of the areas closer to the plant (e.g. Zn ≫ 2000 mg kg −1 and Cd ≫ 20 mg kg −1 , which are the Intervention Values for Industrial Areas) and the greatest contamination risks are related to the more labile phases that circulate throughout the alluvial plains, the shallow sediments and the stream bed. Monitoring the mineral/chemical contamination and its extent also constitutes a useful basis for future proposals to remediate and recover this industrial area in order to decrease medium-and long-term negative impacts of metal contamination on the local and downstream environments.

This study presents for the first time the diet of a Late Antiquity population in southern Portugal (Civitas of Pax Julia), from the Roman villa of Monte da Cegonha (predominantly 7th century CE). Stable isotope analysis (δ 13 C, δ 15 N, δ 18 O, 87 Sr/ 86 Sr) of human and faunal bone collagen and apatite was conducted in order to understand the influence of Roman subsistence strategies on the way of life of rural inhabitants of the area of Pax Julia and to explore their diet (types of ingested plants, amount of animal resources, terrestrial versus marine resources). X-ray diffraction (XRD) and Fourier transform infra-red spectroscopy (FTIR) analyses were used to determine the degree of bone diagenesis and assess the reliability of the bone stable isotopic composition for palaeodietary reconstruction. Anthropological analysis revealed a cariogenic diet, rich in starchy food and carbohydrates, in at least in two individuals based on the frequency of dental caries. Collagen and apatite carbon isotopic analysis suggested that C 3 plants were the basis of the population's diet, complemented with some terrestrial meat and its byproducts as reflected by the observed bone collagen nitrogen isotopic composition. Moreover, whilst the fairly low apatite-collagen spacing recorded in some skeletons (at around 4‰) may have been due to freshwater organisms intake, the relatively low nitrogen values observed indicate that this consumption did not occur very often, unless in the form of fresh fish of low trophic level or fish sauces. There were no significant differences in isotopic values depending on gender or burial type. Strontium and oxygen isotopic composition of bone apatite revealed a sedentary community, with the exception of a male individual who probably did not spend his childhood in Monte da Cegonha.

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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 > 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.

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