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Stratigraphic and sedimentological study of distal alluvial and lacustrine deposits in the Plana de la Negra-Sancho Abarca area (western-central Ebro Basin, NE Iberia) within the early and middle Miocene allows five main lithofacies to be characterized and mapped within two tectosedimentary units, construction of a sedimentary facies model and discussion on allogenic controls on sedimentation. In this area, the boundary between tectosedimentary units T5 and T6 appears to be conformable and is marked by the change from dominant clastics to carbonates. Correlation of the studied outcrops with nearby sections that already had magnetostratigraphic and biostratigraphic data allows the studied succession to be dated from C5Dr to C5Cn (Burdigalian-Langhian), placing the boundary T5/T6 at ca. 16.1-16.05Ma. Seven vertical facies sequences document deposition of distal alluvial clastics and palustrine and lacustrine carbonates. Sandstones and mudstones represent low-sinuosity channels and lateral and terminal splays by unconfined flows runnig across the alluvial plain, associated to the Pyrenean-derived Luna fluvial system. The carbonates contain charophytes, ostracods, bivalves and gastropods, indicating deposition in 2-4m deep lakes. Laminated carbonate facies record reworking of shore carbonates and the influx fine-siliciclastic sediment offshore. Abundant bioturbation and desiccation features indicate episodic submergence and subaerial exposure. Four main episodes of alluvial and associated palustrine/lacustrine facies belt shifts are identified. Alluvial deposition in the studied T5 unit is related to low lake level conditions, rather than to a Pyrenean uplift. The maximum extent of the freshwater carbonates occur at the base of unit T6. This is consistent with conditions of increasing humidity of the Middle Miocene Climatic Optimum.

Eochelone voltregana n. sp. is a new marine cryptodiran cheloniid found at the Priabonian levels (latest Eocene) of the Vespella marls member of the Vic–Manlleu marls formation. It is the second cheloniid from Santa Cecília de Voltregà (Osona County, Spain), the first one being Osonachelus decorata from the same formation. Shell parameters indicate that the new species belongs to a branch of sea turtles including the Eocene Anglo–Franco–Belgian forms Argillochelys, Puppigerus and Eochelone (the shell of the latter was studied here for the first time) as well as Glarichelys from the Oligocene of Switzerland, all of them predating the worldwide living Miocene genera. The description of two other more littoral–continental Eocene species is given: Trionyx sp., from an older layer of the same formation; and the podocnemidid erymnochelyine, Cordichelys from a more basal layer of a middle Eocene (Lutetian) formation. The last one is identified as the only evidence of the Shweboemys subgroup in the European record, being distinct from the other known Osona County pleurodire Eocenochelus farresi, which is a member of the Erymnochelys group (same subfamily), from the younger Priabonian Sant Martí Xic layer. Thus, an update on the marine turtle fauna of the eastern Ebro Basin that variably opened in the east during Eocene times is provided. The turtles of Osona County belong to two suborders and five genera with three new species and extend the known distribution of their families (LSID urn:lsid:zoobank.org:act:48CE8676-7B82-4EF2-8165-27BEE90129F2).

En este trabajo se describen los nuevos hallazgos de rumiantes fósiles del Mioceno inferior (Rambliense, MN3) de las Bardenas Reales (Navarra). Este material está compuesto por dentición y ha sido clasificado como Andegameryx aff. andegaviensis Ginsburg, 1971. El estudio morfológico y métrico muestra que los restos de las Bardenas son muy semejantes a los de la población española de Andegameryx andegaviensis de Cetina de Aragón (Zaragoza), de talla algo mayor que las poblaciones francesas de esta especie. Sin embargo, también tiene afinidades con material de Andegameryx procedente de otras localidades españolas como Loranca del Campo (Cuenca). Los nuevos hallazgos permiten confirmar sin dudas la presencia de Andegameryx en las Bardenas Reales (Cuenca del Ebro), poniendo de manifiesto que este género de rumiante estuvo ampliamente extendido en las cuencas interiores de España durante el Mioceno inferior.

En este trabajo se estudian las asociaciones de ostrácodos identificadas en tres unidades aluviales preservadas en Bardenas Reales de Navarra (Cuenca del Ebro, NE Península Ibérica), para reconstruir la evolución paleoambiental de esta área durante el Holoceno final. Las especies de ostrácodos más comunes en las muestras estudiadas son Ilyocypris bradyi Sars y Paralimnocythere aff. psammophila (Flössner), acompañadas por Pseudocandona albicans (Brady). Las variaciones en su abundancia relativa a lo largo de dichas unidades aluviales permiten caracterizar cambios internos en el ambiente de depósito. Así, la unidad depositada entre 4763±87 y 2848±55 años cal. BP presenta como especie más abundante a I. bradyi, lo que indica la existencia de pequeños arroyos o riachuelos con agua corriente que se desarrollaron probablemente en llanuras de inundación fluviales. Sin embargo, de 2848±55 a 836±65 años cal. BP Paralimnocythere aff. psammophila es la especie dominante, representando el establecimiento de un medio acuático efímero y de aguas estancadas, posiblemente relacionado con condiciones climáticas más áridas (Anomalía Climática Medieval). Finalmente, la asociación de ostrácodos identificada en el Reciente (191±97 a 127±82 años cal. BP) está constituida principalmente por I. bradyi, que indicaría la presencia de nuevo de aguas corrientes. Esta última asociación parece estar vinculada a la influencia de condiciones climáticas húmedas y frías (Pequeña Edad del Hielo) durante el Reciente en esta área. Por lo tanto, la evolución paleoambiental para el Holoceno final de Bardenas Reales de Navarra, identificada a partir de las asociaciones de ostrácodos, muestra una buena correlación con los cambios climáticos rápidos holocenos deducidos en otros registros continentales del NE de la Península Ibérica.

En este trabajo se realiza, por vez primera, un análisis paleoambiental y bioestratigráfico de los depósitos aluviales del Mioceno inferior de la sección de Cenicero (sector NO de la Cuenca del Ebro; N de la Península Ibérica), a partir de las asociaciones de ostrácodos y micromamíferos preservadas en estos materiales. Una de las principales características de esta sección es la inusual abundancia de ejemplares de ostrácodos no transportados, en comparación con otras secciones europeas de edad y ambiente sedimentario similares, lo que permite hacer inferencias paleoambientales precisas. La variación en las asociaciones de ostrácodos identificadas, defini-das por especies como Cyclocypris laevis, Ilyocypris bradyi, Ilyocypris gibba, Limnocythere sp. o Pseudocandona parallela, parece sugerir el desarrollo de pequeños cuerpos de agua dulce, someros y efímeros, enmarcados en un ambiente general aluvial distal y/o de llanura de inundación. Hacia techo de la sección, se registra una mayor permanencia temporal de estas acumulaciones y condiciones más estables y favorables del medio para el desarrollo de los ostrácodos. Así mismo, se observan variaciones en la temperatura y salinidad del agua a lo largo de la sección, que podrían estar relacionadas con cambios en el régimen pluviométrico local. La presencia de micromamíferos en uno de los niveles estudiados ha permitido obtener una datación precisa de la sección. Así, la aparición de Armantomys daamsi sitúa la sección de Cenicero dentro de la zona local Y2 (MN2) de edad Ageniense (Mioceno inferior).

En este trabajo se realiza la descripción de los fósiles de tortuga encontrados en los yacimientos del Aragoniense medio-superior de Monteagudo, Tarazona de Aragón, El Buste y La Ciesma. Además, se ha comparado la asociación paleoquelionológica descrita en estas localidades con la descrita en localidades más antiguas del mismo sector de la Cuenca del Ebro. La diferencia entre la asociación de la Biozona Z-A de las Bardenas Reales de Navarra y la descrita en el resto de las localidades puede deberse al medio sedimentario y/o a los cambios de humedad y temperatura relativas acaecidos a lo largo del Mioceno inferior-medio.

Las Bardenas Reales de Navarra se encuentran en el borde NW de la cuenca terciaria del Ebro. Los sedimentos que podemos encontrar en la mayor parte del área de estudio pertenecen a facies fluvio-palustres de la Formación Tudela. Las localidades fosilíferas estarían incluidas dentro de la Biozona MN2b-MN· (Biozonas Z-A del Rambliense o Aquitaniense superior-Burdigaliense inforior). En esta área se han encontrado restos fósiles de peces, anfibios, lagartos, anfisbénidos, serpientes, tortugas, cocodrilos, flamencos y los mamíferos que se describen en este trabajo como insectívoros, quirópteros, eomídos, gliridos, esciúridos, cricétidos, lagomorfos, perisodáctilos y artiodáctilos.

Se describen restos fósiles dentarios, craneales y postcraneales pertenecientes a la familia Bovidae del yacimiento de Tarazona de Aragón. Según las características morfológicas y métricas de la dentición y los núcleos óseos, existen dos formas en este yacimiento del Mioceno medio de la Cuenca del Ebro. Una ha sido atribuida al género Eotragus y clasificada como E. aff. sansaniensis, mostrando características más derivadas que el resto de las formas ibéricas del mismo género. La otra se clasifica, provisionalmente, como aff. Tethytragus, ya que guarda similitudes con la especie ibérica Tethytragus langai y diferencias evidentes con respecto a Eotragus. Los dos taxones se diferencian netamente respecto a la talla, hipsodoncia y morfología de la dentición; sobre todo, las diferencias de desarrollo y prominencia de los estilos/estílidos y costillas mismos son evidentes.

El yacimiento kárstico cuaternario de la Sierra de Quibas (Abanilla, Murcia) ha proporcionado una amplia lista faunística constituida por 53 especies repartidas entre gasterópodos, miriápodos, anfibios, reptiles, aves y mamíferos. En el conjunto de los gasterópodos destaca Palaeoglandina, un género que se extingue en el resto de Europa durante el Plioceno y que se mantiene como relicto en el Pleistoceno de la Península Ibérica. Dos de las especies de aves determinadas, Gypaetus barbatus y Gerontieus eremita, y una de las serpientes, Elaphe cf. E. sealaris, apenas se hallan representadas en el registro fósil. Hay además varias especies de aves cuya aparición en Quibas supone la primera cita en el Pleistoceno inferior de la Península Ibérica. Entre los mamíferos posee una especial relevancia la presencia del cercopitécido Macaca sylvanus. La asociación de los taxones Arvieola deuealion, Castillomys rivas rivas, Eliomys intermedius, Equus altidens y Capra sp. aff. C. alba permite la correlación con Plines 1, Orce 3 y Venta Micena, entre otros. El yacimiento de Quibas puede situarse, por tanto, antes del final del Pleistoceno inferior, con una antigüedad entre 1.3 y 1 Ma. Por lo que se refiere a las condiciones paleoclimáticas, podemos inferir a partir de la asociación faunística un régimen xerófilo, muy semejante al actual en el área geográfica, aunque quizás con valores de humedad y temperatura algo superiores. El entorno de la cavidad kárstica estaba formado por roquedo calcáreo con áreas abiertas de matorral, pero en las proximidades se desarrollaron humedales y zonas arboladas, como así lo atestigua la presencia de aves y micromamíferos típicos de estos hábitats.

Se describe un conjunto de icnitas fósiles de mamíferos ubicado en los alrededores de la localidad navarra de Olcoz (Depresión del Ebro). Las huellas se localizan en niveles areniscosos de la «Formación de Mués», de posible edad Sueviense (Oligoceno inferior). Por su morfología pueden asignarse a mamíferos artiodáctilos y resultan comparables a Entelodontipus, constituyendo este hallazgo una segunda cita para dicho icnogénero. En este yacimiento se constata una notable variabilidad morfológica de las huellas, resultado de la distinta penetración y desplazamiento de los autópodos en el sustrato. La presencia en Olcoz de numerosas icnitas formando rastros subparalelos permite inferir el comportamiento gregario de sus productores.

The Mediterranean coast of Spain is marked by several clusters of Palaeolithic sites: to the south of the Pyrenees, in the area around the Ebro River, in the central part, and on the south coast, one of the southernmost regions in Europe. The number of sites is small compared with northern Iberia, but like that region, the Palaeolithic occupations are accompanied by several rock art ensembles. The archaeological material (both biotic and abiotic resources) and radiocarbon dates presented here were obtained during archaeological fieldwork of professor J. Fortea in the Late Pleistocene deposits in Cueva Victoria, located near the modern coastline and about 150 km north of the Strait of Gibraltar. In the three occupation phases, marine resources were acquired by shell-fishing (focusing almost exclusively on the clam Ruditapes decussatus ), fishing, and the use of beached marine mammals. This contrasts with the limited data about the exploitation of terrestrial resources by hunting and gathering animals and plants. The study is completed by the study of artefacts (lithic and bone industry and objects of adornment) that help to understand the subsistence strategies of the cave occupants and enable a comparison with other groups inhabiting the Mediterranean coasts of the Iberian Peninsula during Greenland Interstadial 1, between ca . 15.1 and 13.6 cal BP., Competing Interests: The authors declare no conflict of interest., (© 2022 The Author(s).)

We present a new locality with at least 880 vertebrate tracks found at the top of a limestone bed from the lower Miocene Tudela Formation (Spain). The trampled surface was formed by artiodactyls that crossed a muddy carbonate accumulated under the influence of water level variations in a palustrine environment. The tracks reflect different types of morphological preservation. The well-preserved tracks have tetradactyl digit impressions caused by both manus and pes, and are the type series of a new artiodactyl ichnotaxon, Fustinianapodus arriazui ichnogen. nov. and ichnosp. nov. The rest of the tracks, which are not as well preserved, are didactyl and were classified as undetermined artiodactyl tracks. According to their preservation, morphology, size, arrangement and orientation, we propose that this tracksite is the product of a social behaviour, particularly gregariousness, of a multi-age group of artiodactyls ~19 Ma ago. The morphologic and palaeoecologic data presented here suggest that the trackmakers were a group of anthracotheres with a livelihood similar to current hippos. They crossed, periodically, a fresh water palustrine area along some preferential pathways (trails).

The Islamic necropolis discovered in Tauste (Zaragoza, Spain) is the only evidence that a large Muslim community lived in the area between the 8th and 10th centuries. A multi-isotope approach has been used to investigate the mobility and diet of this medieval Muslim population living in a shifting frontier region. Thirty-one individuals were analyzed to determine δ15N, δ13C, δ18O and 87Sr/86Sr composition. A combination of strontium and oxygen isotope analysis indicated that most individuals were of local origin although three females and two males were non-local. The non-local males would be from a warmer zone whereas two of the females would be from a more mountainous geographical region and the third from a geologically-different area. The extremely high δ15N baseline at Tauste was due to bedrock composition (gypsum and salt). High individual δ15N values were related to the manuring effect and consumption of fish. Adult males were the most privileged members of society in the medieval Muslim world and, as isotope data reflected, consumed more animal proteins than females and young males.

Libyan desert glass (LDG) is a melt product whose origin is still a matter of controversy. With the purpose of adding new information about this enigma, the present paper analyzes the inner part of LDG specimens and compares them with the results of LDG surfaces. An integrated analytical methodology was used combining different techniques such as Raman spectroscopy, in point-by-point and imaging modes, scanning electron microscopy with X-ray microanalysis (SEM-EDS), energy-dispersive micro X-ray fluorescence spectrometry (μ-EDXRF), electron probe micro analyzer (EPMA), and optical cathodoluminescence (Optical-CL). According to our results, flow structures of the melt and the amorphous nature of the matrix could be discerned. Moreover, the observed displacement of Raman bands, such as in the cases of quartz and zircon, and the identification of certain compounds such as coesite (the most clarifying phase of high pressures), α-cristobalite, gypsum, anhydrite, corundum, rutile, amorphous calcite, aragonite, and calcite allowed us to know that LDGs could be subjected to shock pressures between 6 and more than 30 GPa, and temperatures between 300 and 1470 °C. The differences of temperature and pressure would be provoked by different cooling processes during the impact. Besides, in most cases the minerals corresponding to high pressure and temperatures were located in the inner part of the LDGs, with some exceptions that could be explained because they were trapped subsequently to the impact; there was more than one impact or heterogeneous cooling.Furthermore, nitrogen and oxygen gases were identified inside bubbles, which could have been introduced from the terrestrial atmosphere during the meteorite impact.These data helped us to clarify some clues about the origin of these enigmatic samples.

This work outlines a temperate latitude beachrock occurrence, which represents the legacy of heavy anthropogenic environmental disturbance. The units contain high amounts of slag and iron-rich wastes derived from metallurgical activities that attest the impact of the past industrial development on such coastal systems. The exposition of the anthropogenic wastes to weathering processes, such as the influence of marine aerosols and the chemical attack of acid gases like the SOx coming from the nearby urban-industrial atmosphere, gave rise to the formation of early diagenetic ferruginous cements. A new analytical methodology based on the combination of micro-Raman spectroscopy (MRS), Raman chemical imaging, SEM-EDS and the Structural and Chemical Analyzer (SCA, an emerging system that hyphenates micro-Raman and SEM-EDS), was applied for the first time to characterize the ferruginous cements. The MRS analyses revealed Fe 2+ /Fe 3+ oxides and oxyhydroxides, CaCO 3 polymorphs and less frequently silicates. The Fe mineral species detected were hydrated goethite, hematite, magnetite, magnesioferrite, lepidocrocite and goethite. Complementary Raman imaging, SEM-EDS and SCA analyses unraveled the preferential distribution of hydrated goethite. The identified iron mineral phases are weathering sub-products of hematite commonly derived from atmospheric/aqueous leaching processes triggered by the chemical attack of the acid gases. EDS showed the existence of other elements such as Si, Mg, Cl, Na, Al, K and sporadically S that indicated the importance of permeability, atmospheric deposition and the acid attack. Additionally, calcite and gypsum minerals also evidenced the action of meteoric waters, dry deposition processes or the attack of SOx acid gases. The presence of such compounds is modifying the cement stratigraphy and suggests that the dissolution of carbonates is currently taking place. Those facts influence the erosive susceptibility and the release of the anthropogenic materials trapped originally in the beachrocks, which could act as potential secondary sources of contaminants to the coastal environment., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Three very different records are combined here to reconstruct the evolution of environments in the Cantabrian Region during the Upper Pleistocene, covering ~35.000 years. Two of these records come from Antoliñako Koba (Bizkaia, Spain), an exceptional prehistoric deposit comprising 9 chrono-cultural units (Aurignacian to Epipaleolithic). The palaeoecological signal of small-vertebrate communities and red deer stable-isotope data (δ(13)C and δ(15)N) from this mainland site are contrasted to marine microfaunal evidence (planktonic and benthic foraminifers, ostracods and δ(18)O data) gathered at the southern Bay of Biscay. Many radiocarbon dates for the Antoliña's sequence, made it possible to compare the different proxies among them and with other well-known North-Atlantic records. Cooling and warming events regionally recorded, mostly coincide with the climatic evolution of the Upper Pleistocene in the north hemisphere.

The extent of vertical contamination is intimately related to the soil solution and surface chemistry of the soil matrix with reference to the metal and waste matrix in question. The present research demonstrated the impact that the dissolved CO2 of the meteoric waters, which acidify the environment with pH values below 4, has in the increase of the metal mobility. Although under the given conditions the Zn remains mainly dissolved, the initial PbS and ZnS have evolved into newly formed secondary carbonates and sulphates (i.e., hydrozincite, gunningite, hydrocerussite) that can be found in the efflorescences. The chemical simulation done on the weathering of the original sulphide ores for the formation of these secondary minerals has proved the transient storage mainly of Pb. Nonetheless, many of the minerals formed inside the galleries will be easily dissolved in the next rains and release in an ionic form to the groundwater. The analytical procedure exposed has been proved to be useful not only for the characterization of AMD but also for the prediction of the mobility of metals., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

The determination of crystal size of chert samples can provide suitable information about the raw material used for the manufacture of archeological items. X-ray diffraction (XRD) has been widely used for this purpose in several scientific areas. However, the historical value of archeological pieces makes this procedure sometimes unfeasible and thus, non-invasive new analytical approaches are required. In this sense, a new method was developed relating the crystal size obtained by means of XRD and infrared spectroscopy (IR) using partial least squares regression. The IR spectra collected from a large amount of different geological chert samples of archeological use were pre-processed following different treatments (i.e., derivatization or sample-wise normalization) to obtain the best regression model. The full cross-validation was satisfactorily validated using real samples and the experimental root mean standard error of precision value was 165 Å whereas the average precision of the estimated size value was 3%. The features of infrared bands were also evaluated in order to know the background of the prediction ability. In the studied case, the variance in the model was associated to the differences in the characteristic stretching and bending infrared bands of SiO(2). Based on this fact, it would be feasible to estimate the crystal size if it is built beforehand a chemometric model relating the size measured by standard methods and the IR spectra., (Copyright © 2012 Elsevier B.V. All rights reserved.)

Background: We describe the first occurrence in the fossil record of an aquatic avian twig-nest with five eggs in situ (Early Miocene Tudela Formation, Ebro Basin, Spain). Extensive outcrops of this formation reveal autochthonous avian osteological and oological fossils that represent a single taxon identified as a basal phoenicopterid. Although the eggshell structure is definitively phoenicopterid, the characteristics of both the nest and the eggs are similar to those of modern grebes. These observations allow us to address the origin of the disparities between the sister taxa Podicipedidae and Phoenicopteridae crown clades, and traces the evolution of the nesting and reproductive environments for phoenicopteriforms., Methodology/principal Findings: Multi-disciplinary analyses performed on fossilized vegetation and eggshells from the eggs in the nest and its embedding sediments indicate that this new phoenicopterid thrived under a semi-arid climate in an oligohaline (seasonally mesohaline) shallow endorheic lacustine environment. High-end microcharacterizations including SEM, TEM, and EBSD techniques were pivotal to identifying these phoenicopterid eggshells. Anatomical comparisons of the fossil bones with those of Phoenicopteriformes and Podicipediformes crown clades and extinct palaelodids confirm that this avian fossil assemblage belongs to a new and basal phoenicopterid., Conclusions/significance: Although the Podicipediformes-Phoenicopteriformes sister group relationship is now well supported, flamingos and grebes exhibit feeding, reproductive, and nesting strategies that diverge significantly. Our multi-disciplinary study is the first to reveal that the phoenicopteriform reproductive behaviour, nesting ecology and nest characteristics derived from grebe-like type strategies to reach the extremely specialized conditions observed in modern flamingo crown groups. Furthermore, our study enables us to map ecological and reproductive characters on the Phoenicopteriformes evolutionary lineage. Our results demonstrate that the nesting paleoenvironments of flamingos were closely linked to the unique ecology of this locality, which is a direct result of special climatic (high evaporitic regime) and geological (fault system) conditions.

Beachrocks are coastal sedimentary formations resulting from a relative rapid cementation of beach sediments by the precipitation of carbonate cements. These lithified structures are not usually observed at temperate settings. The present work is focused on the occurrence of a significant intertidal cementation in sand-gravel beaches formed among 43°N latitude coastline, close to the Nerbioi-Ibaizabal estuary (Bilbao, Bay of Biscay, North of Spain). Raman micro-spectroscopy combined with SEM-EDX analyses and petrographic descriptions have been applied for the determination of the cement generations and the cemented materials compositions of the beachrock outcrops. In general terms, the cements described were: Cement Generation 1 (CG 1, aragonite, high-magnesium calcite and silicate mixtures), Cement Generation 2 (CG 2, aragonite) and Cement Generation 3 (CG 3, mixtures of CaCO(3) polymorphs and iron oxides). The rest of the interstitial porosity of the rocks appeared either empty or filled with heterogeneous cemented mixtures of previously reworked compounds. The mineralogy, the regular distribution and the isopachous character of the carbonate cements together with the accurate cementation at advanced seaward bands propose a possible marine-phreatic context for the beachrock formation. However, the impure cements and the materials covering the interstitial porosity seem to be the result of both, the weathering actions consequences and the surface alterations of specific grains. Moreover, the presence of modern cemented materials (e.g. slag, bricks and pebbles) suggest a recent formation of the phenomenon., (Copyright © 2011 Elsevier B.V. All rights reserved.)

The analysis of organic biomarkers in chert samples offers key information about the environmental conditions in which these samples were formed, and this information can be used to track the lithic materials of many archaeological artifacts. Since the content of the organic fraction is very low and the complexity of the organic extracts is quite high, we have optimized the GC×GC separation of these mixtures. Making use of mixture of C(16)H(34)-C(44)H(90)n-alkane standards, a central composite design was carried out taking into account the carrier flow in the first and second columns, the modulation period and the discharge time. Regarding the measured responses, though the initially considered one was the peak volume, we have also evaluated the effects on the number of modulated peaks per analyte, the symmetry of the modulated peaks and the number of detected compounds. The final optimum conditions were defined as follows: a hydrogen flow of 1.2 mL/min in the first column and 18 mL/min in the second one, a modulation period of 1.4 s and a discharge time of 0.1 s and under these conditions all the response variables showed optimum values. Based on this optimized method several chert samples obtained from different stratigraphic levels in an ancient quarry were studied and we were able to distinguish them on the basis of the different constituents of organic biomarkers, such as mono-methylated alkanes, cyclic n-alkanes, branched alkanes, steranes and hopanes., (Copyright © 2010 Elsevier B.V. All rights reserved.)

The analysis of hydrocarbons in chert rocks provides a worthwhile source of information regarding the geochemical features of a depositional setting. Since the typical analytical procedure requires long Soxhlet extractions and the use of large quantities of sample (30-50 g), in this work we have optimised the focused ultrasound extraction (FUSE) and the microwave-assisted extraction (MAE) to make available a less severe procedure. In both cases a full experimental design including solvent mixture composition (Dichloromethane/Hexane/Acetone) and process variables (sonication time and cycles, and extraction temperature and time) by means of D-optimal designs. In the extracted fractions hydrocarbons (C(16)-C(40)) were analysed by gas-chromatography-mass spectrometry. In the case of FUSE the process variables were the most sensitive variables and the optimum conditions were defined at 60:40 DCM/Hex mixture and a sonication time of 30 min and 9 cycles. In the case of MAE all the variables shown a significant effect on the extraction yield and the most adequate conditions (60:30:10 DCM/Hex/Ace mixture and an irradiation time of 15 min at 110 °C) were established from the analysis of the response surface. Both methods were systematically applied with different chert samples collected in Cucho (Trebiño County, Burgos, Spain) and we were able to assure quantitative extractions (>85%) in the first extraction. Additionally, from the distribution patterns of n-alkanes obtained in the different chert samples (nodular chert, laminar chert and massive-brechoid chert) collected in Cucho, we were able to distinguish different origins and diagenetic history., (Copyright © 2010 Elsevier B.V. All rights reserved.)

The study of lithic raw materials recovered from archaeological sites offers relevant data on source catchment areas. Additionally, it can provide first hand information on artefact displacement, interchange networks and it can reflect the way in which the artefacts were employed. In order to characterize geological and archaeological chert samples and with the aim of finding an analytical fingerprint infrared and Raman spectroscopies were used for molecular analysis and X-ray Fluorescence spectrometry for elemental analysis. In this work, different chert samples coming from several localities with geological and archaeological importance from the Basque Country have been collected and analysed. As a consequence, Raman spectroscopy allowed to distinguish between alpha-quartz and moganite in chert samples without organic matter and it is suggested that the ratio of those two components is related to the source of the chert. In addition, the impurities that appear in the samples (CaCO(3), iron oxides and organic matter) can open new features to distinguish the samples and in this way, it would be possible to discuss the use and transport of the lithic artifacts from the sources to the final settlements.