Naturally deformed biotite in contact-metamorphosed slates affected by a shear zone of the Southern Iberian Massif near Jaén (SE Spain) were studied by X-ray diffraction, optical microscopy, scanning electron microscopy, electron probe microanalysis and high-resolution transmission and analytical electron microscopy. Biotite is found in the contact metamorphism aureole produced by the intrusion of a granodioritic stock, but shear strain caused its deformation. The southern part of the shear band is strongly deformed, containing thick clay gouge zones. The northern part is less deformed and develops weaker planar-linear fabrics. X-ray diffraction data reveal the predominance of the 2M1 biotite in the undeformed samples whereas the 1M polytype is predominant in the sheared samples. Chemical data and electron images of the biotite from unsheared slates do not show the presence of intercalated phases. This biotite is almost defect-free and electron diffraction patterns have sharp reflections indicating a two-layer polytype (probably 2M1). Back-scattered electron images from the deformed biotite in the moderate deformation part of the shear zone do not reveal intergrown minerals, but the electron microprobe analyses show some Fe- and Mg-enriched compositions. Transmission electron microscopy indicates that disordered polytype packets are predominant (probably 1Md). Their electron diffraction patterns have diffuse streaking along c*. These packets have high dislocation densities, microcavities with ∼5 Å latticefringe regions (probably brucite-like sheets) and interlayering of chlorite-berthierine. Kaolinized biotite can be observed in the clay gouges from the strongly deformed south part of the shear zone. The degree of streaking, as an indication of the intensity of deformation, revealed that the disordered polytype packets are more deformed than the two-layer polytype packets. The microcavities of the disordered polytype packets could act as potential channels for transport of fluids during the shearing stage and serve as sites for chloritization of biotite, producing chlorite-berthierine domains within biotite. Berthierine is an intermediate metastable phase replaced by chlorite with along-layer transitions.

A geochemical and mineralogical study has allowed us to address the factors controlling distribution pattern, residence and behaviour of rare earth elements (REE) during kaolinization of Variscan granitoids in NW Spain. Mineral composition of the deeply weathered samples is dominated by kaolinite, with minor amounts of quartz, muscovite-illite, alkaline feldspar and traces of resistant minerals (rutile, ilmenite, zircon and monazite). Variable amounts of Si, Na, Ca, K, Rb, Cs, Ba, U and P were lost from the weathering profile, as a result of feldspars, mica and apatite breakdown, whereas Al, Fe, Ti, Zr, Th, Hf and REE were concentrated in the residual kaolin. Chondrite-normalized REE patterns of the kaolins show an overall enrichment of light REE (LaN/SmN = 1.22–2.53), heavy REE depletion (GdN/YbN = 2.42–15.10) and a strong negative Eu anomaly (Eu/Eu* = 0.11–0.25), probably inherited from the parent granite. Nevertheless, the normalization to the parent granite reveals some REE fractionation and increasing positive Eu anomalies with advancing weathering, in response to the breakdown of feldspars. Different grain-size fractions show similar REE distribution patterns, but differ in concentration levels. Although the fine fractions are the most important REE reservoir, there is no positive correlation with clay mineralogy. The correlative behaviour among P2O5, Th and REE in the <2 mm fraction suggests that monazite plays a dominant role controlling the REE budget in the weathering profile.

We have carried out optical microscopy, X-ray diffraction (XRD) and scanning and transmission electron microscopy (SEM and TEM) studies of phyllosilicates from black slates of very low to low-grade metamorphism. Such slates belong to a Middle/Late Devonian basin and an Early Carboniferous basin associated with the Porto–Tomar–Ferreira do Alentejo strike-slip shear zone (Ossa-Morena Zone, Portuguese Iberian Variscan Massif). These black slates are imbricated in an Upper Proterozoic substratum of higher metamorphic grade. Kübler Index values of white micas and mineral assemblages deduced from the XRD, SEM and TEM data (muscovite, chlorite and pyrophyllite) indicate high anchizonal and epizonal metamorphic conditions for slates from these basins. The b parameter and the phengitic contents of mica suggest the occurrence of low pressures (1–2 kbar) related to an extensional geotectonic setting. The dense fracture network shown by SEM images and the high density of crystal defects revealed by the TEM study in the eastern basin, adjacent to faults produced by shearing, suggest that their epizonal phyllosilicates were more affected during deformation than those belonging to the western basin, favouring the development of a retrograde association (siderite, kaolin group minerals and Al-smectite) on the epizonal paragenesis. Microcavities formed along phyllosilicate cleavage acted as channels for fluid transport favouring alteration under low-temperature conditions.

Kaolinite aggregates are the major alteration product in the strongly deformed areas of a shear zone developed in contact-metamorphosed slates from the Southern Iberian Massif near Jaén (SE Spain). Muscovite and Fe-rich chlorite in strain shadows of broken andalusite crystals were observed in slates from less deformed areas. The presence of phyllosilicate packets nearly perpendicular to each other and veinlets parallel to {110} of andalusite reveal the importance of cleavage-controlled fracturing of andalusite to the mineral reactions. The compositional similarity between kaolinite and andalusite suggests a direct transformation of andalusite to kaolinite in the strongly altered area. The absence of clear preferred orientation of phyllosilicates relative to andalusite, and the compositional differences of andalusite with muscovite and chlorite from the less altered samples, indicate andalusite dissolution and chlorite-muscovite precipitation during a first mineral-growth stage. Muscovite-kaolinite and chlorite-kaolinite intergrowths indicate a later retrograde replacement stage.

Flysch-type, syn-orogenic deposits of Carboniferous age occur in relation to the emplacement of a large allochthonous nappe stack in the Variscan belt of NW Iberia. New U–Pb age populations of detrital zircons obtained using laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) are considered together with others from previously dated samples to establish the relationships between sedimentation and thrusting. The age populations of four syn-orogenic formations are compared with those of the pre-orogenic sequence in the Autochthon and Parautochthon, representing the Gondwanan passive margin, and in the Allochthon, formed by peri-Gondwanan and oceanic terranes. In addition, a new structural study has been carried out to understand the relationships between the syn-orogenic deposits and the development of Variscan structures. The aims are to identify the sources of sediments and to establish the relationship between Variscan structural evolution and syn-orogenic sedimentation. Development of a forebulge outwards from the allochthonous front, deduced from the structural study, suggests the existence of depocentres that hosted the syn-orogenic sediments. Together with the trend shown by the more recent zircons in each formation, that are younger towards the external zones, the data suggest that sedimentation occurred in progressively migrating depocentres formed in front of the allochthonous wedge during its emplacement. The zircon age populations point to the Allochthon as the main source of detritus for the syn-orogenic basins, with perhaps a limited participation of the Parautochthon and Autochthon in the younger formations.

The type material of Agraulos antiquus Sdzuy, 1961 from the La Herrería Formation, northern Spain, is revised together with additional material and included in the new genus Lunagraulos. The stratigraphical range of Lunagraulos antiquus (Sdzuy, 1961) – occurring below that of the trilobite species of the genera Lunolenus, Metadoxides and Dolerolenus in the type locality of Los Barrios de Luna in the province of León, northern Spain – and the accompanying ichnofossil assemblage demonstrate an Ovetian age (lower part of Cambrian Stage 3, currently being discussed by the International Subcommission on Cambrian Stratigraphy) for this species. Moreover, the trilobite Lunagraulos tamamensis n. gen. n. sp. is found in the Tamames Sandstone near the village of La Rinconada in the province of Salamanca, central Spain. The biostratigraphical position of this new taxon and its accompanying ichnoassemblage is also analysed and assigned to the lowermost Ovetian Stage. The genus Lunagraulos is therefore the oldest agraulid found in the fossil record. The exceptional presence of Lunagraulos in a marine coarse siliciclastic succession – a facies rather typical for the ichnofossils Cruziana and Rusophycus, some of the oldest signs of trilobite activity – suggests that first trilobite representatives may have inhabited high- to middle-energy, marine environments. This hypothesis may also explain both the taxonomic and biostratigraphic heterogeneity of the first trilobite genera appearing across the world, due to preservation problems in this type of facies. Comparison of the Lunagraulos biostratigraphy with other coeval Spanish fossil assemblages allows us to propose its intercontinental correlation with the oldest records of currently known trilobites.

The uppermost metavolcanic layer of the Cambro-Ordovician Ollo de Sapo Formation, the largest accumulation of pre-Variscan igneous rocks in the Iberian Peninsula, have been dated in its northernmost part using U–Pb SHRIMP-RG zircon age techniques at 479.0 ± 4.7 Ma. The age obtained is the youngest age found so far in the metavolcanic facies of Ollo de Sapo Formation and represents the cessation of the rifting-related Cambro-Ordovician Ollo de Sapo volcanism at the northernmost tip of the Iberian Peninsula. Our results show that the Cambro-Ordovician volcanism in the NW of the Iberian Peninsula is not as short-lived as previously thought and confirm the correlation between the Cambro-Ordovician volcanic sequences that crop out in the Central Iberian Zone and the French Southern Armorican Massif. Finally, our study suggests that the cessation of the Cambro-Ordovician volcanism along the Ibero-Armorican Arc was synchronic or, less probably, slightly diachronic with younger ages towards the north (in present-day geographical coordinates).

The Zarza la Mayor and Zarza de Montánchez tonalites and Arroyo de la Luz granodiorite are part of a tonalitic–granodioritic belt located along the Schistose-Greywacke Domain of the Central Iberian Zone. These intrusions are also part of the Central Extremadura Batholith, a set of plutons ranging from tonalite to leucogranite that have been considered a prime example of Variscan syn-kinematic plutonism. New LA-ICP-MS and CA-ID-TIMS U–Pb dating reveals that the Zarza la Mayor tonalite–granodiorite is an Early Ordovician intrusion. The LA-ICP-MS data show that there is an absence of inherited cores, despite some complex internal zoning with obvious resorption features in some of the zircon crystals. Dating of monazite and zircon by CA-ID-TIMS provides a concordant age of 478.1 ± 0.8 Ma. This age coincides with electron microprobe analysis (EMPA) monazite chemical ages for the Zarza de Montánchez (482 ± 10 Ma) and Arroyo de la Luz (470 ± 15 Ma) intrusions. These new data indicate the presence of an Early Ordovician belt of calc-alkaline tonalite–granodiorite in the Schistose-Greywacke Domain – the Beira Baixa–Central Extremadura tonalite–granodiorite belt – which resembles a continental magmatic arc. This belt is contemporaneous with the Ollo de Sapo magmatic event further north in the Central Iberian Zone.