The Nasrid emirate of southern Iberia emanated power through architecture; this project aims to better understand how this was made possible, via an interdisciplinary exploration of the Alhambra monument and other Al-Andalus constructions. Initial results of archaeological campaigns, structure chronologies and communication plans undertaken in 2021 and 2022 are presented.

Muscovite-kaolinite intergrowths found in Albian sandstones of the Basque Cantabrian basin (northern Spain) were studied by optical, scanning and electron microscopy and electron microprobe analysis. Kaolinitization begins at grain edges, forming the characteristic fanned-out textures, and propagates toward the interior along the cleavages of muscovite. Kaolinite and muscovite occur as thick packets, being free of interlayering. Phase boundaries between both minerals show bidimensional crystallographic continuity, and no intermediate phases have been identified. The data obtained suggest that muscovite only supplied a template suitable for the epitactic crystallization of kaolinite, while Al was available in sufficient amounts due to the dissolution of detrital K-feldspar. Very small packets of magnetite or maghemite showing a coherent orientation with the kaolinite crystals have been recognized, and could be responsible for the small Fe contents usually detected in electron microprobe analyses of kaolinite.

Textural relationships between authigenic kaolinite and deformation microstructures in the intergrowths, combined with previous information about burial conditions, show that alteration proceeded during a late stage of the diagenetic history, related to the uplift of the studied materials as a result of the Alpine orogeny.

In spite of decades of research on the subject, the crystal structure of illite is still poorly understood. The purpose of this study was to address this problem by investigating the nature of the interlayer content in illite IMt-2 from Silver Hill, Montana, using analytical transmission electron microscopy (ATEM), thermogravimetry (TG), and X-ray powder diffraction (XRPD) analyses. The ATEM data, together with literature and TG results, yielded the formula K0.70a0.01(H2O)0.42 (Al1.53Fe2+0.06Fe3+0.19Mg0.28)Σ−2.06(Si3.44Al0.56)O10(OH)2 or, assuming the presence of H3O+, K0.69Na0.01(H3O)+0.28(Al1.47Fe2+0.06Fe3+0.19Mg0.28)Σ−1.99(Si3.40Al0.60)O10(OH)2. The first formula indicates surplus interlayer and octahedral species, whereas the second shows no excess. The XRPD data were refined by Rietveld techniques, down to an Rp factor of 10.48–13.8%. The mineral composition consists largely of illite-2M1, illite-1M, and minor quartz. Although the refinement accuracy is limited by the intrinsic poor quality diffraction of the illites, the partially refined model is consistent with the chemical composition; in particular, attempts to introduce octahedral cations in excess of 2 were fruitless. All the results support the simple structural model, by which the illite structure strictly corresponds to a dioctahedral mica with H3O+ replacing K. As a consequence, the crystalchemical formula of illites should be calculated on the basis of six tetrahedral plus octahedral cations.

Some aspects of the crystal structure of illite are not understood properly yet, in spite of its abundance and significance as a component of soils, sediments, and low-grade metamorphic rocks. The present study aimed to explore the role of hydronium cations in the interlayer space of illite in a theoreticalexperimental approach in order to clarify previous controversial reports. The infrared spectroscopy of this mineral has been studied experimentally and by means of atomistic calculations at the quantum mechanical level. The tetrahedral charge is critical for the stability of the hydronium cations, the presence of which has probably been underestimated in previous studies. In the present study, computational studies have shown that the hydronium cations in aqueous solutions are likely to be intercalated in the interlayer space of illite, exchanging for K cations. During the drying process these cations are stabilized by hydrogen bonds in the interlayer space of illite.

The mechanism for the kaolinization of smectite is extremely complex. The purpose of this study was to explore this mechanism by providing more microscopic information about kaolinite-smectite (K-S) intermediate phases. Crystal-chemical changes were investigated and integrated in a model of the transformation mechanism. Eight K-S samples from three localities, derived from volcanic ash beds, were studied using transmission and analytical electron microscopy (TEM, AEM) and high-resolution TEM (HRTEM). The study completes a previous investigation, using several analytical techniques. The samples cover the range of K-S composition available from the previously studied sample set. Analysis by TEM indicated the preservation of particle morphology throughout the process. Most K-S particles had anhedral, smectite-like morphology, and only the most kaolinitic specimen revealed the coexistence of anhedral and euhedral, hexagonal particles. Analytical electron microscopy showed large chemical variations within samples, corresponding to various degrees of smectite kaolinization. Comparison of chemical results (Si/Al) and d060 values (proxy for octahedral composition) with the extent of kaolinization from thermogravimetry (TG) indicates that chemical changes in the octahedral sheet occur mainly when the proportion of kaolinite is 40–70%. The results above are consistent with kaolinization occurring via layer-by-layer transformation through the progressive loss of individual tetrahedral sheets in smectite layers and subsequent chemical changes in the octahedral sheet. Such a mechanism would produce the results observed in this study: (1) most particles preserve their original morphology; (2) significant variation in terms of the extent of transformation of particles within samples, and (3) formation of crystal structures intermediate between those of smectite and kaolinite, with parts of the tetrahedral sheets missing (kaolinite-like patches). Such structures become least stable at kaolinite ∼50%, when the perimeter of the kaolinite-like patches is largest and chemical changes in the octahedral sheet can occur more easily. Kaolinite layers could not be resolved by HRTEM in most cases and showed lattice fringes corresponding to superstructures. A model was established to quantify kaolinite and smectite layers in the HRTEM images with results which matched TG-derived values.

The effects of a subvolcanic intrusion on its host rocks in the Priego de Córdoba area (SE Spain) was studied by optical microscopy, X-ray diffraction and electron microscopy. The intrusion of a laccolith of stratiform dolerite in partially consolidated marly sediments at quite shallow depths below the ocean floor took place during the intracontinental rifting phase of the Subbetic zone of the Betic Cordilleras. In the first stage, contact metamorphism caused the crystallization of calc-silicate consisting of grossular andradite garnet, diopside, vesuvianite and titanite for which the upper temperature limit was 500°C. Phyllosilicates are found in a network of veins cross-cutting the carbonate and calc-silicate matrix, indicating their formation during a process of hydrothermal alteration superimposed on the contact aureole. In the area closest to the subvolcanic rocks, saponite is the main phyllosilicate although some dispersed chlorite is found. In the zone furthest from the contact, corrensite together with saponite and beidellitic smectites were observed. The presence of low-temperature phases (saponite) in the area closest to the laccolith reveals the evolution of the hydrothermal system toward cooler conditions. In the early stage, the circulation of a hot hydrothermal fluid caused the crystallization of chlorite in the area surrounding the subvolcanic body and corrensite in the more distal area, which might have begun even during the contact metamorphism stage. A cooling phase followed, resulting in the crystallization of saponite in the host rocks, and the crystallization of dioctahedral and trioctahedral smectites inside the subvolcanic body.

Clay processes, mineral reactions, and element budgets in oceans continue to be important topics for scientific investigation, particularly with respect to understanding better the roles of chemistry, formation mechanism, and input from hydrothermal fluids, seawater, and non-hydrothermal mineral phases.To that end, the present study was undertaken.Thre e samples of submarine metalliferous sediments of hydrothermal origin were studied to investigate the formation of smectite, usually Fe-rich, which takes place in such environments.The samples are from the historical collection returned by the British HMS Challenger expedition (1872–1876) and kept at the Natural History Museum in London.The samples were collected from the vicinity of the Pacific–Antarctic Ridge and the Chile Ridge.The samples were analyzed by means of X-ray diffraction (XRD), chemical analysis, scanning electron microscopyenergy dispersive X-ray spectroscopy (SEM-EDX), infrared (IR), and transmission electron microscopyanalytical electron microscopy (TEM-AEM).After removal of biogenic calcite the samples appeared to consist mainly of two low-crystallinity phases mixed intimately: Fe/Mn (oxyhydr)oxides and a Si-Al-Mg- Fe phase of similar chemical characteristics to smectite and with variable proportions of the above elements, as indicated by XRD, IR, and SEM-EDX.In particular, analysis by XRD revealed the presence of highly disordered δ-MnO2.The TEM-AEM analysis showed that Fe/MnOOH particles have Fe/Mn ratios in the range 25–0.2 and textures changing from granular to veil-like as the proportion ofMn increased. The smectite-like material has the morphology and chemistry of smectite, as well as 10–15 Å lattice fringes. Selected area electron diffraction (SAED) patterns indicated a very poorly crystalline material: in some cases distances between diffraction rings corresponded to d values of smectite.The smectite composition indicated a main Fe-rich dioctahedral component with a substantialMg-rich trioctahedral component (total octahedral occupancy between 2.02 and 2.51 atoms per O10[OH]2). The (proto-) smectite is interpreted to have formed within the metalliferous sediment, as a slow reaction between Fe/MnOOH, seawater (providing Mg), detrital silicates from the continent (providing Si and Al), and X-ray amorphous silica of hydrothermal origin that adsorbed on Fe/MnOOH phases and deposited with them.This material is possibly in the process of maturation into well crystallized smectite.

The arguments of Vidal et al. (2010) against the incorporation of H3O+ rather than of H2O in the interlayer position of illite are disputable. Stoichiometric arguments do indeed suggest that the excess water in the Silver Hill illite is in the formof H3O+. No reason exists to assume less water content in the IMt-2 sample than in those determined by Hower and Mowatt (1966) and confirmed by the thermogravimetric analyses of Nieto et al. (2010). The comparison between element contents calculated from end-members and those from the structural formula in figure 1 of Vidal et al. (2010) is not an experimental result, but rather a trivial mathematical artifact. The fact that thermodynamic models, based on the incorporation of interlayer H2O in illite, may provide reasonable estimates neither proves nor disproves the presence of H3O+; this is because thermodynamics is a non-atomistic, macroscopic approach.

Two preferred textures were observed in the Alhama de Murcia Fault rocks: (a) foliated bands (>100 µm thick) rich in well-crystallized dioctahedral micas, quartz, hematite and dolomite; and (b) ultrafine-grained bands (<100 µm thick) made of patches composed of small mica crystals (<15 µm) and dispersed Fe-oxides. In both textures, kaolinite forms intergrowths or patches of randomly oriented crystals filling gaps or opening layers of presumably inherited detrital mica crystals, which is interpreted as an epitaxial growth from fluids. The Na/K ratio of mica crystals in the thin ultrafine-grained bands shows a wider range than the micas from the foliated bands including muscovitic, intermediate Na/K and paragonitic compositions. The absence of the 0.98 nm intermediate peak in the diffractograms indicates that the small micas are submicroscopically paragonite and phengite intergrowths. The d001 values of the K-dioctahedral micas in the <2 µm and whole fractions are clearly different from each other. The d001 values of micas of the <2 µm fraction are larger, indicating a higher K and lower Na content in the small micas. Their composition corresponds to lower temperatures, suggesting their growth during a genetic episode in the fault. The textural relationships indicate a late growth of kaolinite, probably due to the fluid–rock interaction along fault planes and fractures. The neoformed clay minerals might alter the stability of the fault plane. The absence of expandable clay minerals and the relatively high frictional strength of kaolinite under wet conditions might explain the observed velocity-neutral behaviour of this gouge and earthquake propagation towards the surface.

The present study examines the micro- and nano-texture and composition of ammonium-bearing and potassium micas in very-low grade metamorphic black Silurian shales from the SE Iberian Range (NE Spain). Two organic-rich shales were studied by X-ray diffraction (XRD), infrared spectroscopy (IR), transmission electron microscopy (TEM), analytical electron microscopy (AEM) and electron energy loss spectroscopy (EELS). The XRD showed the presence of two populations of micas: pure K micas with d001 = 9.98 Å and ammonium-bearing micas with larger d001 values (10.08 Å and 10.05 Å). The latter values indicate NH4 contents between 13 and 29% in the interlayer, which was confirmed by IR. Interstratifications of smectite and mica layers in the mica packets were not detected by XRD and TEM. Mica packets with sizes ranging from 100 to 250 Å show disordered polytypes and (001) lattice fringes that reflect the presence of K- and NH4-bearing layers (9.9–10.2 Å).

The combination of AEM and EELS analyses on powdered and lamellar samples indicates that micas have typical dioctahedral compositions with highly variable K contents. This variation in K is consistent with the presence of K and NH4 in the interlayers, even though the NH4 and K are not distributed homogeneously; rather they are segregated in nm-sized domains in the mica interlayer.

In the northernmost Calchaquí Valley (Salta, Argentina), the Paleogene continental sediments show a transition from smectite, at the top, to R3 I-S (>90% illite) through R1 I-S (65–80% illite), in contrast to the remaining sectors, containing smectite up to the bottom. Samples at the base of the succession were characterized by high-quality step-scan X-ray diffraction (XRD), scanning electron microscopy (SEM) and analytical high-resolution transmission electron microscopy (HRTEM). Analysis by SEM demonstrated dissolution of primary phases (feldspars, micas and quartz) and crystallization of illite, I-S and kaolinite. As this alteration is not pervasive, an intermediate fluid/rock ratio could be inferred. The lattice-fringe images of the samples from upper parts of the sequence show abundant I1-rich areas, whereas in the lower parts of the sequence, illite packets and I3 I-S coexist and compositions evolve towards muscovite (tetrahedral-charge increase, principally compensated by Mgby- Al substitution in octahedral sites and by a slight decrease in Ca in interlayer sites). As burial temperatures were probably similar in all the samples, depth was not responsible for the illite formation at the bottom. The TEM textures suggest that illitization proceeded mainly by dissolution-crystallization. The active faults close to the northern Calchaquí Valley probably promoted the circulation of hot, deep fluids, favouring illitization.

Introduction. Tejocote (Crataegus spp.) is an edible fruit species that some Mesoamerican cultures have cultivated since pre-Hispanic times in Mexico; however, this fruit crop has not undergone formal breeding. It is unknown whether morphological markers associated with fruit size exist to be used for indirect selection; this could be important, because this species has a large cycle. Our research aimed at studying phenotypic correlations between leaf and stomata characters with fruit weight; such correlations might be used as morphological markers for selection of superior germplasm for fruit weight. Materials and methods. Pearson’s correlation coefficients of 36 leaf variables and three leaf stomata variables with fruit weight were calculated in 94 genotypes of four different species. Results. As expected, the correlations calculated for each species and for the species pool differed. However, the number of veins in leaves of reproductive shoots was positively correlated with fruit weight (P ≤ 0.05) in the two most important horticultural species. On the other hand, C. mexicana was the best option for selecting superior germplasm, and the most significant variables correlated with fruit weight in this species were leaf major axis length of large vegetative shoots, leaf elongation ratio and number of veins of reproductive shoot leaves. Discussion. These variables could be good selection indices or morphological markers that can be used for early screening of germplasm for yield potential.

This study examined phonemic (letters), semantic (animals) and action verbal fluency cues in twenty-four patients with FRDA, and twenty matched healthy control subjects. The Action Fluency Test (AFT) is a newly-developed verbal fluency cue that consists in asking the subject to rapidly generate verbs. Given the high presence of dysarthria and cognitive slowness in FRDA patients, control tasks were administered in order to dissociate motor/articulatory impairment and cognitive slowness from verbal fluency deficit. Results showed that patients and control subjects performed similarly on the semantic fluency task. In contrast, patients performed significantly poorer on phonemic and action fluency tests. Correlational analyses showed that the deficits cannot be attributed to dysarthria or cognitive slowness. Although executive processes are necessary for initiating and monitoring all verbal fluency tasks, phonemic and action fluency may place a greater burden on strategic processes, given that they require a more unusual type of lexicon search. Thus, the deficits found occur in tasks that require greater executive/prefrontal control. This impairment might be the result of an affectation of cerebellum-prefrontal cortex connections, although the possibility of a primary prefrontal dysfunction remains to be investigated. (JINS, 2007, 13, 944–952.)

Field surveys were carried out in coffee plantations in Chiapas, Mexico, to collect and identify fungi associated with the cuticle, gut, faeces and galleries of the coffee berry borer, Hypothenemus hampei. Insects and coffee berries containing galleries were collected in three coffee farms at different altitudes: Rosario Izapa (425 m), La Alianza (700 m) and Monteperla (950 m). An additional sample consisting of coffee berry borers reared in the laboratory on meridic diets was also included. Results show that there is a great diversity of fungi associated with this insect. 212 cultures, including 40 species distributed in 22 genera, were isolated. The recovery of fungi from the galleries was markedly less than from the borer's body. Three of the isolated species were undescribed; two belonging to the Penicillium and one to Hanseniaspora. Most of the species were collected from the cuticle of the insect, and the presence of fungi was not correlated with altitude. Fusarium, Penicillium, Candida and Aspergillus were the dominant genera with percentage abundance of 26.4, 18.7, 13.4 and 12.5%, respectively. The present study provides a detailed description of the mycobiota associated with H. hampei and represents a significant advance in the understanding of the relationship among this insect and the fungi associated with it.