Quantitative X-ray Maps Analaysis of Composition and Microstructure of Permian High-Temperature Relicts in Acidic Rocks from the Sesia-Lanzo Zone Eclogitic Continental Crust, Western Alps

Three samples of meta-acidic rocks with pre-Alpine metamorphic relicts from the Sesia-Lanzo Zone eclogitic continental crust were investigated using stepwise controlled elemental maps by means of the Quantitative X-ray Maps Analyzer (Q-XRMA). Samples were chosen with the aim of analysing the reacting zones along the boundaries between the pre-Alpine and Alpine mineral phases, which developed in low chemically reactive systems. The quantitative data treatment of the X-ray images was based on a former multivariate statistical analytical stage followed by a sequential phase and sub-phase classification and permitted to isolate and to quantitatively investigate the local paragenetic equilibria. The parageneses thus observed were interpreted as related to the pre-Alpine metamorphic or magmatic stages as well as to local Alpine re-equilibrations. On the basis of electron microprobe analysis, specific compositional ranges were defined in micro-domains of the relict and new paragenetic equilibria. In this way calibrated compositional maps were obtained and used to contour different types of reacting boundaries between adjacent solid solution phases. The pre-Alpine and Alpine mineral parageneses thus obtained allowed to perform geothermobarometry on a statistically meaningful and reliable dataset. In general, metamorphic temperatures cluster at 600–700 ∘C and 450–550 ∘C, with lower temperatures referred to a retrograde metamorphic re-equilibration. In all the cases described, pre-Alpine parageneses were overprinted by an Alpine metamorphic mineral assemblage. Pressure-temperature estimates of the Alpine stage averagely range between 420 to 550 ∘C and 12 to 16.5 kbar. The PT constraints permitted to better define the pre-Alpine metamorphic scenario of the western Austroalpine sectors, as well as to better understand the influence of the pre-Alpine metamorphic inheritance on the forthcoming Alpine tectonic evolution.

Improving Calibration Strategy for LIBS Heavy Metals Analysis in Agriculture Applications

A new calibration procedure, known as mapping conditional-calibration laser-induced breakdown spectroscopy (LIBS), has been suggested to improve analysis results for heterogeneous samples. The procedure is based on LIBS elemental mapping, followed by signal conditioning in every sampling spot to skip signal outliers, then by finalizing the calibration curve construction. The suggested mapping conditional calibration procedure was verified for zinc analysis in soybean grist samples. The laser parameters correspond to those of the hand-held LIBS instrument in order to estimate the influence of sample surface heterogeneity under on-site analysis conditions. The laser spot (60 μm) was equal to or smaller than the typical size of grist particles (40–500 μm) but laser crater dimensions were significantly greater and varied widely (150–450 μm). The LIBS mapping of different spectral signals (atomic and ionic lines for major and minor components) was achieved. Elemental maps were normalized to achieve signal maps that were conditionally spotted to skip signal outliers. It was demonstrated that the suggested mapping conditional-calibration LIBS provided 15 ppm RMSECV for zinc determination in heterogeneous samples, which is typical for agricultural products.

Supplemental Material: Clay templates in Ediacaran vendotaeniaceans: Implications for the taphonomy of carbonaceous fossils

Suplementary figures including field images, additional XRD patterns, MIR spectra, EDS and XRF elemental maps.

Supplemental Material: Clay templates in Ediacaran vendotaeniaceans: Implications for the taphonomy of carbonaceous fossils

Suplementary figures including field images, additional XRD patterns, MIR spectra, EDS and XRF elemental maps.

Crystal Chemistry of Six Grossular Garnet Samples from Different Well-Known Localities

Two isotropic grossular (ideally Ca3Al2Si3O12) samples from (1) Canada and (2) Tanzania, three optically anisotropic grossular samples (3, 4, 5) from Mexico, and one (6) anisotropic sample from Italy were studied. The crystal structure of the six samples was refined in the cubic space group Ia3¯d, using monochromatic synchrotron high-resolution powder X-ray diffraction (HRPXRD) data and the Rietveld method. The compositions of the samples were obtained from electron microprobe analyses (EPMA). The HRPXRD traces show a single cubic phase for two isotropic samples, whereas the four anisotropic samples contain two different cubic phases that were also resolved using X-ray elemental line scans, backscattered electron (BSE) images, and elemental maps. Structural mismatch from two cubic phases intergrown in the birefringent samples gives rise to strain-induced optical anisotropy. Considering the garnet general formula, [8]X3[6]Y2[4]Z3[4]O12, the results of this study show that with increasing unit-cell parameter, the Y-O distance increases linearly and rather steeply, the average <X-O> distance increases just slightly in response to substitution mainly on the Y site, while the Z-O distance remains nearly constant. The X and Z sites in grossular contain Ca and Si atoms, respectively; both sites show insignificant substitutions by other atoms, which is supported by a constant Z-O distance and only a slight increase in the average <X-O> distance. The main cation exchange is realized in the Y site, where Fe3+ (ionic radius = 0.645 Å) replaces Al3+ (ionic radius = 0.545 Å), so the Y-O distance increases the most.

Abstract P-47: Analysis of Phosphorus Distribution in Giant Bacteriophage Capsid by Electron Energy Loss Spectroscopy

Background: We have recently developed a method to visualize the distribution of DNA in the cytoplasm of bacteria by analytical electron microscopy (EM), using the Phosphorus signal (dsDNA contains two phosphate groups per each nucleotide pair), that was detected and mapped onto the image of the cell (Danilova et al, 2020; Loiko et al, 2020). Here we applied this technique to study much smaller objects – the DNA packing inside bacteriophage heads. We studied phiEL, giant phiKZ-like bacteriophage of the Myoviridae family that infects Pseudomonas aeruginosa (Krylov et al, 2003). We have earlier demonstrated that this phage contains an ‘inner body’ inside its capsid, which is responsible for the specific DNA packing (Sokolova et al, 2014). Methods: The phage propagation was performed as described before (Sokolova et al, 2014). A 3 ul sample of purified bacteriophage phiEL was applied to the glow-discharged carbon-coated copper grid and stained with freshly prepared ammonium Molybdate 2% aquatic solution for 30 sec. Grids were loaded into Gatan cooling holder and the temperature of the specimen was kept at -180°C. EELS spectra and phosphorus elemental maps were obtained on JEOL2100 microscope, operating at 200 kV with the Gatan GIF Quantum ER spectrometer in STEM mode. Pixel size was set to 15-20 nm. STEM drift correction was applied after each 40-50 pixels. Each spectrum was obtained at a 6.0 mrad collection angle, 0.25 eV dispersion, and 132 eV energy shift. The spectra from different pixels were aligned to carbon K-edge. Results: Phosphorus mapping inside and outside the bacteriophage capsid was performed (Fig. 1). Outside the capsid, the phosphorus signal was practically absent, which corresponds to the presence of DNA only inside the capsid. The distribution of phosphorus inside the capsid was uneven: the rectangular area in the middle of the capsid contained a weak signal, while a more intense signal was detected on the periphery. This can be explained by the presence of an ‘inner body’ inside (Fig. 1C). Conclusion: Thus, our results justify the possibility of using the analytical EM technique to study the distribution of DNA by mapping Phosphorus in biological nano-objects at relatively low content of the element.

MAP2XANES: a Jupiter interactive notebook for elemental mapping and XANES speciation

MAP2XANES is an intuitive Jupiter notebook that automatizes the analysis of synchrotron X-ray fluorescence imaging and X-ray absorption spectroscopy for the characterization of complex and heterogeneous samples. The notebook uses basic modules and functions from Numpy, Scipy, Pandas, iPywidgets and Matplotlib libraries for a powerful data reduction process that, in just a few clicks, guides the user through the visualization of elemental maps, space-resolved absorption spectra and their automatized analysis. In particular, by means of linear combination fit of the XANES spectra, the notebook determines the chemical species distribution in the sample under investigation. The direct output of the analysis process is the correlation between the different elemental distributions and the spatial localization of the chemical species detected. An application to mineralogy is thus presented, analyzing the Mn2+, Mn3+ and Mn4+ distribution in a mineral sample of hausmannite (Mn2+Mn2 3+O4), courtesy of the Museum of Natural Science of Barcelona.

Blueschist mylonitic zones accommodating syn-subduction exhumation of deeply buried continental crust: the example of the Rocca Canavese Thrust Sheets Unit (Sesia–Lanzo Zone, Italian Western Alps)

The Rocca Canavese Thrust Sheets Unit (RCTU) is a subduction-related mélange that represents the eastern-most complex of the Sesia–Lanzo Zone (SLZ), bounded by the Periadriatic (Canavese) Lineament that separates the Alpine subduction complex from the Southalpine domain. The RCTU is limited to the south by the Lanzo Massif (LM) and to the east by the Eclogitic Micaschists Complex (EMC). Particularly the tectonic contact area of the RCTU, adjacent to the neighbouring SLZ and the LM is characterised by a 100–200-m-thick mylonitic to ultra-mylonitic zone (MZ) that was active under blueschist-to greenschist-facies conditions. Despite the dominant mylonitic structure, some rocks (garnet-bearing gneiss, garnet-free gneiss and orthogneiss) still preserve pre-mylonitic parageneses in meter-sized domains. The scarcity of superposed structures and the small size of relicts impose a detailed microstructural analysis supported by chemical investigation to reconstruct the tectono-metamorphic history of the MZ. Therefore, we integrated the classical meso- and microstructural analysis approach with a novel quantitative technique based on the Quantitative X-Ray Map Analyzer (Q-XRMA), used to classify rock-forming minerals starting from an array of X-ray elemental maps, both at whole thin section and micro-domain scale, as well as to calibrate the maps for pixel-based chemical analysis and end-member component maps, relevant for a more robust conventional geothermobarometer application as well for calculating reliable PT pseudosections. Pre-Alpine relicts are garnet and white mica porphyroclasts in the garnet-bearing gneiss and biotite and K-feldspar porphyroclasts in garnet-free gneiss and orthogneiss, respectively, providing no PT constraints. The Alpine evolution of the MZ rocks, has been subdivided in three deformation and metamorphic stages. The first Alpine structural and metamorphic equilibration stage (D1 event) occurred at a pressure of ca. 1.25–1.4 GPa and at a temperature of ca. 420–510 °C, i.e. under blueschist-facies conditions. The D2 event, characterised by a mylonitic foliation that is pervasive in the MZ, occurred at ca. 0.95–1.1 GPa and ca. 380–500 °C, i.e. under epidote-blueschist-facies conditions. The D2 PT conditions in the MZ rocks are similar to those predicted for the blocks that constitute the RCTU mélange, and they overlap with the exhumation paths of the EMC and LM units. Therefore, the RCTU, EMC and LM rocks became coupled together during the D2 event. This coupling occurred during the exhumation of the different tectono-metamorphic units belonging to both continental and oceanic lithosphere and under a relatively cold thermal regime, typical for an active oceanic subduction zone, pre-dating Alpine continental collision.

Effect of TiB2 addition on the microstructural, electrical, and mechanical behavior of Cu–TiB2 composites processed via spark plasma sintering

In this investigation, copper–TiB2 metal matrix composites were fabricated by spark plasma sintering. The effect of TiB2 (2.5, 5, 7.5, and 10 wt.%) additions on the microstructural, electrical, and mechanical properties of the composites was investigated. There was a remarkable reduction in processing time and temperature by this process as compared to conventional sintering. Scanning electron microscopy with energy dispersive X-ray spectroscopy elemental maps revealed a homogeneous distribution of TiB2 in the copper matrix. The hardness of the composites exhibited no consistent trend with the addition of TiB2. An improvement in tensile strength was observed at the expense of ductility. Electrical conductivity showed a decreasing trend. Morphology of the fracture surfaces was analyzed to predict the nature of failure under tensile load.