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Multimodal imaging and spectroscopy like concurrent scanning transmission X-ray microscopy (STXM) and X-ray fluorescence (XRF) are highly desirable as they allow retrieving complementary information. This paper reports on the design, development, integration and field testing of a novel in situ atomic force microscopy (AFM) instrument for operation under high vacuum in a synchrotron soft X-ray microscopy STXM–XRF end-station. A combination of μXRF and AFM is demonstrated for the first time in the soft X-ray regime, with an outlook for the full XRF–STXM–AFM combination. [ABSTRACT FROM AUTHOR]

Scanning microscopies and spectroscopies like X-ray Fluorescence (XRF), Scanning Transmission X-ray Microscopy (STXM), and Ptychography are of very high scientific importance as they can be employed in several research fields. Methodology and technology advances aim at analysing larger samples at better resolutions, improved sensitivities and higher acquisition speeds. The frontiers of those advances are in detectors, radiation sources, motors, but also in acquisition and analysis software together with general methodology improvements. We have recently introduced and fully implemented an intelligent scanning methodology based on compressive sensing, on a soft X-ray microscopy beamline. This demonstrated sparse low energy XRF scanning of dynamically chosen regions of interest in combination with STXM, yielding spectroimaging data in the megapixel-range and in shorter timeframes than were previously not feasible. This research has been further developed and has been applied to scientific applications in biology. The developments are mostly in the dynamic triggering decisional mechanism in order to incorporate modern Machine Learning (ML) but also in the suitable integration of the method in the control system, making it available for other beamlines and imaging techniques. On the applications front, the method was previously successfully used on different samples, from lung and ovarian human tissues to plant root sections. This manuscript introduces the latest methodology advances and demonstrates their applications in life and environmental sciences. Lastly, it highlights the auxiliary development of a mobile application, designed to assist the user in the selection of specific regions of interest in an easy way. [ABSTRACT FROM AUTHOR]

The release of nanoplastics (NPs) in the environment is a significant health concern for long-term exposed humans. Although their usage has certainly revolutionized several application fields, at nanometer size, NPs can easily interact at the cellular level, resulting in potential harmful effects. Micro/Nanoplastics (M/NPs) have a demonstrated impact on mammalian endocrine components, such as the thyroid, adrenal gland, testes, and ovaries, while more investigations on prenatal and postnatal exposure are urgently required. The number of literature studies on the NPs' presence in biological samples is increasing. However, only a few offer a close study on the model environmental NP-immune system interaction exploited by advanced microscopy techniques. The present study highlights substantial morphological and lipid metabolism alterations in human M1 macrophages exposed to labeled polypropylene and polyvinyl chloride nanoparticles (PP and PVC NPs) (20 mg/ml). The results are interpreted by advanced microscopy techniques combined with standard laboratory tests and fluorescence microscopy. We report the accurate detection of polymeric nanoparticles doped with cadmium selenide quantum dots (CdSe-QDs NPs) by following the Se (L line) X-ray fluorescence emission peak at higher sub-cellular resolution, compared to the supportive light fluorescence microscopy. In addition, scanning transmission X-ray microscopy (STXM) imaging successfully revealed morphological changes in NP-exposed macrophages, providing input for Fourier transform infrared (FTIR) spectroscopy analyses, which underlined the chemical modifications in macromolecular components, specifically in lipid response. The present evidence was confirmed by quantifying the lipid droplet (LD) contents in PP and PVC NPsexposed macrophages (0-100 mg/ml) by Oil Red O staining. Hence, even at experimental NPs' concentrations and incubation time, they do not significantly affect cell viability; they cause an evident lipid metabolism impairment, a hallmark of phagocytosis and oxidative stress. [ABSTRACT FROM AUTHOR]

An improved understanding of an ovary's structures is highly desirable to support advances in folliculogenesis knowledge and reproductive medicine, with particular attention to fertility preservation options for prepubertal girls with malignant tumors. Although currently the golden standard for structural analysis is provided by combining histological sections, staining, and visible 2D microscopic inspection, synchrotron radiation phase-contrast microtomography is becoming a new challenge for three-dimensional studies at micrometric resolution. To this aim, the proper use of contrast agents can improve the visualization of internal structures in ovary tissues, which normally present a low radiopacity. In this study, we report a comparison of four staining protocols, based on iodine or tungsten containing agents, applied to bovine ovarian tissues fixed in Bouin's solution. The microtomography (microCT) analyses at two synchrotron facilities under different set-ups were performed at different energies in order to maximize the image contrast. While tungsten-based agents allow large structures to be well identified, Iodine ones better highlight smaller features, especially when acquired above the K-edge energy of the specific metal. Further scans performed at lower energy where the setup was optimized for overall quality and sensitivity from phase-contrast still provided highly resolved visualization of follicular and intrafollicular structures at different maturation stages, independent of the staining protocol. The analyses were complemented by X-ray Fluorescence mapping on 2D sections, showing that the tungsten-based agent has a higher penetration in this type of tissues. [ABSTRACT FROM AUTHOR]

Scanning transmission X-ray microscopy (STXM) provides the imaging of biological specimens allowing the parallel collection of localized spectroscopic information by X-ray fluorescence (XRF) and/or X-ray Absorption Near Edge Spectroscopy (XANES). The complex metabolic mechanisms which can take place in biological systems can be explored by these techniques by tracing even small quantities of the chemical elements involved in the metabolic pathways. Here, we present a review of the most recent publications in the synchrotrons' scenario where soft X-ray spectro-microscopy has been employed in life science as well as in environmental research. [ABSTRACT FROM AUTHOR]

Background: Although X-ray fluorescence microscopy is becoming a widely used technique for single-cell analysis, sample preparation for this microscopy remains one of the main challenges in obtaining optimal conditions for the measurements in the X-ray regime. The information available to researchers on sample treatment is inadequate and unclear, sometimes leading to wasted time and jeopardizing the experiment's success. Many cell fixation methods have been described, but none of them have been systematically tested and declared the most suitable for synchrotron X-ray microscopy. Methods: The HEC-1-A endometrial cells, human spermatozoa, and human embryonic kidney (HEK-293) cells were fixed with organic solvents and cross-linking methods: 70% ethanol, 3.7%, and 2% paraformaldehyde; in addition, HEK-293 cells were subjected to methanol/ C3H6O treatment and cryofixation. Fixation methods were compared by coupling low-energy X-ray fluorescence with scanning transmission X-ray microscopy and atomic force microscopy. Results: Organic solvents lead to greater dehydration of cells, which has the most significant effect on the distribution and depletion of diffusion elements. Paraformaldehyde provides robust and reproducible data. Finally, the cryofixed cells provide the best morphology and element content results. Conclusion: Although cryofixation seems to be the most appropriate method as it allows for keeping cells closer to physiological conditions, it has some technical limitations. Paraformaldehyde, when used at the average concentration of 3.7%, is also an excellent alternative for X-ray microscopy. [ABSTRACT FROM AUTHOR]

Label-free spectromicroscopy methods offer the capability to examine complex cellular phenomena. Electron and X-ray based spectromicroscopy methods, though powerful, have been hard to implement with hydrated objects due to the vacuum incompatibility of the samples and due to the parasitic signals from (or drastic attenuation by) the liquid matrix surrounding the biological object of interest. Similarly, for many techniques that operate at ambient pressure, such as Fourier transform infrared spectromicroscopy (FTIRM), the aqueous environment imposes severe limitations due to the strong absorption of liquid water in the infrared regime. Here we propose a microfabricated multi-compartmental and reusable hydrated sample platform suitable for use with several analytical techniques, which employs the conformal encapsulation of biological specimens by a few layers of atomically thin graphene. Such an electron, X-ray, and infrared transparent, molecularly impermeable and mechanically robust enclosure preserves the hydrated environment around the object for a sufficient time to allow in situ examination of hydrated bio-objects with techniques operating under both ambient and high vacuum conditions. An additional hydration source, provided by hydrogel pads lithographically patterned in the liquid state near/around the specimen and co-encapsulated, has been added to further extend the hydration lifetime. Note that the in-liquid lithographic electron beam-induced gelation procedure allows for addressable capture and immobilization of the biological cells from the solution. Scanning electron microscopy and optical fluorescence microscopy, as well as synchrotron radiation based FTIR and X-ray fluorescence microscopy, have been used to test the applicability of the platform and for its validation with yeast, A549 human carcinoma lung cells and micropatterned gels as biological object phantoms. [ABSTRACT FROM AUTHOR]

X-ray ptychography is an advanced computational microscopy technique, which is delivering exceptionally detailed quantitative imaging of biological and nanotechnology specimens, which can be used for high-precision X-ray measurements. However, coarse parametrisation in propagation distance, position errors and partial coherence frequently threaten the experimental viability. In this work, we formally introduce these actors, solving the whole reconstruction as an optimisation problem. A modern deep learning framework was used to autonomously correct the setup incoherences, thus improving the quality of a ptychography reconstruction. Automatic procedures are indeed crucial to reduce the time for a reliable analysis, which has a significant impact on all the fields that use this kind of microscopy. We implemented our algorithm in our software framework, SciComPty, releasing it as open-source. We tested our system on both synthetic datasets, as well as on real data acquired at the TwinMic beamline of the Elettra synchrotron facility. [ABSTRACT FROM AUTHOR]

Soft X-ray microscopy coupled with low energy X-ray fluorescence is a powerful tool for investigating complex biological systems like cells and tissues. Due to certain characteristics of X-ray sources, sample stage motors, and detectors, the examination of large areas at high resolutions is very time consuming, often confining the analysis only to a restricted number of pre-selected representative regions. Here we propose and demonstrate a compressive sensing method that provides an alternative approach for overcoming such limitations and can be applied to different kinds of samples and other microscopy and analytical techniques. [ABSTRACT FROM AUTHOR]

Progress in nanotechnology calls for material probing techniques of high sensitivity and resolution. Such techniques are also used for high-impact studies of nanoscale materials in medicine and biology. Soft X-ray microscopy has been successfully used for investigating complex biological processes occurring at micrometric and sub-micrometric length scales and is one of the most powerful tools in medicine and the life sciences. Here, we present the capabilities of the TwinMic soft X-ray microscopy end-station at the Elettra synchrotron in the context of medical and biological imaging, while we also describe novel uses and developments. [ABSTRACT FROM AUTHOR]

Hydrophobic treatment is one of the most important interventions usually carried out for the conservation of stone artefacts and monuments. The study here reported aims to answer a general question about how two polymers confer different protective performance. Two fluorinated-based polymer formulates applied on samples of Cusa's stone confer a different level of water repellence and water vapour permeability. The observed protection action is here explained on the basis of chemico-physical interactions. The distribution of the polymer in the pore network was investigated using scanning electron microscopy and X-ray microscopy. The interactions between the stone substrate and the protective agents were investigated by means of solid state NMR spectroscopy. The ss-NMR findings reveal no significant changes in the chemical neighbourhood of the observed nuclei of each protective agent when applied onto the stone surface and provide information on the changes in the organization and dynamics of the studied systems, as well as on the mobility of polymer chains. This allowed us to explain the different macroscopic behaviours provided by each protective agent to the stone substrate. [ABSTRACT FROM AUTHOR]

Radiation damage upon soft X‐ray exposure is an important issue to be considered in soft X‐ray microscopy. The work presented here is part of a more extended study on the topic and focuses on the effects of soft X‐rays on paraffin, a common embedding medium for soft‐tissues, and on ultralene and Si3N4 windows as sample supports. Our studies suggest that the sample environment indeed plays an important role in the radiation damage process and therefore should be carefully taken into account for the analysis and interpretation of new data. The radiation damage effects were followed over time using a combination of Fourier transform infrared (FTIR) microspectroscopy and X‐ray fluorescence (XRF), and it was demonstrated that, for higher doses, an oxidation of both embedding medium and ultralene substrate takes place after the irradiated sample is exposed to air. This oxidation is reflected in a clear increase of C=O and O—H infrared bands and on the XRF oxygen maps, correlated with a decrease of the aliphatic infrared signal. The results also show that the oxidation process may affect quantitative evaluation of light element concentrations. [ABSTRACT FROM AUTHOR]

As the prospect of human beings exposed to new nanomaterials increases, there are growing concerns about the foetal exposure and effects of such nanomaterials during pregnancy. Among others, due to their ample usage, it becomes urgent to address the vulnerability of the human placental barrier to carbon nanotubes (CNTs). Recently, by applying a combination of advanced synchrotron‐based X‐ray microscopy and X‐ray fluorescence (XRF) techniques, we demonstrated that raw single‐walled CNTs (SWCNTs) may cause an asbestos‐like iron‐related toxicity in mesothelial (MeT5A) cells. This work shows the results obtained with the same approach and experimental conditions in human choriocarcinoma (BeWo) cells as a placental model. XRF microscopy in mild and soft X‐ray regimes was used to map the distribution of P, S, Ca, and Fe in exposed and control cells, whereas absorption and phase‐contrast imaging (soft X‐ray microscopy) provided simultaneous morphological information. The findings show that exposure to SWCNTs affects cell viability and causes a small increase in intracellular iron content, further confirmed by the stimulation of the ferritin protein. It is interesting to note that the iron changes are negligible when highly purified SWCNTs are used. In all tested conditions, including exposure to iron sulfate, the iron accumulation or ferritin increase was much lower in BeWo cells than in MeT5A ones, suggesting a different iron metabolism and possibly a lower vulnerability of the placental barrier to iron‐rich nanomaterials. [ABSTRACT FROM AUTHOR]

It is well recognized that a large number of pulmonary diseases are induced by the effects of inhaled particulates. Anthracosis is defined as an asymptomatic, mild form of pneumoconiosis caused by the accumulation of “black carbon” in the lungs due to repeated exposure to air pollution or inhalation of smoke or coal dust particles. Since the human population is progressively exposed to an increasing number and doses of anthropogenic micro and nano particles/compounds, there is a pressing urgency to explore toxicological impact arising from these exposures and the molecular mechanisms driving the body defense or possible related diseases. The toxicity mechanisms are clearly related to chemical composition and physical and surface properties of materials. A combination of synchrotron radiation-based (SR-based) nano X-ray fluorescence (XRF) imaging and soft X-ray microscopy was used to chemically characterize environmental particulates (anthracosis) in lung tissues from urban subjects with the aim of better understanding the complex nature of related lungs' deposits. High-resolution XRF analyses performed at ESRF and Elettra synchrotrons allowed discriminating single particles in the heterogeneous aggregates found in the lung tissue. The small particles have variable composition resulting from the different combinations of Ti with O, K and Si, Al and Si, or Zn and Fe with O. Interestingly, simultaneous absorption and phase contrast images showed the particulate morphology and allowed to predict the presence of very dense nanoparticles or high concentration of heavy elements. [ABSTRACT FROM AUTHOR]

The current status of the TwinMic beamline at Elettra synchrotron light source, that hosts the European twin X-ray microscopy station, is reported. The X-ray source, provided by a short hybrid undulator with source size and divergence intermediate between bending magnets and conventional undulators, is energy-tailored using a collimated plane-grating monochromator. The TwinMic spectromicroscopy experimental station combines scanning and full-field imaging in a single instrument, with contrast modes such as absorption, differential phase, interference and darkfield. The implementation of coherent diffractive imaging modalities and ptychography is ongoing. Typically, scanning transmission X-ray microscopy images are simultaneously collected in transmission and differential phase contrast and can be complemented by chemical and elemental analysis using across-absorption-edge imaging, X-ray absorption near-edge structure or low-energy X-ray fluorescence. The lateral resolutions depend on the particular imaging and contrast mode chosen. The TwinMic range of applications covers diverse research fields such as biology, biochemistry, medicine, pharmacology, environment, geochemistry, food, agriculture and materials science. They will be illustrated in the paper with representative results. [ABSTRACT FROM AUTHOR]

The last decades have witnessed substantial efforts in the development of several detector technologies for X-ray fluorescence (XRF) applications. In spite of the increasing trend towards performing, cost-effective and reliable XRF systems, detectors for soft X-ray spectroscopy still remain a challenge, requiring further study, engineering and customization in order to yield effective and efficient systems. In this paper we report on the development, first characterization and tests of a novel multielement detector system based on low leakage current silicon drift detectors (SDD) coupled to ultra low noise custom CMOS preamplifiers for synchrotron-based low energy XRF. This new system exhibits the potential for improving the count rate by at least an order of magnitude resulting in ten-fold shorter dwell time at an energy resolution similar to that of single element silicon drift detectors. [ABSTRACT FROM AUTHOR]

Low energy X-ray fluorescence (XRF) and soft X-ray absorption (XAS) microspectroscopies at high space-resolution are employed for the investigation of the coelectrodeposition of composites consisting of a polypyrrole(PPy)-matrix and Mn-based ternary dispersoids, that have been proposed as promising electrocatalysts for oxygen-reduction electrodes. Specifically, we studied Mn-Co-Cu/PP, Mn-Co-Mg/PPy and Mn-Ni-Mg/PPy co-electrodeposits. The Mn-Co-Cu system features the best ORR electrocatalytic activity in terms of electron transfer number, onset potential, half-wave potential and current density. XRF maps and micro-XAS spectra yield compositional and chemical state distributions, contributing unique molecular-level information on the pulse-plating processes. Mn, Ni, Co and Mg exhibit a bimodal distribution consisting of mesoscopic aggregates of micrometric globuli, separated by polymer-rich ridges. Within this common qualitative scenario, the individual systems exhibit quantitatively different chemical distribution patterns, resulting from specific electrokinetic and electrosorption properties of the single components. The electrodeposits consist of 3+,4+-oxide particles, accompanied by combinations of Co0/Co2+, Ni0/Ni2+ and Cu0,+/Cu2+ resulting from the alternance of cathodic and anodic pulses. The formation of highly electroactive Mn3+,4+ in the as-fabricated material is a specific feature of the ternary systems, deriving from synergistic stabilisation brought about by two types of bivalent dopants as well as by galvanic contact to elemental metal; this result represents a considerable improvement in material quality with respect to previously studied Mn/PPy and Mn-based/PPy binaries. [ABSTRACT FROM AUTHOR]

Cobalt/polypyrrole ORR electrocatalysts has been electrochemically synthesized by a potentiostatic anodic/cathodic pulse-plating procedure. The deposition electrochemistry has been studied by cyclic voltammetry and in-situ Micro Raman Spectroscopy complemented with scanning X-ray microscopy and micro-spot X-ray absorption spectroscopy (µ-XAS). Linear sweep voltammetry (LSV) under oxygen reduction has been used to assess the electrocatalytic effect of as-electrodeposited Co/PPy. The obtained results have provided new information about the concomitant electropolymerisation and metal incorporation processes occurring under different pulsed co-electrodeposition conditions, important for optimising the electrosynthesis procedure. The colocation of O and Co, evidenced by the O and Co XRF maps indicates that the Co in the formed composite is in oxidized state and for composites formed at low currents using shorter Co pulses coexistence of both CoO and Co3O4is evidenced by the Co L3XAS spectra. Bimodal Co distribution as micro-grains on a background of nano-grains and co-nulcleation of PPy and Co is evidenced by correlation of Co and N XRF maps. [ABSTRACT FROM AUTHOR]

Background: Increasing evidences support a correlation between magnesium (Mg) homeostasis and colorectal cancer (CRC). Nevertheless, the role of Mg and its transporters as diagnostic markers in CRC is still a matter of debate. In this study we combined X-ray Fluorescence Microscopy and databases information to investigate the possible correlation between Mg imbalance and CRC. Methods: CRC tissue samples and their non-tumoural counterpart from four patients were collected and analysed for total Mg level and distribution by X-Ray Fluorescence Microscopy. We also reviewed the scientific literature and the main tissue expression databases to collect data on Mg transporters expression in CRC. Results: We found a significantly higher content of total Mg in CRC samples when compared to non-tumoural tissues. Mg distribution was also impaired in CRC. Conversely, we evidenced an uncertain correlation between Mg transporters expression and colon malignancies. Discussion: Although further studies are necessary to determine the correlation between different cancer types and stages, this is the first report proposing the measurement of Mg tissue localisation as a marker in CRC. This study represents thus a proof-of-concept that paves the way for the design of a larger prospective investigation of Mg in CRC. [ABSTRACT FROM AUTHOR]

The corrosion control of WC-Co type hardmetals is steadily gaining momentum for novel crucial applications in the Oil & Gas and food industries. The corrosion rate of the Co-based binder, and the extent to which coupling to WC speeds it up, are strongly influenced by alloying. In this paper, we investigate the impact of Cr on the corrosion-product film formation of Co- and Co Ni based hardmetal binders in acidic, neutral and alkaline aqueous solutions. We centred our study on the role of Cr in driving the distribution of oxidized Co and Ni at the micrometre scale, thanks to synchrotron-based soft-X ray microspectroscopy. We have investigated morphochemical distributions for the following grades: Co 96 Cr 4 , Co 48 Ni 48 Cr 4 , Co 50 Cr 50. Chemical-state mapping has been complemented by electrochemical measurements and metallographic observations. Amounts of Cr and Ni of ca. 50% notably increase the corrosion resistance in all ambients, with a stronger beneficial effect of the former element. 4% addition of Cr results in slight positive effects, with the exception of the Co Ni system in alkaline ambient, that, together with Co 50 Cr 50 , outperforms the other grades. In all investigated alloy-ambient combinations, a continuous oxidized metal film grows, onto which micrometric island form of shape and dimensions that depend on the specific grade and aggressive conditions. Quantitative descriptors of chemical-state maps and their theoretical interpretation in terms of electrochemical phase-formation by oxy-hydroxide precipitation, allow to correlate the island patterns with the degree of pseudopassivation. Unlabelled Image • Role of Cr in corrosion resistance of Co- and Co-Ni-based hardmetal model binders. • Corrosion of Co Cr based grades studied in aerated aqueous solutions in pH range 1–10. • Soft-X ray microspectroscopy yields chemical-state maps of pseudopassivation films. • Pseudopassivation layers form oxidized metal patterns, depending on attack conditions. • Corrosion resistance correlates with morphochemical details of oxide film patterns. [ABSTRACT FROM AUTHOR]

In this study, we explore the behaviour of intracellular magnesium during bone phenotype modulation in a 3D cell model built to mimic osteogenesis. In addition, we measured the amount of magnesium in the mineral depositions generated during osteogenic induction. A two-fold increase of intracellular magnesium content was found, both at three and seven days from the induction of differentiation. By X-ray microscopy, we characterized the morphology and chemical composition of the mineral depositions secreted by 3D cultured differentiated cells finding a marked co-localization of Mg with P at seven days of differentiation. This is the first experimental evidence on the presence of Mg in the mineral depositions generated during biomineralization, suggesting that Mg incorporation occurs during the bone forming process. In conclusion, this study on the one hand attests to an evident involvement of Mg in the process of cell differentiation, and, on the other hand, indicates that its multifaceted role needs further investigation. [ABSTRACT FROM AUTHOR]

Human exposure to asbestos can cause a wide variety of lung diseases that are still a current major health concern, even if asbestos has been banned in many countries. It has been shown in many studies that asbestos fibers, ingested by alveolar macrophages, disrupt lung iron homeostasis by sequestering iron. Calcium can also be deposited on the fibers. The pathways along which iron and above all calcium interact with fibers are still unknown. Our aim was that of investigating if the iron accumulation induced by the inhaled asbestos fibers also involves calcium ions accumulation. Lung sections of asbestos-exposed mice were analyzed using an extremely sensitive procedure available at the synchrotron facilities, that provides morphological and chemical information based on X-ray fluorescence microspectroscopy (μ-XRF). In this study we show that (1) where conventional histochemical procedures revealed only weak deposits of iron and calcium, μ-XRF analysis is able to detect significant deposits of both iron and calcium on the inhaled asbestos fibers; (2) the extent of the deposition of these ions is proportionally directly related and (3) iron and calcium deposition on inhaled asbestos fibers is concomitant with the appearance of inflammatory and hyperplastic reactions. [ABSTRACT FROM AUTHOR]

The sodium consumption in many countries is too high, which results in increased risk for hypertension, cardiovascular diseases, stroke and premature death. Inhomogeneous sodium distribution using layering is a viable way to reduce sodium in bread that normally contains a lot of sodium. Prevention of sodium migration during production and storage is important for the function of this approach. Furthermore, the distribution of sodium between starch and gluten influences their properties. The spatial distribution of sodium was investigated at high resolution using combinations of X-ray fluorescence microscopy (XFM), scanning transmission X-ray microscopy (STXM), light microscopy (LM), scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) and image analysis. Reference breads and layered bread samples were baked with one salt-free layer and one layer containing 3.6 wt% sodium chloride salt. The obtained results showed that the concentration of sodium is higher in the starch phase than in the gluten phase and that sodium migrates across the layer interface from the salt-containing to the salt-free layer. The ratios between the sodium concentration in the starch and gluten phases were dependent on the sodium concentration across the interfaces. Furthermore, magnesium and phosphor signals in bread yeast cells were observed using XFM. • New method to investigate the spatial distribution of sodium in bread using advanced microscopy. • High resolution maps of the spatial distribution of sodium between starch and gluten. • Sodium preferentially localises in the starch phase. • Identification of yeast cells in bread using magnesium and phosphor signals. [ABSTRACT FROM AUTHOR]

Electrodeposition of graphene-supported Co for ORR electrocatalysts from an acetonitrile solution has been studied by a multi-technique approach, combining a suite of spectroscopic methods with electrochemical measurements, allowing a molecular-level understanding of potentiostatic and pulsed-potential plating processes from the organic solvent onto a freestanding graphene film. The formation of the graphene film by the light-scribe approach has been monitored by Raman spectroscopy; the electrodeposition process has been clarified by cyclic voltammetry and the compositional and chemical-state distribution of Co have been investigated ex situ by soft X-ray absorption spectroscopy and fluorescence mapping, showing that both spatial distribution and valence state are homogeneous and independent of the local current density. The deposit consists in micrometric aggregates of Co/CoO nanoparticles with diameter ca. 30 nm (pulsed) and 200 nm (potentiostatic deposition). Potentiostatic deposition allows to obtain better ORR electrocatalytic perfomance in terms of nnumber of transferred electrons, onset/ half-wave potential and current density. [ABSTRACT FROM AUTHOR]

Abstract: The effect of the concentration of cobalt ferrite (CoFe2O4) nanoparticles (NPs) on their intracellular location and distribution has been explored by synchrotron radiation X-ray and fluorescence microscopy (SR-XRF) monitoring the evolution of NPs elemental composition as well. In cells exposed to low concentrations of CoFe2O4 NPs, the NPs preferentially segregate in the perinuclear region preserving their initial chemical content. At concentrations exceeding 500μM the XRF spectra indicate the presence of Co and Fe also in the nuclear region, accompanied by sensible changes in the cellular morphology. The increase of the Co/Fe ratio measured in the nuclear compartment indicates that above certain concentrations the CoFe2O4 NPs intracellular distribution could be accompanied by biodegradation resulting in Co accumulation in the nucleus. [Copyright &y& Elsevier]

Abstract: We report a pilot study in in situ electrochemical X-ray dynamic microscopy, based on a model system: the anodic and cathodic behaviour of Ag in neutral NaCl and (NH4)2SO4 aqueous solutions. In situ X-ray imaging highlighted mesoscopic features related to corrosion processes, yielding soluble (NH4 + solution) and insoluble (Cl− solution) corrosion products, as well as cathodic growth morphologies. X-ray absorption and phase contrast images were collected, confirming the feasibility of soft X-ray microscopic measurements with lateral resolution down to a few tens of nm in electrochemical cells for operation in a high vacuum environment in presence of liquid electrolytes. [Copyright &y& Elsevier]

Graphical abstract Highlights • Juncus acutus stores trace elements mainly in the root epidermis. • Zn speciation evolves from the rhizosphere to the different plant compartments. • Biominerals occur as site-specific detoxification mechanisms. Abstract Juncus acutus , an halophite plant pioneer in extremely polluted mine areas, was harvested in three different locations of Sardinia (Italy), having Zn soil concentration up to 80 g/kg, and Zn water concentration ranging between 10−3 g/L and 10−1 g/L. Rhizosphere and plant samples were investigated combining X-ray microscopy (XM)/spectroscopy (XAFS) and infrared microspectroscopy (FTIR) to elucidate the chemical composition, (bio)mineralogy and Zn coordinative environment. The multi-technique approach allowed recognizing different biomineralization processes, and Zn complexes in the plant tissues. The Zn chemical environment in root biominerals is multi-phase and, depending on the sampling site, can comprise amorphous Zn silicate, Zn apatite, hydrozincite, and Zn sulphate. Zn cysteine and Zn histidine, complexes quoted as part of a detoxification strategy, were found mainly in plants from the site where the Zn water concentration has the highest values. This different site-specific mode of Zn biomineralization has relevant implications for phytoremediation techniques and for further biotechnology development, which can be better designed and developed after knowledge of site-specific-molecular processes ruling mineral evolution and biomineralization. Carboxylic groups and organic compounds (lignin, cellulose, hemicellulose, pectin and esters) were identified by FTIR analysis, thought the Zn speciation is not apparently linked to these carboxylic group rich biopolymers. [ABSTRACT FROM AUTHOR]