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Abstract: Understanding the role of metal ions in normal and abnormal cell function continues to emerge as a critical research area in the biological and biochemical sciences. This is especially true in the context of brain health and neurodegenerative diseases, as the brain is especially enriched in metal ions. A range of microscopy and bioanalytical techniques are available to assist in characterizing and observing changes to the brain metallome. As is the case in many other scientific fields, the integration of multiple analytical methods often yields a more complete chemical picture and deeper biological understanding. Herein, we present a case study applying 4 different analytical methods to provide spatially resolved characterization of chemical and biochemical parameters relating to the iron (Fe) metallome within a specific brain region, cornu ammonis sector 1 (CA1) of the hippocampus. The CA1 hippocampal sector was chosen for investigation due to its known endogenous enrichment in Fe and its selective vulnerability to neurodegeneration. The 4 analytical techniques applied were X-ray fluorescence microscopy (to quantify Fe distribution); X-ray absorption near-edge structure (XANES) spectroscopy to reveal information on Fe oxidation state and coordination environment; immuno-fluorescence to reveal relative abundance of Fe storage proteins (heavy chain ferritin and mitochondrial ferritin); and spatial transcriptomics to reveal gene expression pathways relevant to Fe homeostasis. Collectively, the results highlight that although pyramidal neurons in lateral and medial regions of the hippocampal CA1 sector are morphologically similar, key differences in the Fe metallome are evident. The observed differences within the hippocampal CA1 sector potentially indicate a higher oxidative environment and higher metabolic turnover in medial CA1 neurons relative to lateral CA1 neurons, which may account for the heightened vulnerability to neurodegeneration that is observed in the medial CA1 sector.

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Abstract: The deposition of calcium phosphate mineral within a collagen matrix plays a pivotal role in the formation of bone and teeth, yet understanding its precise mechanism and time-dependence remains a significant challenge. Conventional approaches are often constrained to ex situ studies and as a result the intrinsic dynamics governing collagen mineralization remains unclear. To address this knowledge gap, we developed a custom thermal flow cell to enable in situ characterization using Raman spectroscopy and small/wide-angle X-ray scattering for comparable sample settings. This approach allowed us to monitor the intricate process of collagen matrix mineralization from the initial infiltration of precursor phases to the formation of intermediate phosphate phases, and ultimately to the predominant growth of hydroxyapatite. Our findings reveal a striking expansion of the collagen matrix during initial infiltration, followed by compression in the early stages of mineralization, likely driven by water expulsion, which suggests the development of pre-stress similar to that observed in bone. As mineralization progressed, the matrix expanded once again, correlated with crystal growth. Post-mortem analyses confirmed the presence of intrafibrillar mineralization, with remarkable agreement to bone formation at up to 9 h of mineralization before over-mineralization occurred. Our study further identified a tessellated mineralization pattern within the collagen matrix, a feature also seen in bone, pointing to a highly regulated physico-chemical control of the mineralization dynamics. These insights deepen our understanding of the fundamental processes governing bone mineralization with broad implications for designing advanced biomaterials.

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Abstract: Achieving safe and sustainable nanomaterials remains challenging—not necessarily from limited synthetic innovation but due to gaps in observing structural and chemical transformations under environmental conditions. Here, we make a call for a tri-beam operando characterization strategy, integrating synchrotron, neutron, and X-ray free-electron laser (XFEL) techniques into one synergistic experimental framework. Unlike traditional methods providing disconnected snapshots, tri-beam analysis dynamically tracks nanomaterial evolution from atomic-scale changes to structural collapse under near-real-world/quasi-realistic conditions. This holistic approach reveals previously hidden degradation pathways, transient states, and physicochemical thresholds that reshape definitions of material safety. Enhanced by robotic automation, machine learning, and findable, accessible, interoperable, and reusable (FAIR) data principles, our method directly supports Europe’s safe and sustainable by design (SSbD) initiative. We propose embedding tri-beam datasets into regulatory standards, predictive models, and AI-driven screening workflows. Ultimately, tri-beam operando characterization represents a transformative platform for designing resilient, high-performance nanomaterials that meet the environmental and societal demands of the 21st century.

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Abstract: This chapter (Nano-Imaging for Advanced X-ray Fluorescence and Absorption Spectroscopy Applications) is a contribution to the Geostandards and Geoanalytical Research Handbook of Rock and Mineral Analysis – an online textbook that is a fully revised and updated edition of A Handbook of Silicate Rock Analysis (P. J. Potts, 1987, Blackie, Glasgow). Chapter 16 (from Section 3 of the handbook devoted to microbeam techniques) has been designed to provide a coherent progression, starting with a brief introduction of the essential fundamentals and the practical information needed to understand the experimental specifics of nano-XRF imaging. This concise yet crucial information is followed by a comprehensive presentation of current applications of nano-XRF imaging, with examples showcasing elemental measurement and XAS applications based on nano-XRF imaging. To conclude, the final section offers a brief overview of emerging perspectives that should be of particular interest to young researchers at the beginning of their careers.

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Abstract: Renewable sources could replace hydrocarbons, but sustainability imposes the integration with reliable and efficient energy storage (EES) facilities like rechargeable batteries. The ssuccessful operation of rechargeable batteries depends on the concerted occurrence of an enormous number of physico-chemical, electrical, thermal and mechanical processes, taking place over wide spatial (nm - cm) and temporal (10-14s - hours) ranges. Disentangling this scenario, to gain control over their relative roles on practical operation, durability and safety, calls for the capability of imaging what happens inside batteries at length-scales ranging from material structure up to battery components at the device scale, and correlating this information with the electrical performance over time. This perspective implies joint efforts in three key directions: (i) the acquisition of focused in operando data, in real-life or close to real-life conditions; (ii) their multiscale modelling and (iii) integration of this information into electrical diagnostics and control tools. Synchrotron-based scanning nanoprobes can contribute crucially to point (i) and provide unique factual input for points (ii) and (iii). Wide range of novel electrochemical cells for in operando muti-modal spectro-microscopy are designed and these systems provide fundamental answers to technologically relevant questions raised by R&D on state-of-the art as well as next-generation lithium and post-lithium battery studies and developments. Among realistic cell configurations, both coin-cells and pouch cells with an optical window, featuring specially – but straightforwardly – shaped electrodes, can be used for in situ and in operando measurements. Here, we present the current capabilities of the I14 and I08 beamlines at Diamond Light Source UK, which are in user operation mode, as well as give an outline of planned future upgrades. We describe our current instrumentation and software infrastructure, including an automated processing pipeline that provides users with a ptychographic reconstruction in near real time. We show results from a few scientific examples of in-operando and in-situ studies on batteries and catalysts samples using multi-modal X-ray Nanoprobes which allow the use of imaging and spectroscopy to access nanoscale chemical and structural information. Spectro-ptychography offers the unique capability to image in-operando electrochemical cells at high spatial resolution and with chemical specificity, further enhanced by the upcoming upgrade to Diamond II with an expected increase in coherent flux.