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We developed universal sample holders [the Kochi grid, Kochi clamp, and Okazaki cell) and a transfer vessel (facility-to-facility transfer container (FFTC)] to analyze sensitive and fragile samples, such as extremely small extraterrestrial materials. The holders and container prevent degradation, contamination due to the terrestrial atmosphere (water vapor and oxygen gas) and small particles, as well as mechanical sample damage. The FFTC can isolate the samples from the effects of the atmosphere for more than a week. The Kochi grid and clamp were made for a coordinated micro/nano-analysis that utilizes a focused-ion beam apparatus, transmission electron microscope, and nanoscale secondary ion mass spectrometry. The Okazaki cell was developed as an additional attachment for a scanning transmission X-ray microscope that uses near-edge X-ray absorption fine structure (NEXAFS). These new apparatuses help to minimize possible alterations from the exposure of the samples to air. The coordinated analysis involving these holders was successfully carried out without any sample damage or loss, thereby enabling us to obtain sufficient analytical datasets of textures, crystallography, elemental/isotopic abundances, and molecular functional groups for µm-sized minerals and organics in both the Antarctic micrometeorite and a carbonaceous chondrite. We will apply the coordinated analysis to acquire the complex characteristics in samples obtained by the future spacecraft sample return mission.

The Hayabusa2 and OSIRIS-REx missions have successfully returned pristine materials from the carbonaceous asteroids Ryugu and Bennu, respectively. These missions offer a unique opportunity to study space weathering processes, primarily driven by solar wind irradiation and micrometeorite bombardment, which continuously affect the surface of airless bodies. Coordinated surface and sub-surface techniques, including micro-infrared spectroscopy (micro-IR), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FE-SEM), and micro-Raman spectroscopy, have proven particularly valuable for unveiling the nature of these intricate processes. However, a sample holder specifically designed for extraterrestrial samples to facilitate coordinated surface analyses has yet to be reported. This study presents the development and application of a new sample holder (SH) and sample holder container (SHC), specifically designed to optimize the efficiency of coordinated surface analyses of extraterrestrial materials while preserving their integrity. The SH securely holds irregular millimeter-sized, high-friable grains (e.g., Ivuna-type carbonaceous chondrites) for sequential analyses such as micro-IR, XPS, FE-SEM, micro-Raman, and ion irradiation. The latter is critical for simulating space weathering processes. The SH was designed with high-purity materials, including molybdenum and alumina (Al 2 O 3 ), ensuring low chemical contamination risk and high-mechanical stability. The SHC complements this setup by providing a secure solution for transporting samples among different facilities. It allow to maintain an inert gas environment or high vacuum condition to prevent contamination from exposure to the terrestrial atmosphere. This combined system was successfully applied in the coordinated surface analysis of two Ryugu grains, preserving their chemical and physical integrity while facilitating detailed investigations into space weathering effects. These technical advancements provide a robust framework for multidisciplinary research on sensitive extraterrestrial materials, ensuring accurate and precise results and securing sample integrity throughout the coordinated analyses. Graphical Abstract

Steadily growing interest in magnetic characterization of organic compounds for therapeutic purposes or of other irregularly shaped specimens calls for refinements of experimental methodology to satisfy experimental challenges. Encapsulation in capsules remains the method of choice, but its applicability in precise magnetometry is limited. This is particularly true for minute specimens in the single milligram range as they are outweighed by the capsules and are subject to large alignment errors. We present here a completely new experimental methodology that permits 30-fold in situ reduction of the signal of capsules by substantially restoring the symmetry of the sample holder that is otherwise broken by the presence of the capsule. In practical terms it means that the standard 30 mg capsule is seen by the magnetometer as approximately a 1 mg object, effectively opening the window for precise magnetometry of single milligram specimens. The method is shown to work down to 1.8 K and in the whole range of the magnetic fields. The method is demonstrated and validated using the reciprocal space option of MPMS-SQUID magnetometers; however, it can be easily incorporated in any magnetometer that can accommodate straw sample holders (i.e., the VSM-SQUID). Importantly, the improved sensitivity is accomplished relying only on the standard accessories and data reduction method provided by the SQUID manufacturer, eliminating the need for elaborate raw data manipulations.

The Raman characterization of catalysts (as for any material) is generally a difficult task, since the numerous drawbacks affecting this technique, e.g. overlapping with photoemission phenomena and excitation induced sample damaging. These side effects are detrimental toward advanced applications of Raman spectroscopy, as in situ and/or operando ones. If photoemission can be often avoided by changing the excitation wavelength, the sample damaging requires to take advantage of specific tools, developed ad hoc. The aim of this work is to show the potentialities of a novel Raman setup, specifically designed for the in situ study of catalytic materials, where the sample is moved by means of a magnetic-driven sample-holder, reducing the excitation induced damaging to a negligible extent. Various examples related to catalysis field (involving inorganic, organic and mixed systems) are reported to support this statement.

A new method for variable temperature infrared spectroscopy studies of minerals is presented. A sample heating/cooling apparatus incorporating a modified button sample holder with thermoelectric temperature control is described. By employing different programs to heat and cool samples with temperatures varying in different ways, various aspects of mineral powders are investigated. Infrared spectroscopy methodologies for identifying sample structural changes as a function of temperature are described. The results obtained for a variety of minerals are provided as examples. The high precision and accuracy of this approach permit the detection of subtle crystallographic unit cell distortions as a function of temperature. A < 0.25% reduction in O-H stretching vibration band intensity associated with water desorption from a quartz sample is observed at 150 °C. By employing step temperature heating profiles, reversible and irreversible sample changes can be distinguished. Variable temperature infrared spectroscopy analyses demonstrate the utility of the technique for profiling sample dehydration processes and for elucidating interactions between mineral functionalities and absorbates as a function of temperature.

Serial crystallography (SX) technique using synchrotron X-ray allows the visualization of room-temperature crystal structures with low-dose data collection as well as time-resolved molecular dynamics. In an SX experiment, delivery of numerous crystals for X-ray interaction, in a serial manner, is very important. Fixed-target scanning approach has the advantage of dramatically minimizing sample consumption as well as any physical damage to crystal sample, compared to other sample delivery methods. Here, we introduce the simple approach of fixed-target serial synchrotron crystallography (FT-SSX) using nylon mesh and enclosed film (NAM)-based sample holder. The NAM-based sample holder consisted of X-ray-transparent nylon-mesh and polyimide film, attached to a magnetic base. This sample holder was mounted to a goniometer head on macromolecular crystallography beamline, and translated along vertical and horizontal directions for raster scanning by the goniometer. Diffraction data were collected in two raster scanning approaches: (i) 100 ms X-ray exposure and 0.011° oscillation at each scan point and (ii) 500 ms X-ray exposure and 0.222° oscillation at each scan point. Using this approach, we determined the room-temperature crystal structures of lysozyme and glucose isomerase at 1.5–2.0 Å resolution. The sample holder produced negligible X-ray background scattering for data processing. Therefore, the new approach provided an opportunity to perform FT-SSX with high accessibility using macromolecular crystallography beamlines at synchrotron without any special equipment.

The design features and applications of button sample holders are described. The similarities and contrasts between the button method and the transmission cell and attenuated total reflection techniques are discussed. Different button sample holder analysis methodologies are outlined, and examples are provided for mid-infrared spectroscopy measurements of solids, liquids, and pastes. Results obtained for 10-nonadecanone powder, a vitamin C tablet, a soil sample, and poly(methyl methacrylate) are used to illustrate different solid sample analysis approaches. Time-dependent spectrum variations detected during evaporation of a blood drop are elucidated and spectra obtained from different quantities of liquid chlorobenzene loaded into buttons and transmission cells are characterized. Infrared spectra derived from three toothpaste brands are compared and a sample perturbation study to identify temperature-dependent changes to the structure of poly(bisphenol A carbonate) is provided as an example of variable temperature infrared spectroscopy.

This study is dedicated to an in−depth analysis of the combustion characteristics of extruded polystyrene (XPS) as a building insulation material with the aim of accurately assessing its fire risk in the built environment. Innovatively, this research employed a cone calorimeter equipped with a self−designed insulating sample holder to conduct a systematic experimental study. Additionally, it performed a comprehensive analysis of the ignition characteristics, heat release rate, fire hazard, smoke release, and toxic gas emission of XPS materials. The experimental results revealed that the combustion behavior of XPS is influenced by multiple factors, including the content of flame retardants and external heat flux, which significantly affect the fire hazard of XPS. When the thermal radiation intensity escalates from 25 kW/m2 to 55 kW/m2, the peak heat release rate of XPS−B1 rises from 428 kW/m2 to 535 kW/m2, marking an increase of 25.00%. Conversely, the peak heat release rate of XPS−B2 surges from 348 kW/m2 to 579 kW/m2, reflecting a substantial increase of 66.38%. This research not only provides a solid theoretical foundation and detailed experimental data for the fire behavior of XPS materials but also holds significant practical importance for enhancing the fire safety of buildings. Overall, this research contributes to the scientific understanding of XPS insulation materials and supports the development of more effective fire prevention measures in construction.

PGAI-NT, a neutron-based element composition and structure analysis method, is well applicable to the non-destructive characterization of valuable artefacts, paleontological, bulk geological samples or to industrial reverse engineering. To set up the measurement geometry and scanning positions for items with unconstrained shapes, sizes, and matrices, accurate knowledge of the object’s geometry is a must. We applied portable structured-light 3D optical scanning or segmented neutron/X-ray tomography data to produce 3D meshes of the complex samples. Subsequently, 3D printing was used to fabricate detailed replicas of museum objects, as well as their gentle ad hoc sample holders, or produce custom parts of the Budapest PGAA instrument.

Light-sheet microscopy has emerged as the preferred means for high-throughput volumetric imaging of cleared tissues. However, there is a need for a flexible system that can address imaging applications with varied requirements in terms of resolution, sample size, tissue-clearing protocol, and transparent sample-holder material. Here, we present a ‘hybrid’ system that combines a unique non-orthogonal dual-objective and conventional (orthogonal) open-top light-sheet (OTLS) architecture for versatile multi-scale volumetric imaging. We demonstrate efficient screening and targeted sub-micrometer imaging of sparse axons within an intact, cleared mouse brain. The same system enables high-throughput automated imaging of multiple specimens, as spotlighted by a quantitative multi-scale analysis of brain metastases. Compared with existing academic and commercial light-sheet microscopy systems, our hybrid OTLS system provides a unique combination of versatility and performance necessary to satisfy the diverse requirements of a growing number of cleared-tissue imaging applications. A ‘hybrid’ open-top light-sheet microscope is described, which can be used for broad multi-scale volumetric imaging of one or more large tissues, cleared with diverse protocols, and conveniently mounted on an array of sample holders.