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Results for “micro-XRF”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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9 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Sulphur variations in annually layered stalagmites using benchtop micro-XRF

Variation of sulphur in annually laminated stalagmites can be used to infer the impact of past volcanic activities, anthropogenic pollution, and climate change due to increased bushfire activity. The synchrotron radiation micro-X-Ray fluorescence (SR-XRF) microprobe is a powerful tool to analyse and image sulphur recorded in stalagmites with micrometre resolution. However, access to SR-XRF beamlines can be limited, so researchers must select the most promising stalagmites for imaging. Benchtop micro-XRF is an effective tool for trace elemental analysis of speleothem samples and is a candidate for routine laboratory measurement of sulphur along stalagmite laminae and screening for SR-XRF. Here, this study describes a protocol using matrix-matched standards to measure annual variations of sulphur at trace to percent level along the laminae of two Western Australian stalagmites, one of which already having been analysed using SR-XRF. Parameters that affected quantitation include X-ray tube voltage and current, spot size of the X-ray beam and stalagmite surface roughness and porosity. The use of a 20 μm X-ray spot size provides sub-annual spatial resolution that can be completed in an overnight scan. The features in a 1000 point micro-XRF analysis of sulphur along a 20 mm transect show good consistency with SR-XRF microprobe data. Micro-XRF mapping was also performed to produce chemical images on the stalagmite and compared with Raman and X-ray diffraction (XRD) to confirm that the stalagmite is exclusively calcite, with no aragonite, and that the source of sulphur in the samples was gypsum and anhydrite. Regions of very high sulphur in the micro-XRF maps were found to be artefacts due to diffraction of the incident beam but these could be efficiently removed by using a multiple point statistics approach to produce a clean image suitable for analysis of the laminae. This work shows the potential of micro-XRF for routine analysis of sulphur in stalagmites, and to streamline sample characterisation before SR-XRF imaging.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Micro-XRF mapping and quantitative assessment of Cd in rice ( Oryza sativa L.) roots

Understanding Cd uptake and distribution in rice roots is important for breeding varieties that do not accumulate Cd in the grain to any large extent. Here, we examined the physiological and molecular factors responsible for Cd uptake and transport differences between two japonica rice cultivars prescreened as high (zhefu7) or low (Xiangzaoxian45) accumulators of Cd in the grain. No significant differences in Cd uptake between the two cultivars were observed; however, Xiangzaoxian45 retained most of the absorbed Cd in the roots, whereas zhefu7 showed higher transport of Cd from the root to the shoot, regardless of the duration of exposure to Cd. The inability to sequester Cd into root vacuoles caused high accumulation of Cd in the grain in zhefu7, whereas inefficient transport of Cd from roots to shoots in Xiangzaoxian45 caused low accumulation of Cd in the grain. Cd sequestration in the roots and transport from the root to the shoot were greatly influenced by the expression patterns of transport-related genes OsHMA3 and OsHMA2, respectively. Further, micro-X-ray fluorescence spectroscopy mapping confirmed that more Cd was sequestered in the roots of Xiangzaoxian45 than in those of zhefu7, with a significant amount of Cd localized in the root hairs, as well as in the meristematic and elongation zones, and dermal and stele tissues. Finally, we propose that effective Cd sequestration in root vacuoles was the major determinant of divergent Cd-accumulation patterns in the two rice cultivars under study.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Using micro-XRF to characterize chloride ingress through cold joints in 3D printed concrete

Digital fabrication methods with concrete have been rapidly developing, with many problems related to component production and material control being solved in recent years. These processes produce inherently layered cementitious components that are anisotropic, and in many cases, produces a weak interface between layers, which are generally referred to as cold joints. While material strength at these interfaces has been well studied in recent years, durability has received less attention, even though cold joints can function as channels for aggressive agents, such as chlorides. This work presents a method using micro-X-ray fluorescence (μXRF) to image chloride ingress into layer interfaces of 3D printed fine-grained concrete specimens produced with varying layer deposition time intervals, and also compares it to neutron imaging of moisture uptake. The results show that cold joints formed after a 1 day time interval are highly susceptible to chloride ingress, and that curing conditions play a major role in how quickly interfacial transport can take place. The μXRF method is also shown to be useful for study of transport of chlorides in cold joints, due to its spatial resolution and direct analysis of an aggressive species of interest.

36 MATERIALS SCIENCE↗
DOE OSTI2023

The evolution of soil microstructure and micromineralogy along a soil age gradient on the Galápagos Islands (Ecuador)

The islands of the Galápagos archipelago are of different ages due to the combination of a geostationary volcanic hotspot and the eastward movement of the Nazca tectonic plate. Taking advantage of this, a soil chronosequence (1.5–1070 ka) has recently been established covering four of the islands. This was used to investigate the temporal development of soil microstructure and micromineralogy using micromorphological methods in combination with synchrotron-based mineralogical and geochemical microanalyses. Along the chronosequence, the microstructure changed from intergrain microaggregates in the young soils to angular blocky microaggregates in the older soils. In the young soils, a high amount of vitric scoria and weatherable minerals occur, but they quickly disappear with age, and micromass increased fast. The micromorphological studies as well as micro-XRD and micro-XRF revealed increasing heterogeneity of soil microstructure and micromineralogy due to weathering and pedogenic processes until intermediate soil age. In the oldest soils, the microstructure became more uniform again, de-mixing pedofeatures like clay coatings have completely disappeared, and kaolinite, hematite and gibbsite dominate the mineralogical composition. Our study shows that the development of soil microstructure mirrors macroscopic soil profile development showing increasing differentiation until intermediate developmental stages and receding heterogeneity in highly weathered soils.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2020

Recent Advances in Nuclear Forensic Chemistry

Nuclear forensics is a rapidly growing field with a widespread impact on global nonproliferation. From the beginning, nuclear forensic capabilities have been inextricably bound to existing limitations within chemistry and materials science. As nuclear forensics has continued to develop as a unique field of research, new advances in chemistry have revolutionized our ability to rapidly and quantitatively analyze radioactive materials for attribution. In particular, microanalytical techniques originally developed for nanoscience, such as micro-XRF, SIMS, and SEM-EDX, have enabled spatially resolved chemical analyses to be performed with only nanograms of material. Such techniques have redefined the paradigm for pre- and postdetonation nuclear forensics, as large quantities of material are no longer necessary for full characterization and attribution. This Review explains how modern nuclear forensic techniques have developed from their origins in chemistry and provides real-world examples of how these techniques have been used to characterize radioactive materials, including fallout from nuclear detonations such as the 1945 Trinity test.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2022

Distribution of Mn Oxidation States in Grassland Soils and Their Relationships with Soil Pores

Manganese (Mn) is known to be an active contributor to processing and cycling of soil organic carbon (C), yet the exact mechanisms behind its interactions with C are poorly understood. Plant diversity in terrestrial ecosystems drives feedback links between plant C inputs and soil pores, where the latter, in turn, impact the redox environment and Mn. This study examined associations between soil pores (>36 μm Ø) and Mn within intact soils from two grassland ecosystems, after their >6-year implementation in a replicated field experiment. In this work, we used μ-XRF imaging and XANES spectroscopy to explore spatial distribution patterns of Mn oxidation states, combined with X-ray computed microtomography and 2D zymography. A high plant diversity system (restored prairie) increased soil C and modified spatial distribution patterns of soil pores as compared to a single species system (monoculture switchgrass). In switchgrass, the abundance of oxidized and reduced Mn oxidation states varied with distance from pores consistently with anticipated O 2 diffusion, while in the soil from restored prairie, the spatial patterns suggested that biological activity played a greater role in influencing Mn distributions. Based on the findings, we propose a hypothesis that Mn transformations promote C gains in soils of high plant diversity grasslands.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

Chemical state mapping of simulant Chernobyl lava-like fuel containing material using micro-focused synchrotron X-ray spectroscopy

Uranium speciation and redox behaviour is of critical importance in the nuclear fuel cycle. X-ray absorption near-edge spectroscopy (XANES) is commonly used to probe the oxidation state and speciation of uranium, and other elements, at the macroscopic and microscopic scale, within nuclear materials. Two-dimensional (2D) speciation maps, derived from microfocus X-ray fluorescence and XANES data, provide essential information on the spatial variation and gradients of the oxidation state of redox active elements such as uranium. In the present work, we elaborate and evaluate approaches to the construction of 2D speciation maps, in an effort to maximize sensitivity to the U oxidation state at the U L 3 -edge, applied to a suite of synthetic Chernobyl lava specimens. Our analysis shows that calibration of speciation maps can be improved by determination of the normalized X-ray absorption at excitation energies selected to maximize oxidation state contrast. The maps are calibrated to the normalized absorption of U L 3 XANES spectra of relevant reference compounds, modelled using a combination of arctangent and pseudo-Voigt functions (to represent the photoelectric absorption and multiple-scattering contributions). We validate this approach by microfocus X-ray diffraction and XANES analysis of points of interest, which afford average U oxidation states in excellent agreement with those estimated from the chemical state maps. This simple and easy-to-implement approach is general and transferrable, and will assist in the future analysis of real lava-like fuel-containing materials to understand their environmental degradation, which is a source of radioactive dust production within the Chernobyl shelter.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Major to trace element imaging and analysis of iron age glasses using stage scanning in the analytical dual beam microscope (tandem)

Dark and clear silicate glasses formed during an iron age vitrification event ≈ 1500 years ago at the Broborg hillfort near Uppsala, Sweden have been analyzed using a scanning electron microscope equipped with a micro-X-ray fluorescence (μXRF) spectrometer. Correlated µXRF and electron beam-induced energy dispersive spectrometry (EDS) X-ray maps were collected via stage-scanning at constant velocity. This coupled procedure represents a new approach for the cultural heritage community to conduct analytical studies of archaeometric specimens composed of metal, ceramic, or mixed inorganic/organic materials, where major and trace element compositions are registered in space for areas up to the centimeter-length scale at micrometer-scale resolution. Overview images were used to select areas for EDS beam scan maps correlated with multispectral cathodoluminescence (CL) imaging and co-located quantitative EDS and μXRF point analysis. Fe, Ca, Mg, Ti, P, Mn, Zr, Zn, and Y are enriched in the dark glass, while Si, Al, K, Na, Ba, Sr, Rb, and Ga are enriched in the clear glass. Unmelted material is comprised predominately of quartz (SiO 2 ) along with trace apatite (Ca 5 (PO 4 ) 3 [Cl,OH]) and zircon (ZrSiO 4 ). Multivariate statistical analysis was used to measure the area fractions of high variance components while lower variance components represented phase mixtures. Differences between calculated melt viscosities for the glass compositions are consistent with field and laboratory observations. Coupled large area EDS and μXRF imaging shows significant promise for informed selection of higher spatial resolution and higher sensitivity follow-up studies, e.g., those performed using synchrotron analysis.

36 MATERIALS SCIENCE↗