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At least 1,657 records · Page 92

Overall Traveling-Wave-Tube Efficiency Improved By Optimized Multistage Depressed Collector Design

Depressed Collector Design The microwave traveling wave tube (TWT) is used widely for space communications and high-power airborne transmitting sources. One of the most important features in designing a TWT is overall efficiency. Yet, overall TWT efficiency is strongly dependent on the efficiency of the electron beam collector, particularly for high values of collector efficiency. For these reasons, the NASA Glenn Research Center developed an optimization algorithm based on simulated annealing to quickly design highly efficient multistage depressed collectors (MDC's). Simulated annealing is a strategy for solving highly nonlinear combinatorial optimization problems. Its major advantage over other methods is its ability to avoid becoming trapped in local minima. Simulated annealing is based on an analogy to statistical thermodynamics, specifically the physical process of annealing: heating a material to a temperature that permits many atomic rearrangements and then cooling it carefully and slowly, until it freezes into a strong, minimum-energy crystalline structure. This minimum energy crystal corresponds to the optimal solution of a mathematical optimization problem. The TWT used as a baseline for optimization was the 32-GHz, 10-W, helical TWT developed for the Cassini mission to Saturn. The method of collector analysis and design used was a 2-1/2-dimensional computational procedure that employs two types of codes, a large signal analysis code and an electron trajectory code. The large signal analysis code produces the spatial, energetic, and temporal distributions of the spent beam entering the MDC. An electron trajectory code uses the resultant data to perform the actual collector analysis. The MDC was optimized for maximum MDC efficiency and minimum final kinetic energy of all collected electrons (to reduce heat transfer). The preceding figure shows the geometric and electrical configuration of an optimized collector with an efficiency of 93.8 percent. The results show the improvement in collector efficiency from 89.7 to 93.8 percent, resulting in an increase of three overall efficiency points. In addition, the time to design a highly efficient MDC was reduced from a month to a few days. All work was done in-house at Glenn for the High Rate Data Delivery Program. Future plans include optimizing the MDC and TWT interaction circuit in tandem to further improve overall TWT efficiency.

Vaden, Karl R.↗

Characterizing soil water content variability across spatial scales from optimized high-resolution distributed temperature sensing technique

Fiber-optic Distributed Temperature Sensing, when combined with the Single-probe Heat-pulse technique can measure soil moisture (θ) across spatial scales. The key limitation of this system is in obtaining the relationship between soil thermal conductivity (λ) and θ for a specific field. Using the Department of Energy Atmospheric Radiation Measurement (ARM) site, this study tested a new methodology to account for the spatial variability in the λ-θ relationship using a Gaussian processes model. The resulting accurate θ measurements (RMSE = 0.03 m 3 m –3 ) were used to characterize the spatial variability of θ across scales and to develop an empirical equation that can correct for the changes in the θ spatial variability observed at different spatial resolutions. In addition, the number of required samples to accurately characterize θ and its variability over scales ranging from 5 m and 350 m were estimated. Finally, these findings provide key information to scale soil moisture from centimeters to hundreds of meters for process understanding.

54 ENVIRONMENTAL SCIENCES↗

Theory of hydromagnetic turbulence

The present state of MHD turbulence theory as a possible solar wind research tool is surveyed. The theory is statistical, and does not make statements about individual events. The ensembles considered typically have individual realizations which differ qualitatively, unlike equilibrium statistical mechanics. Most of the theory deals with highly symmetric situations; most of these symmetries have yet to be tested in the solar wind. The applicability of MHD itself to solar wind parameters is highly questionable; yet it has no competitors, as a potentially comprehensive dynamical description. The purpose of solar wind research require sharper articulation. If they are to understand radial turbulent plasma flows from spheres, laboratory experiments and numerical solution of equations of motion may be cheap alternative to spacecraft. If "real life" information is demanded, multiple spacecraft with variable separation may be necessary to go further. The principal emphasis in the theory so far has been on spectral behavior for spatial covariances in wave number space. There is no respectable theory of these for highly anisotropic situations. A rather slow development of theory acts as a brake on justifiable measurement, at this point.

Montgomery, D.↗

Superclustering in the explosion scenario

A simple toy model is used to study the spatial distribution of rich clusters in a generic type of explosion scenario. The model, parameterized by the distribution of shell radii and the filling factor, places spherical shells at random and identifies each 'knot' as a cluster. The resulting cluster correlation function is close to a power law extending to the diameter of the largest spheres. Richer clusters form at the intersections of bigger shells and so have stronger correlations. Typical shell radii and filling factors are required to produce the observed number density of clusters. Models with a power-law radius distribution also reproduce the richness distribution of clusters in the Abell catalog. Supercluster multiplicity functions, void probabilities, number counts, topology statistics, and velocity correlations confirm the presence of strong superclustering and quantify the non-Gaussian nature of the model.

Weinberg, David H.↗

Data for Determining Spatially Varying Profit-Maximizing Management Practices for Miscanthus and Switchgrass Production in the Rainfed United States

The compiled datasets include county-level variables used for simulating miscanthus and switchgrass production in 2287 counties across the rainfed US including 5-year (2012-2016) averaged growing season degree days (GDD), 5-year (2012-2016) averaged growing season cumulative precipitation, National Commodity Crop Productivity Index (NCCPI) values, regional dummies (only for miscanthus), the regional-level random effect of the yield response function, N price, land cash rent, the first year fixed cost (only for switchgrass), and separate datasets for simulating an alternative model assuming a constant N rate. The GAMS codes are used to run the simulation to obtain the main results including the age-varying profit-maximizing N rate, biomass yields, and annual profits for miscanthus and switchgrass production across counties in the rainfed US. The STATA codes are used to merge and analyze simulation results and create summary statistics tables and key figures.

Age↗

Experimental investigation of multi-scale strain-field heterogeneity in rocks

Rocks have inherently heterogeneous micro-structures. The mechanical response of these heterogeneous micro-structures primarily governs the overall macroscopic behavior of intact rocks, as these features cause heterogeneity in the distribution of stress and strain within a rock volume. These attributes have generally been studied through numerical tools, but in this study, the stress-induced multi-scale spatial heterogeneity in the strain-field of three types of rocks was analyzed experimentally. The full-field non-contact strain measurement approach of 2D Digital Image Correlation (DIC) was employed for real-time evaluation of the progression of strain-field heterogeneity across the surface of the rock specimens when subjected to uniaxial compression. The results show that the strain-field heterogeneity is a characteristic of the inherent heterogeneity of the rock specimens, and that it amplifies with the magnitude of stress applied on the rock specimens. The changes in the strain-field heterogeneity with loading were consistent with established microcrack evolution processes in the rock specimens. The statistical fluctuation in the strain-field heterogeneity of the three rocks at varying gauge lengths (GL) was then analyzed for the determination of the Representative Volume Element (RVE) length-scale at increasing load levels. The evolution of the RVE length-scale with loading facilitates an objective way of determination of the stress at which the strain-field heterogeneity increases and begins to influence the overall global response of the material. The RVE length-scale variation with loading showed that at the RVE length-scale reaches the specimen-scale at load levels well below the peak strength.

2D-digital image correlation↗

NEON AOP Survey of Upper East River CO Watersheds: Waveform LiDAR Binary Data

The waveform Light Detection and Ranging (LiDAR) data in this package were generated through a National Ecological Observatory Network Airborne Observation Platform (NEON AOP) acquisition over watersheds of interest surrounding Crested Butte, Colorado. The remote sensing imagery acquired by the NEON AOP supports an interdisciplinary project on hydrology, biogeochemistry, and ecosystem functioning in a snow-dominated headwater environment. These waveform LiDAR data enable spatially continuous estimation of vegetation structure parameters to facilitate analyses of the major environmental drivers of structural and compositional variability. The package contains 97 compressed file archives in 7-zip (.7z) format, each corresponding to one acquisition flightpath. Within each .7z archive is a set of constituent files describing properties of the LiDAR waveforms, such as return intensity, geolocation, outgoing pulse and other behavior of the sensor and signals. Once downloaded, the files must first be unzipped using the widely distributed command-line software utility 7z, using the command '7z x \[filename\].7z \[target_directory\]'. All files within the .7z archives can be opened in IDL, MatLab, or the open-source R statistical computing environment. Further details about the data package are in the attached user guide (neon_aop_crbu_waveformlidar_userguide.pdf). This work was supported by the Watershed Function Science Focus Area at Lawrence Berkeley National Laboratory funded by the US Department of Energy, Office of Science, Biological and Environmental Research under Contract No. DE-AC02-05CH11231.

2018 NEON and 2025 CHESS Campaigns↗

High–Yield Deterministic Focused Ion Beam Implantation of Quantum Defects Enabled by In Situ Photoluminescence Feedback

Focused ion beam implantation is ideally suited for placing defect centers in wide bandgap semiconductors with nanometer spatial resolution. However, the fact that only a few percent of implanted defects can be activated to become efficient single photon emitters prevents this powerful capability to reach its full potential in photonic/electronic integration of quantum defects. Here an industry adaptive scalable technique is demonstrated to deterministically create single defects in commercial grade silicon carbide by performing repeated low ion number implantation and in situ photoluminescence evaluation after each round of implantation. An array of 9 single defects in 13 targeted locations is successfully created—a ≈70% yield which is more than an order of magnitude higher than achieved in a typical single pass ion implantation. The remaining emitters exhibit non-classical photon emission statistics corresponding to the existence of at most two emitters. This approach can be further integrated with other advanced techniques such as in situ annealing and cryogenic operations to extend to other material platforms for various quantum information technologies.

36 MATERIALS SCIENCE↗

Lidar Altimeter Measurements of Canopy Structure: Methods and Validation for Closed Canopy, Broadleaf Forests

Lidar altimeter observations of vegetated landscapes provide a time-resolved measure of laser pulse backscatter energy from canopy surfaces and the underlying ground. Airborne lidar altimeter data was acquired using the Scanning Lidar Imager of Canopies by Echo Recovery (SLICER) for a successional sequence of four, closed-canopy, deciduous forest stands in eastern Maryland. The four stands were selected so as to include a range of canopy structures of importance to forest ecosystem function, including variation in the height and roughness of the outer-most canopy surface and the vertical organization of canopy stories and gaps. The character of the SLICER backscatter signal is described and a method is developed that accounts for occlusion of the laser energy by canopy surfaces, transforming the backscatter signal to a canopy height profile (CHP) that quantitatively represents the relative vertical distribution of canopy surface area. The transformation applies an increased weighting to the backscatter amplitude as a function of closure through the canopy and assumes a horizontally random distribution of the canopy components. SLICER CHPs, averaged over areas of overlap where lidar ground tracks intersect, are shown to be highly reproducible. CHP transects across the four stands reveal spatial variations in vegetation, at the scale of the individual 10 m diameter laser footprints, within and between stands. Averaged SLICER CHPs are compared to analogous height profile results derived from ground-based sightings to plant intercepts measured on plots within the four stands. Tbe plots were located on the segments of the lidar ground tracks from which averaged SLICER CHPs were derived, and the ground observations were acquired within two weeks of the SLICER data acquisition to minimize temporal change. The differences in canopy structure between the four stands is similarly described by the SLICER and ground-based CHP results, however a Chi-square test of similarity documents differences that are statistically significant. The differences are discussed in terms of measurement properties that define the smoothness of the resulting CHPs and Lidar Altimeter Measurements of Canopy Structure - Harding et al. canopy properties that may vertically bias the CHP representations of canopy structure. The statistical differences are most likely due to the more noisy character of the ground-based CHPs, especially high in the canopy where ground-based sightings are rare resulting in an underestimate of canopy surface area and height, and to departures from the assumption of horizontal randomness which bias the CHPs toward the observer (upward for SLICER and downward for ground-based CHPs). The results demonstrate that the SLICER observations reliably provide a measure of canopy structure that reveals ecologically interesting structural variations such as those characterizing a successional sequence of closed-canopy, broadleaf forest stands.

Harding, D. J.↗

A SmallSat Concept to Resolve Diurnal and Vertical Variations of Aerosols, Clouds, and Boundary Layer Height

A SmallSat mission concept is formulated here to carry out Time-varying Optical Measurements of Clouds and Aerosol Transport (TOMCAT) from space while embracing low-cost opportunities enabled by the revolution in Earth science observation technologies. TOMCAT’s “around-the-clock” measurements will provide needed insights and strong synergy with existing Earth observation satellites to 1) statistically resolve diurnal and vertical variation of cirrus cloud properties (key to Earth’s radiation budget), 2) determine the impacts of regional and seasonal planetary boundary layer (PBL) diurnal variation on surface air quality and low-level cloud distributions, and 3) characterize smoke and dust emission processes impacting their long-range transport on the subseasonal to seasonal time scales. Clouds, aerosol particles, and the PBL play critical roles in Earth’s climate system at multiple spatiotemporal scales. Yet their vertical variations as a function of local time are poorly measured from space. Active sensors for profiling the atmosphere typically utilize sun-synchronous low-Earth orbits (LEO) with rather limited temporal and spatial coverage, inhibiting the characterization of spatiotemporal variability. Pairing compact active lidar and passive multiangle remote sensing technologies from an inclined LEO platform enables measurements of the diurnal and vertical variability of aerosols, clouds, and aerosol-mixing-layer (or PBL) height in tropical-to-midlatitude regions where most of the world’s population resides. TOMCAT is conceived to bring potential societal benefits by delivering its data products in near–real time and offering on-demand hazard-monitoring capabilities to profile fire injection of smoke particles, the frontal lofting of dust particles, and the eruptive rise of volcanic plumes.

John E. Yorks↗

Permafrost Carbon: Progress on Understanding Stocks and Fluxes Across Northern Terrestrial Ecosystems

Significant progress in permafrost carbon science made over the past decades include the identification of vast permafrost carbon stocks, the development of new pan-Arctic permafrost maps, an increase in terrestrial measurement sites for CO 2 and methane fluxes, and important factors affecting carbon cycling, including vegetation changes, periods of soil freezing and thawing, wildfire, and other disturbance events. Process-based modeling studies now include key elements of permafrost carbon cycling and advances in statistical modeling and inverse modeling enhance understanding of permafrost region C budgets. By combining existing data syntheses and model outputs, the permafrost region is likely a wetland methane source and small terrestrial ecosystem CO 2 sink with lower net CO 2 uptake toward higher latitudes, excluding wildfire emissions. For 2002–2014, the strongest CO2 sink was located in western Canada (median: -52 g C m -2 y -1 ) and smallest sinks in Alaska, Canadian tundra, and Siberian tundra (medians: -5 to -9 g C m -2 y -1 ). Eurasian regions had the largest median wetland methane fluxes (16–18 g CH4 m -2 y -1 ). Quantifying the regional scale carbon balance remains challenging because of high spatial and temporal variability and relatively low density of observations. More accurate permafrost region carbon fluxes require: (a) the development of better maps characterizing wetlands and dynamics of vegetation and disturbances, including abrupt permafrost thaw; (b) the establishment of new year-round CO 2 and methane flux sites in underrepresented areas; and (c) improved models that better represent important permafrost carbon cycle dynamics, including non-growing season emissions and disturbance effects.

54 ENVIRONMENTAL SCIENCES↗

Hierarchical off-diagonal low-rank approximation of Hessians in inverse problems, with application to ice sheet model initialization

Obtaining lightweight and accurate approximations of discretized objective functional Hessians in inverse problems governed by partial differential equations (PDEs) is essential to make both deterministic and Bayesian statistical large-scale inverse problems computationally tractable. The cubic computational complexity of dense linear algebraic tasks, such as Cholesky factorization, that provide a means to sample Gaussian distributions and determine solutions of Newton linear systems is a computational bottleneck at large-scale. These tasks can be reduced to log-linear complexity by utilizing hierarchical off-diagonal low-rank (HODLR) matrix approximations. In this work, we show that a class of Hessians that arise from inverse problems governed by PDEs are well approximated by the HODLR matrix format. In particular, we study inverse problems governed by PDEs that model the instantaneous viscous flow of ice sheets. In these problems, we seek a spatially distributed basal sliding parameter field such that the flow predicted by the ice sheet model is consistent with ice sheet surface velocity observations. Here, we demonstrate the use of HODLR Hessian approximation to efficiently sample the Laplace approximation of the posterior distribution with covariance further approximated by HODLR matrix compression. Computational studies are performed which illustrate ice sheet problem regimes for which the Gauss–Newton data-misfit Hessian is more efficiently approximated by the HODLR matrix format than the low-rank (LR) format. We then demonstrate that HODLR approximations can be favorable, when compared to global LR approximations, for large-scale problems by studying the data-misfit Hessian associated with inverse problems governed by the first-order Stokes flow model on the Humboldt glacier and Greenland ice sheet.

97 MATHEMATICS AND COMPUTING↗

A Compound Poisson Generator Approach to Point-source Inference in Astrophysics

Abstract The identification and description of point sources is one of the oldest problems in astronomy, yet even today the correct statistical treatment for point sources remains one of the field’s hardest problems. For dim or crowded sources, likelihood-based inference methods are required to estimate the uncertainty on the characteristics of the source population. In this work, a new parametric likelihood is constructed for this problem using compound Poisson generator (CPG) functionals that incorporate instrumental effects from first principles. We demonstrate that the CPG approach exhibits a number of advantages over non-Poissonian template fitting (NPTF)—an existing method—in a series of test scenarios in the context of X-ray astronomy. These demonstrations show that the effect of the point-spread function, effective area, and choice of point-source spatial distribution cannot, generally, be factorized as they are in NPTF, while the new CPG construction is validated in these scenarios. Separately, an examination of the diffuse-flux emission limit is used to show that most simple choices of priors on the standard parameterization of the population model can result in unexpected biases: when a model comprising both a point-source population and diffuse component is applied to this limit, nearly all observed flux will be assigned to either the population or to the diffuse component. A new parameterization is presented for these priors that properly estimates the uncertainties in this limit. In this choice of priors, CPG correctly identifies that the fraction of flux assigned to the population model cannot be constrained by the data.

79 ASTRONOMY AND ASTROPHYSICS↗

Evaluation of global terrestrial evapotranspiration using state-of-the-art approaches in remote sensing, machine learning and land surface modeling

Abstract. Evapotranspiration (ET) is critical in linking global water, carbon and energy cycles. However, direct measurement of global terrestrial ET is not feasible. Here, we first reviewed the basic theory and state-of-the-art approaches for estimating global terrestrial ET, including remote-sensing-based physical models, machine-learning algorithms and land surface models (LSMs). We then utilized 4 remote-sensing-based physical models, 2 machine-learning algorithms and 14 LSMs to analyze the spatial and temporal variations in global terrestrial ET. The results showed that the ensemble means of annual global terrestrial ET estimated by these three categories of approaches agreed well, with values ranging from 589.6 mm yr-1 (6.56×104 km3 yr-1) to 617.1 mm yr-1 (6.87×10 4 km3 yr -1 ). For the period from 1982 to 2011, both the ensembles of remote-sensing-based physical models and machine-learning algorithms suggested increasing trends in global terrestrial ET (0.62 mm yr -2 with a significance level of p<0.05 and 0.38 mm yr -2 with a significance level of p<0.05, respectively). In contrast, the ensemble mean of the LSMs showed no statistically significant change (0.23 mm yr -2 , p>0.05), although many of the individual LSMs reproduced an increasing trend. Nevertheless, all 20 models used in this study showed that anthropogenic Earth greening had a positive role in increasing terrestrial ET. The concurrent small interannual variability, i.e., relative stability, found in all estimates of global terrestrial ET, suggests that a potential planetary boundary exists in regulating global terrestrial ET, with the value of this boundary being around 600 mm yr -1 . Uncertainties among approaches were identified in specific regions, particularly in the Amazon Basin and arid/semiarid regions. Improvements in parameterizing water stress and canopy dynamics, the utilization of new available satellite retrievals and deep-learning methods, and model–data fusion will advance our predictive understanding of global terrestrial ET.

58 GEOSCIENCES↗

The agglomeration and dispersion dichotomy of human settlements on Earth

Human settlements on Earth are scattered in a multitude of shapes, sizes and spatial arrangements. These patterns are often not random but a result of complex geographical, cultural, economic and historical processes that have profound human and ecological impacts. However, little is known about the global distribution of these patterns and the spatial forces that creates them. This study analyses human settlements from high-resolution satellite imagery and provides a global classification of spatial patterns. We find two emerging classes, namely agglomeration and dispersion. In the former, settlements are fewer than expected based on the predictions of scaling theory, while an unexpectedly high number of settlements characterizes the latter. To explain the observed spatial patterns, we propose a model that combines two agglomeration forces and simulates human settlements’ historical growth. Our results show that our model accurately matches the observed global classification (F1: 0.73), helps to understand and estimate the growth of human settlements and, in turn, the distribution and physical dynamics of all human settlements on Earth, from small villages to cities.

54 ENVIRONMENTAL SCIENCES↗

Intentional Uranium Tagging for Material Provenance and Pathway Forensics (LA19-Intentional-Forensics-NDD3Bb) (Annual Report for FY21)

This report describes the outcomes of the third and final year of a project to research the feasibility of tagging uranium materials, especially nuclear fuels. The experimental focus remained on metallic uranium forms under prospective surface and bulk tagging scenarios. Overall, the results showed that the tags could be successfully imparted and characterized in both as-built and degraded conditions. This was in line with expectations coming into this project, indicating promise for both surface and bulk tagging of metallic forms of uranium. Multiple surface tagging techniques and detection strategies were explored in FY21, with an emphasis on improving tag quality, readability, and detection in the field. Non-radioactive materials were used as a testbed. Selective deposition via laser beam was determined to be successful in imparting a readable titanium deposit on a stainless steel base plate, and can be read with high resolution characterization techniques (e.g., scanning electron microscopy) and field capable tools (e.g., eddy current testing). Other deposition techniques, such as selective deposition via electron beam and photoluminescent tags, were explored in FY21, and while success for these techniques would be dependent on additional work, these techniques showed potential for surface tagging applications. To survey bulk taggant elements for bulk uranium metal, 16 tagging elements were spread among 18 depleted uranium castings (4 baseline, 3 mix, 1 dilution, and 10 recycle). Most of these were made and characterized in FY21. Taggant acceptability was based upon manufacturability, detectability, and persistence from the standpoint of two detection options: bulk chemical analysis (for “chemical taggants”) and microstructural analysis (for “second phase taggants”). Taggant detection in both up-front manufacturing and in the face of “degradations” such as dilution, mixing, and recycling was generally good. Two independent laboratories carried out chemical analysis on most of the castings, and often at several locations within a casting, and the results are discussed. Scanning electron microscopy+EDS microanalysis revealed the second phases mostly contained the expected tagging elements. The shapes and 2 spatial distributions of these micron-sized carbides, oxides, and intermetallic particles offers opportunities for further science-based investigation and tagging optimization. Overall, V and Co currently appear as the best choices for chemical taggants while Al, Ti, Mn, Co, Pd, and Tb all look good as second phase taggants. The other elements considered here – Sc, Ni, Ge, Nb, Ce, Ta, W, Ir, and Au – while not being ruled out, require more study to become viable options. It is of special note that in the recycling study only one of the 12 elements fell out of detection even after 10 meltings, demonstrating their persistence. An Appendix tabulates all chemical analysis results to enable more quantitative and statistical studies of detection opportunities and limitations, as a part of a related project.

36 MATERIALS SCIENCE↗

Assessment of Extremes in Global Precipitation Products: How Reliable Are They?

Global gridded precipitation products have proven essential for many applications ranging from hydrological modeling and climate model validation to natural hazard risk assessment. They provide a global picture of how precipitation varies across time and space, specifically in regions where ground-based observations are scarce. While the application of global precipitation products has become widespread, there is limited knowledge on how well these products represent the magnitude and frequency of extreme precipitation—the key features in triggering flood hazards. Here, five global precipitation datasets (MSWEP, CFSR, CPC, PERSIANN-CDR, and WFDEI) are compared to each other and to surface observations. The spatial variability of relatively high precipitation events (tail heaviness) and the resulting discrepancy among datasets in the predicted precipitation return levels were evaluated for the time period 1979–2017. The analysis shows that 1) these products do not provide a consistent representation of the behavior of extremes as quantified by the tail heaviness, 2) there is strong spatial variability in the tail index, 3) the spatial patterns of the tail heaviness generally match the Köppen–Geiger climate classification, and 4) the predicted return levels for 100 and 1000 years differ significantly among the gridded products. More generally, our findings reveal shortcomings of global precipitation products in representing extremes and highlight that there is no single global product that performs best for all regions and climates.

Risk assessment↗

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↗