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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Reconciling Chord Length Distributions and Area Distributions for Fields of Fractal Cumulus Clouds

While the total cover of broken cloud fields can in principle be obtained from one-dimensional measurements, the cloud size distribution normally differs between two-dimensional (area) and one-dimensional retrieval (chord length) methods. In this study, we use output from high-resolution Large Eddy Simulations to generate a transfer function between the two. We retrieve chord lengths and areas for many clouds, and plot the one as a function of the other, and vice versa. We find that the cloud area distribution conditional on the chord length behaves like a gamma distribution with well-behaved parameters, with a mean μ=1.1L and a shape parameter β=L−0.645. Using this information, we are able to generate a transfer function that can adjust the chord length distribution so that it comes much closer to the cloud area distribution. Our transfer function improves the error in predicting the mean cloud size, and is performs without strong biases for smaller sample sizes. However, we find that the method is still has difficulties in accurately predicting the frequency of occurrence of the largest cloud sizes.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2023

Determining the tensile strength of fuel surrogate TRISO-coated particle buffer, IPyC, and buffer-IPyC interlayer regions

A novel micro tensile sample fabrication technique for determining the tensile strength of the buffer, IPyC, and buffer -IPyC interlayer regions of surrogate (ZrO2) TRISO fuel particle layers was refined and implemented. Copper micro tensile samples served as baseline materials to verify the methods used. Tensile tests performed in this study, while limited in number, were analyzed using standard and Weibull statistics. As expected, the buffer layer was weakest, with an average ultimate tensile strength of 138.70 MPa, and the IPyC layer samples, were strongest, with an average ultimate tensile strength of 189.74 MPa. In the buffer -IPyC interface samples, all breaks occurred in the buffer region, though the average ultimate tensile strength of the samples, 159.80 MPa, was between the pure buffer and IPyC samples. These results suggest the interlayer region has unique properties, perhaps associated with pyrocarbon infiltration into the buffer layer during particle coating. All interlayer samples fractured within the buffer side; however, the stress strain behavior of some of these samples resembled the behavior of the IPyC layer samples. Here, the buffer and IPyC layer strengths had a normal distribution under Weibull analysis, while the interlayer region had a Rayleigh distribution. Further testing is needed to clarify both the standard and Weibull statistical results

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2023

The rapid-tome, a 3D-printed microtome, and an updated hand-sectioning method for high-quality plant sectioning

Abstract Background Microscopic analysis of plant anatomy is a common procedure in biology to study structure and function that requires high-quality sections for accurate measurements. Hand sectioning of specimens is typically limited to moderately soft tissue while harder samples prohibit sectioning by hand and/or result in inconsistent thicknesses. Results Here we present both a clearly described hand-sectioning method and a novel microtome design that together provide the means to section a variety of plant sample types. The described hand-sectioning method for herbaceous stems works well for softer subjects but is less suitable for samples with secondary growth (e.g., wood production). Instead, the “Rapid-Tome” is a novel tool for sectioning both soft and tougher high-aspect-ratio samples, such as stems and roots, with excellent sample control. The Rapid-Tome can be 3D-printed in approximately 18 h on a mid-quality printer common at university maker spaces. After printing and trimming, Rapid-Tome assembly takes a few minutes with five metal parts common at hardware stores. Users sectioned a variety of plant samples including the hollow internodes of switchgrass ( Panicum virgatum ), fibrous switchgrass roots containing aerenchyma, and woody branches of eastern red cedar ( Juniperus virginiana ) and American sycamore ( Platanus occidentalis ). A comparative analyses with Rapid-Tome-produced sections readily revealed a significant difference in seasonal growth of sycamore xylem vessel area in spring (49%) vs. summer (23%). Additionally, high school students with no prior experience produced sections with the Rapid-Tome adequate for comparative analyses of various plant samples in less than an hour. Conclusions The described hand-sectioning method is suitable for softer tissues, including hollow-stemmed grasses and similar samples. In addition, the Rapid-Tome provides capacity to safely produce high-quality sections of tougher plant materials at a fraction of the cost of traditional microtomes combined with excellent sample control. The Rapid-Tome features rapid sectioning, sample advancement, blade changes, and sample changes; it is highly portable and can be used easily with minimal training making production of thin sections accessible for classroom and outreach use, in addition to research.

3D-printing↗
DOE OSTI2024

Using Convex Optimization to Efficiently Apportion Tracer and Pollutant Sources From Point Concentration Observations

Abstract Rivers transport elements, minerals, chemicals, and pollutants produced in their upstream basins. A sample from a river is a mixture of all of its upstream sources, making it challenging to pinpoint the contribution from each individual source. Here, we show how a nested sample design and convex optimization can be used to efficiently unmix downstream samples of a well‐mixed, conservative tracer in a steady state system into the contributions of their upstream sources. Our approach is significantly faster than previous methods. We represent the river's sub‐catchments, defined by sampling sites, using a directed acyclic graph. This graph is used to build a convex optimization problem which, thanks to its convexity, can be quickly solved to global optimality—in under a second on desktop hardware for data sets of ∼100 samples or fewer. Uncertainties in the upstream predictions can be generated using Monte Carlo resampling. We provide an open‐source implementation of this approach in Python. The inputs required are straightforward: a table containing sample locations and observed tracer concentrations, along with a D8 flow‐direction raster map. As a case study, we use this method to map the elemental geochemistry of sediment sources for rivers draining the Cairngorms mountains, UK. This method could be extended to non‐conservative and non‐steady state tracers. We also show, theoretically, how multiple tracers could be simultaneously inverted to recover upstream run‐off or erosion rates as well as source concentrations. Overall, this approach can provide valuable insights to researchers in various fields, including water quality, geochemical exploration, geochemistry, hydrology, and wastewater epidemiology.

Barnes, Richard↗
DOE OSTI2021

Comparison of methodologies used to determine aromatic lignin unit ratios in lignocellulosic biomass

Abstract Background Multiple analytical methods have been developed to determine the ratios of aromatic lignin units, particularly the syringyl/guaiacyl (S/G) ratio, of lignin biopolymers in plant cell walls. Chemical degradation methods such as thioacidolysis produce aromatic lignin units that are released from certain linkages and may induce chemical changes rendering it difficult to distinguish and determine the source of specific aromatic lignin units released, as is the case with nitrobenzene oxidation methodology. NMR methods provide powerful tools used to analyze cell walls for lignin composition and linkage information. Pyrolysis-mass spectrometry methods are also widely used, particularly as high-throughput methodologies. However, the different techniques used to analyze aromatic lignin unit ratios frequently yield different results within and across particular studies, making it difficult to interpret and compare results. This also makes it difficult to obtain meaningful insights relating these measurements to other characteristics of plant cell walls that may impact biomass sustainability and conversion metrics for the production of bio-derived fuels and chemicals. Results The authors compared the S/G lignin unit ratios obtained from thioacidolysis, pyrolysis-molecular beam mass spectrometry (py-MBMS), HSQC liquid-state NMR and solid-state (ss) NMR methodologies of pine, several genotypes of poplar, and corn stover biomass. An underutilized approach to deconvolute ssNMR spectra was implemented to derive S/G ratios. The S/G ratios obtained for the samples did not agree across the different methods, but trends were similar with the most agreement among the py-MBMS, HSQC NMR and deconvoluted ssNMR methods. The relationship between S/G, thioacidolysis yields, and linkage analysis determined by HSQC is also addressed. Conclusions This work demonstrates that different methods using chemical, thermal, and non-destructive NMR techniques to determine native lignin S/G ratios in plant cell walls may yield different results depending on species and linkage abundances. Spectral deconvolution can be applied to many hardwoods with lignin dominated by S and G units, but the results may not be reliable for some woody and grassy species of more diverse lignin composition. HSQC may be a better method for analyzing lignin in those species given the wealth of information provided on additional aromatic moieties and bond linkages. Additionally, trends or correlations in lignin characteristics such as S/G ratios and lignin linkages within the same species such as poplar may not necessarily exhibit the same trends or correlations made across different biomass types. Careful consideration is required when choosing a method to measure S/G ratios and the benefits and shortcomings of each method discussed here are summarized.

09 BIOMASS FUELS↗
DOE OSTI2023

Radiocarbon analysis of soil microbial biomass via direct chloroform extraction

Microbial processing of soil organic matter is a significant driver of C cycling, yet we lack an understanding of what shapes the turnover of this large terrestrial pool. In part, this is due to limited options for accurately identifying the source of C assimilated by microbial communities. Laboratory incubations are the most common method for this; however, they can introduce artifacts due to sample disruption and processing and can take months to produce sufficient CO 2 for analysis. We present a biomass extraction method which allows for the direct 14 C analysis of microbial biomolecules and compare the results to laboratory incubations. In the upper 50 cm soil depths, the Δ 14 C from incubations was indistinguishable from that of extracted microbial biomass. Below 50 cm, the Δ 14 C of the biomass was more depleted than that of the incubations, either due to the stimulation of labile C decomposition in the incubations, the inclusion of biomolecules from non-living cells in the biomass extractions, or differences in C used for assimilation versus respiration. Our results suggest that measurement of Δ 14 C of microbial biomass extracts can be a useful alternative to soil incubations.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2021

A prediction interval method for uncertainty quantification of regression models

This paper considers calculation of prediction intervals (PIs) by neural networks (NNs) for quantifying uncertainty in regression tasks, so as to provide fast, accurate and robust emulators to accelerate scientific simulations. We propose a novel method to learn lower and upper bounds of the PI using independent NNs without defining an exclusive loss. Our method requires no distributional assumption, does not introduce extra hyper-parameters, and can effectively identify out-of-distribution samples and quantify their uncertainty. We demonstrate advantages of our method using a benchmark problem and two real-world scientific applications.

Zhang, Pei↗
DOE OSTI2024

Reduced-dimension Bayesian optimization for model calibration of transient vapor compression cycles

Development and calibration of first-principles dynamic models of vapor compression cycles (VCCs) is of critical importance for applications that include control design and fault detection and diagnostics. Nevertheless, the inherent complexity of models that are represented by large systems of differential–algebraic equations leads to significant challenges for model calibration processes that utilize classical gradient-based methods. Bayesian optimization (BO) is a sample-efficient and gradient-free approach using a probabilistic surrogate model and optimal search over a feasible parameter space. Despite the benefits of BO in reducing computational costs, challenges remain in dealing with a high-dimensional calibration task resulting from a large set of parameters that have significant impacts on system behavior and need to be calibrated simultaneously. This paper presents a reduced-dimension BO framework for calibrating transient VCCs models where the calibration space is projected to a low-dimensional subspace for accelerating convergence of the solution algorithm and consequently reducing the number of transient simulations. The proposed approach was demonstrated via two case studies associated with different VCC applications where 10 parameters were calibrated in each case using laboratory measurements. The reduced-dimension BO framework only required 1 / 8 th of the iterations associated with a standard BO method that deals with high-dimensional calibration parameters for converged solutions and yielded comparable accuracy. Furthermore, both calibrated models revealed significant accuracy improvements compared to uncalibrated models.

Ma, Jiacheng↗
DOE OSTI2026

Critical Review of Brazil Disk Techniques for Tensile Strength Characterization With an Emphasis on High Explosive Materials

Mechanical properties are a critical performance metric for many high explosive (HE) materials and tensile strength properties are particularly important. Direct tensile measurements using dogbone shaped samples are the gold standard but they have the disadvantage that they are fairly large and require samples machined from billets. Diametral compression, more commonly known as Brazil disk (BD) testing, is an indirect method for measuring tensile strength on smaller and more easily fabricated samples. A review of the BD literature is presented with an emphasis on tensile strength measurements in high explosive materials. BD literature is reviewed in three primary areas: (i) rocks and concrete, (ii) pharmaceutical materials, and (iii) high explosive materials. The literature for rocks/concrete is extensive and dates back over 80 years; despite this there is no consensus on the validity/accuracy of the BD technique or the optimal variant of the BD technique to employ. The pharmaceutical literature is the opposite, being limited in scope and quantity of studies. BD literature on high explosive materials falls in between, not as impressive as in the rocks/concrete community but more substantiative than in the pharmaceutical community. After the review of the literature practical parameters for HE BD testing and recommended future work is discussed.

Brazil disk↗
DOE OSTI2021

Resonant x-ray scattering method for measuring cation stoichiometry in BaSnO 3 thin films

In this study, we develop a resonant scattering technique to measure cation stoichiometry of lanthanum-doped BaSnO 3 (BSO) thin films on a DyScO 3 substrate. Samples are grown by a hybrid molecular beam epitaxy method and display high room-temperature carrier mobilities. The measured thin films are grown with widely differing cation arrival rates, with Ba being evaporated from an elemental source and Sn from a SnO 2 source. Differences in mobilities in these films may arise from differences in Ba/Sn cation stoichiometry. Owing to the similar scattering strength of the Ba and Sn cations, odd-order Bragg peaks of BSO are particularly sensitive to the material's cation stoichiometry, i.e., the Ba/Sn ratio. Sensitivity to cation stoichiometry is further enhanced using the technique of resonant x-ray scattering, which changes the scattering strength of a single element across the Ba L absorption edges. We determine that the Ba/Sn cation stoichiometry varies from unity by less than 1% for films of mobility ranging from 84.8 to 144 cm 2 /(V s) and conclude that the mobility of these films scales with film thickness and growth rate rather than stoichiometry.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Growth phase estimation for abundant bacterial populations sampled longitudinally from human stool metagenomes

Longitudinal sampling of the stool has yielded important insights into the ecological dynamics of the human gut microbiome. However, human stool samples are available approximately once per day, while commensal population doubling times are likely on the order of minutes-to-hours. Despite this mismatch in timescales, much of the prior work on human gut microbiome time series modeling has assumed that day-to-day fluctuations in taxon abundances are related to population growth or death rates, which is likely not the case. Here, we propose an alternative model of the human gut as a stationary system, where population dynamics occur internally and the bacterial population sizes measured in a bolus of stool represent a steady-state endpoint of these dynamics. We formalize this idea as stochastic logistic growth. We show how this model provides a path toward estimating the growth phases of gut bacterial populations in situ. We validate our model predictions using an in vitro Escherichia coli growth experiment. Finally, we show how this method can be applied to densely-sampled human stool metagenomic time series data. We discuss how these growth phase estimates may be used to better inform metabolic modeling in flow-through ecosystems, like animal guts or industrial bioreactors.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2021

Specialized diamond materials for NMR applications

Polarizable diamond materials and methods for obtaining nuclear magnetic resonance spectra of samples external to the diamond materials are described. The diamond materials can include 12C, 13C, substitutional nitrogen, and nitrogen vacancy defects in a crystalline lattice, wherein the substitutional nitrogen concentration is between 10 ppm and 200 ppm, the nitrogen vacancy concentration is between 10 ppb and 10 ppm, and the 13C concentration is greater than 1.1% and not more than 25%. Methods for obtaining nuclear magnetic resonance spectra can include optically pumping a diamond material to generate electron spin hyperpolarization in nitrogen vacancy centers, transferring the electron spin hyperpolarization to nuclei of the sample, and generating a nuclear magnetic resonance spectrum by applying a magnetic field to the sample, exciting the sample with a radio frequency pulse, and detecting a nuclear magnetic resonance response from the sample.

Parker, Alfred↗
DOE OSTI2024

Pressure-Induced Superconductivity In Polycrystalline La 3 Ni 2 O 7 − δ

We synthesized polycrystalline La 3 Ni 2 O 7 − δ ( δ ≈ 0.0 7 ) samples by using the sol-gel method without postannealing under high oxygen pressure, and then measured temperature-dependent resistivity under various hydrostatic pressures up to 18 GPa by using the cubic anvil and two-stage multianvil apparatus. We find that the density-wave-like anomaly in resistivity is progressively suppressed with increasing pressure and the resistivity drop corresponding to the onset of superconductivity emerges at pressure as low as ∼ 6 GPa . Zero resistivity is achieved at 9 GPa below T c zero ≈ 6.6 K , which increases quickly with pressure to 41 K at 18 GPa. However, the diamagnetic response was not detected in the ac magnetic susceptibility measurements up to 15 GPa, indicating a filamentary nature of the observed superconductivity in the studied pressure range. The constructed T − P phase diagram reveals an intimate relationship between superconductivity, density-wave-like order, and the strange-metal-like behaviors. The observation of zero-resistance state in the polycrystalline La 3 Ni 2 O 7 − δ samples under high pressures not only corroborates the recent report of superconductivity in the pressurized La 3 Ni 2 O 7 crystals but also facilitates further studies on this emerging family of nickelate high- T c superconductors. Published by the American Physical Society 2024

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Interlaboratory Reproducibility of Contour Method Data in a High Strength Aluminum Alloy

The contour method for residual stress measurement has seen significant development, but an experimental reproducibility study utilizing physical samples has not been published. A double-blind reproducibly study is reported, having scope beginning with EDM cutting and ending with residual stress calculation. A reinforced I-beam sample geometry is identified for its unique residual stress profile when extracted from residual stress bearing quenched aluminum bar (7050-T74). Contour measurements are prescribed on a midplane of symmetry with dimensions 24.0 mm by 50.0 mm. Fourteen identically prepared samples are fabricated from a single long bar with well characterized and uniform residual stress. Five samples throughout the bar are identified for planning measurements to validate sample uniformity and overall suitability of the residual stress field. The planning measurements employ a range of techniques: contour method, neutron diffraction, and hole-drilling. Eight samples are distributed to an international group of participants to execute their standard measurement practice. A double-blind process is followed to provide anonymity. Results are provided by eight participants: six being self-similar and two being quite different, the latter set aside as outliers. An average residual stress field is established from non-outlying results and the spatial distribution of reproducibility standard deviation is determined. The average stress field ranges from -60 to 70 MPa and the reproducibility standard deviation averages 8.1 MPa on the measurement plane. The average reproducibility standard deviation is about 3 × larger for points within 1.0 mm of plane boundaries (17.6 MPa) than for the remaining points (6.1 MPa). Reproducibility standard deviation (among different labs) for contour method residual stress measurement is found to be very similar to repeatability standard deviation (in a single lab) reported in prior work. The reproducibility observed here, for the entire measurement process, is also similar to that found in a prior reproducibility study limited to contour method data analysis.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Collective Analysis of Alpha Particle Losses Due to Self-Absorption by Mass Loading on Radioactive Particulate Glass Fiber Filters

In this study, we derived a relationship between filter mass loading and the percent loss during analysis using the mass loading data collected from six previous studies of self-absorption. Components of mass loading include particulate dust, radioactive particulates, and filter material. In a research report published in 1984, Higby calculated a minimum burial depth for an alpha particle to be lost due to absorption (100% loss) of about 3.7 mg/cm 2 based on calculations for the range of 239-Pu alpha particles in glass fiber filters. From there, Higby concluded that a correction factor of 0.85 assumes approximately 15% losses in the count rate of both alpha and beta particles. In 2000, Luetzelschwab et al. recommended assuming a 40% loss at a loading of 3.3 mg/cm 2 and a 28% loss for a loading of 2.3 mg/cm 2 which included the frontal face mass of the filter. More recently, the 100% losses due to absorption were reported to be in the 10 mg/cm 2 range. Presented here is a trinomial relationship method of relating percent loss due to self-absorption to filter mass loading, based on data reported by Higby, Luetzelschwab et al., Huang et al., Barnett et al., Smith et al., and Hogue et al. Under normal operating conditions at the stacks monitored by Effluent Management, the mass loading of sample filters averages 0.09 ± 0.12 (2s) mg/cm 2 (excluding negative values and outliers) and ranges from 0 mg/cm 2 to 0.24 mg/cm 2 . Based on current mass loading results for Effluent Management stack sample filters, the forced-zero trinomial relationship method estimated self-absorption losses of less than 5%. Because American National Standards Institute/Health Physics Society N13.1-2011 guidelines indicate a correction factor should be used when the penetration of radioactive material into the collection media or self-absorption of radiation by the material collected would reduce the count rate by more than 5%, it is possible continued application of a correction factor to the Effluent Management stack samples is no longer necessary. Nevertheless, continuing to assign a correction factor at the 5% threshold (i.e., 0.95) would be a conservative approach.

36 MATERIALS SCIENCE↗
DOE OSTI2020

Thermal, mechanical, and electrical properties of LSCo/mullite composite contact materials for solid oxide fuel cells

Lanthanum strontium cobaltite (LSCo) is considered as a good candidate cathode contact material for solid oxide fuel cells, due to high electrical conductivity. However, LSCo has a very large coefficient of thermal expansion (CTE) than the cells and metallic interconnects. As a result, poor mechanical stability is expected during thermal cycling. To minimize the CTE mismatch, we investigate a composite approach involving mixing LSCo with an inert material of low CTE, such as mullite at volume fractions from 0.1 to 0.4. Composite’s CTE shows a decreasing trend with increasing mullite volume fractions, and is consistent with model predictions. X-ray powder diffraction analysis of sintered LSCo/mullite composites exhibits no presence of other phases for samples aged for 500h at 800oC, indicating chemical compatibility. Electrical conductivity by a 4-pt method shows a decreasing trend with increasing mullite content. Contact strength of as-sintered and thermally cycled samples show that only the composite with 0.4 volume fraction has a measurable strength; the other composites have no strength. Overall, the composite approach is demonstrated in the LSCo/mullite system to lower the CTE and hence achieve thermal cycle stability. The addition of the inert phase to the LSCo matrix; however, also reduces the electrical conductivity.

Contact materials, LSCo, mullite, CTE, electrical ↗
DOE OSTI2021

A single column separation method for barium isotope analysis of geologic and hydrologic materials with complex matrices

Abstract The increasing significance of barium (Ba) in environmental and geologic research in recent years has led to interest in the application of the Ba isotopic composition as a tracer for natural materials with complex matrices. Most Ba isotope measurement techniques require separation of Ba from the rest of sample prior to analysis. This paper presents a method using readily available materials and disposable columns that effectively separates Ba from a range of geologic and hydrologic materials, including carbonate minerals, silicate rocks, barite, river water, and fluids with high total dissolved solids and organic content such as oil and gas brines, rapidly and without need for an additional cleanup column. The technique involves off-the-shelf columns and cation exchange resin and a two-reagent elution that uses 2.5 N HCl followed by addition of 2.0 N HNO 3 . We present data to show that major matrix elements from almost any natural material are separated from Ba in a single column pass, and that the method also effectively reduces or eliminates isobaric interferences from lanthanum and cerium.

Matecha, R. M.↗
DOE OSTI2022

RUScal : Software for the analysis of resonant ultrasound spectroscopy measurements

Resonant ultrasound spectroscopy is used to nondestructively measure the elastic resonances of small solids to elucidate the material's elastic properties or other qualities like size, shape, or composition. In this work, we introduce the software RUScal for the purpose of determining elastic properties by analyzing the eigenfrequencies of solid specimens with common shapes, such as rectangular parallelepipeds, cylinders (solid and hollow tube), ellipsoids, and octahedrons, as well as irregularly shaped ellipsoids that can be described analytically. All symmetry classes are supported, from isotropic to triclinic, along with the option to add or remove up to three orthogonal mirror planes as well as the ability to reorient the crystal axes with respect the sample edges via Euler angles. Additional features include tools to help find initial sets of elastic constants, including grid exploration and Monte Carlo methods, a tool to analyze frequencies as a function of sample length or crystal orientation, an error analysis tool to assess fit quality, and formatting of the input and output files for batch fitting, e.g., as a function of temperature. This software was validated with published resonant ultrasound spectroscopy data for various materials, shapes, and symmetries with noted improvements in calculation time compared to finite element methods.

47 OTHER INSTRUMENTATION↗