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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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October 2024 Semiannual Composite Salt Waste Processing Facility (SWPF) Decontaminated Salt Solution (DSS) Toxicity Characteristic Leaching Procedure (TCLP) Results

The aqueous waste from the Salt Waste Processing Facility (SWPF) is sampled semiannually for transfers to the Saltstone Production Facility (SPF). Salt solution is treated at SPF and disposed of in the Saltstone Disposal Facility (SDF). Per request of customer, X-TTR-Z-00027, Revision 0, one SDF waste form (saltstone) sample was prepared in the Savannah River National Laboratory (SRNL) from the SWPF Decontaminated Salt Solution (DSS) Waste Acceptance Criteria (WAC) sample and Z-area premix material for the October 2024 semiannual Toxicity Characteristic Leaching Procedure (TCLP) sample. The sample contained 60:40 (by weight) of slag and fly ash (referred to as the “Cement-Free grout sample”). Results from the technical report support Task 2: ‘Grout Leaching Analyses’ of the Task Technical Request (TTR) prepared by Savannah River Mission Completion (SRMC). At 64 days cured, a sample of the SDF waste form was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure (TCLP). The October 2024 semiannual Cement-Free grout sample met the South Carolina (SC) Code of Regulations for Hazardous Waste Management Regulations (HWMR) 61-79.261.24 and 61-79.268.48 requirements for a non-hazardous waste form with respect to the Resource Conservation and Recovery Act (RCRA) metals and Underlying Hazardous Constituents (UHCs), and met the SPF WAC that was in effect at the time of the sample collection at SWPF.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Calendar Year 2020 Underground Test Area Annual Sampling Report Nevada National Security Site, Nevada (Rev. 1)

This CY 2020 annual sampling report presents the background of the FFACO and Sampling Plan implementation, sampling and analysis methods, sampling results, quality assurance and quality control, regulatory requirements, and analytical data for the CY 2020. Appendix A presents data from samples collected in CY 2020 from the YF/CM CAU and the RM/SM CAU. This sampling was conducted in support of the Sampling Plan at these CAUs prior to approval of the final CRs. Appendix B presents the well completion diagrams for the wells sampled in CY 2020. Appendix C presents data from samples collected in CY 2019. These results were not reported in the previous sampling report because they were not available from the specialized laboratories at the time of the report’s publication.

54 ENVIRONMENTAL SCIENCES↗

April 2024 Semiannual Composite Salt Waste Processing Facility (SWPF) Decontaminated Salt Solution (DSS) Toxicity Characteristic Leaching Procedure (TCLP) Results

The aqueous waste from the Salt Waste Processing Facility (SWPF) is sampled semiannually for transfers to the Saltstone Production Facility (SPF). Salt solution is treated at SPF and disposed of in the Saltstone Disposal Facility (SDF). Per request of customer, X-TTR-Z-00027, Revision 0, one SDF waste form (saltstone) sample was prepared in the Savannah River National Laboratory (SRNL) from the SWPF Decontaminated Salt Solution (DSS) Waste Acceptance Criteria (WAC) sample and Z-area premix material for the April 2024 semiannual Toxicity Characteristic Leaching Procedure (TCLP) sample. The sample contained 60:40 (by weight) of slag and fly ash (referred to as the “Cement-Free grout sample”). Results from the technical report support Task 2: ‘Grout Leaching Analyses’ of the Task Technical Request (TTR) prepared by Savannah River Mission Completion (SRMC). After at least 28 days cured, a sample of the SDF waste form was collected and shipped to a certified laboratory for analysis using the Toxicity Characteristic Leaching Procedure (TCLP). The April 2024 semiannual Cement-Free grout sample met the South Carolina (SC) Code of Regulations for Hazardous Waste Management Regulations (HWMR) 61-79.261.24 and 61-79.268.48 requirements for a non-hazardous waste form with respect to the Resource Conservation and Recovery Act (RCRA) metals and Underlying Hazardous Constituents (UHCs), and met the SPF WAC that was in effect at the time of the tank sampling.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Meta-Study of Particulate Detection Losses on Radioactive Air Sample Filters

Several mathematical relationships between air sample filter mass loading and the correlated analytical self-absorption factor were developed using data from other published research in this meta-study. Gross-alpha and -beta applications are addressed for this research. As filter media becomes loaded with particulate matter, there is potential for measurement losses due to self-absorption by mass loading. Components contributing to absorption include particulate dust, radioactive particulates, and filter material. Standards 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 detection rate by more than 5%. Previously, losses due to self-absorption have been reported up to 100% over a range up to ~10 mg∙cm -2 mass loading. These absorption losses then can be used to determine a correction factor for sample results. For low mass loadings (e.g., ≤0.1 mg∙cm -2 ) corrections factors in the 0.85 - 1 range have been recommended and used, while at higher mass loadings nearer to 10 mg∙cm -2 correction factors closer to 0 (representing near 100% losses) are used. Based on data from published studies, the different methods for relating percent loss due to self-absorption to mass loading include linear, exponential, quadratic, and trinomial derived functions. Where applicable, both forced zero and non-forced zero results were evaluated. From the derived functions evaluated, the trinomial function provided the best fit. Once the sample filter mass loading is known, the trinomial function can be applied to estimate losses and the corresponding self-absorption factor. When applied to routine operating conditions for radiological facility stacks monitored at the Pacific Northwest National Laboratory for an average sample filter mass loading of 0.09 ± 0.12 (2σ) mg∙cm -2 (excluding negative values and outliers) and a range from 0 - 0.24 mg∙cm -2 , the estimated trinomial function nominal self-absorption losses are less than 5% at 0.09 mg∙cm -2 and less than 10% at 0.24 mg∙cm -2 . The trinomial function is one method that may be used to adjust the activity results of an air sample when the sample-specific mass loading is determined. The application of no correction factor when the ANSI/HPS N13.1-2021 guidance of a 5% threshold for loss is not reached with typical stack sample mass loadings may be reasonable in high-efficiency particulate air filtered systems. For simplicity, it would be conservative in assigning the self-absorption correction factor at the 5% threshold (i.e., 0.95) for general uses but in cases of heavy mass loading to calculate the factor.

air sampling↗

Data Report: UT-GOM2-1 Sediment Grain Size Measurements at Site GC 955, Holes H002 and H005

Sediment grain size measurement in marine sediments provides a record of the stratigraphic variation in grain size and thus energy regime at the time of deposition. In addition to the grain size distribution, the degree of sediment sorting can also be calculated, and together they both influence primary sediment porosity and permeability. Here we present sediment grain size results from laser diffraction particle size analysis of samples from pressure cores collected during the 2017 UT GOM2-1 Expedition. We measured both bulk sediment and organic carbon-free sediment fractions for 46 samples and organic carbon-free sediment for 5 samples at Site GC 955, Holes H002 and H005. Differences between the bulk sediment and organic carbon-free fractions reflect the relative amount and size fraction of the organic carbon. The sample results presented here represent the grain size variation of the host lithology across the Green Canyon (GC) 955 gas hydrate reservoir.

03 NATURAL GAS↗

Iodine Air Sampling: Installation and Preliminary Results

The F-Area wetlands are a known sink for radioiodine generated at the Savannah River Site (SRS). Wastewater containing iodine-129 ( 129 I) was discharged into the F-Area Seepage Basins for disposal, but the acidity of the wastewater mobilized some of the contaminants from the basin soil through the vadose zone and into the groundwater; ultimately creating a groundwater plume that extends towards Fourmile Branch and its associated wetland areas. Dissolved radioiodine specifically has migrated to the nearby F-Area wetlands, where it persists as a contaminant of concern. Accumulation and resurfacing of 129 I in the wetlands and nearby areas creates a potential secondary source zone where changes in biogeochemical conditions could result in the release of this sequestered 129 I to the air. Monitoring data has indicated that 129 I has a seasonal behavior at several surface water stations, with high concentrations during summertime and low concentrations during wintertime. Still, it is not known which factors control the seasonal behavior of 129 I. Further, it has been reported that 129 I contributed approximately 23% to the 2019 SRS offsite air pathway dose to the representative person for that year (SRNS, 2020), but air measurements of 129 I have never been taken in the F-Area wetlands. Because air emissions of 129 I from the wetlands have never been investigated, it is not known if this could be a potential release pathway that needs to be included in the site conceptual model. To address these unknowns, the Savannah River National Laboratory (SRNL) has an applied research task to investigate whether 129 I in the wetlands is emitted to the air and, if so, whether air concentrations exhibit seasonal variation. This report presents information about the system recently installed in the F-Area wetlands for measuring 129 I, as well as analysis results for samples collected June through August 2023. Quantification of this constituent will provide a better understanding of the contribution of airborne 129 I from the F-Area wetlands to the offsite dose and better inform ongoing and future remedial actions.

54 ENVIRONMENTAL SCIENCES↗

Evaluation of Significance Tests on Stack Sample Data

In October 2023, external assessors visiting LANL’s Rad-NESHAP team reviewed the annual source term documentation package for stack emissions. This document discusses how the team uses significance tests to determine whether or not a measurement represents an actual detection of emitted radioactive material. The significance tests used in the evaluation compare the measured sample result to the Minimum Detectable Activity (MDA) for the sample; to the uncertainty of that measurement; and to the mean blank sample for the same time period. The blank test uses the average blank plus 2-standard deviations (2σ) of the blank results as a comparison threshold for this final evaluation.

54 ENVIRONMENTAL SCIENCES↗

Phosphorus speciation analysis of fatty-acid-based feedstocks and fast pyrolysis biocrudes via gel permeation chromatography inductively coupled plasma high-resolution mass spectrometry

Renewable feedstocks, such as lignocelulosic fast pyrolysis oils and both vegetable oil and animal fats, are becoming a viable alternative to petroleum for producing high-quality renewable transportation fuels. However, the presence of phosphorus-containing compounds, mainly from phospholipids, in these renewable feedstocks is known to poison and deactivate hydrotreating catalysts during fuel production. In this work, gel permeation chromatography (GPC) combined with inductively coupled plasma high-resolution mass spectrometry (ICP-HRMS) was used to analyze feedstocks including unprocessed soybean oil, animal fat, and pyrolysis oils from red oak and milorganite to identify phosphorus species. The results have shown the presence of a wide range of different phosphorous compounds among all the samples analysed in this work. The GPC-ICP-HRMS analyses of a vegetable oil and two animal fats have shown different fingerprints based on the molecular weight of each of the samples, highlighting the structural differences among their corresponding phosphorus-containing compounds. While the presence of low-molecular-weight species, such as phospholipids, was expected, several high-molecular-weight species (MW > 10 000 Da) have been found, suggesting that high-molecular-weight micelles or liposomes might have been formed due to the high concentration of phospholipids in these samples. Results obtained through the hydroxylation of a mix of phospholipids (asolectin) and its posterior GPC-ICP-HRMS agree with this hypothesis. With respect to the lignocellulosic catalytic fast pyrolysis oil samples, the GPC-ICP-HRMS results obtained suggest that either aggregation or polymerization reactions might have occurred during the pyrolysis process, yielding phosphorus-containing compounds with an approximate molecular weight above 91 000 kDa. In addition, an aggregation phenomenom has been observed for those phosphorus species present within the fast pyrolysis oils after being stored for 3 months, especially for those pyrolysis oils contaning pre-processed feedstocks, such as milorganite.

09 BIOMASS FUELS↗

Effect of processing parameters and strut dimensions on the microstructures and hardness of stainless steel 316L lattice-emulating structures made by powder bed fusion

In this study, we present the effects of input processing parameters and strut thickness (in square struts) on microstructure and properties in laser powder bed fusion additively manufactured stainless steel 316L lattice-emulating structures. Lattice-emulating X-structures with square cross-sections of 1.5, 1.0, and 0.5 mm were fabricated using three different parameter sets with varying power, speed, and therefore, linear energy density. Grain size and morphology were shown to be dictated by epitaxial growth, which was dependent on weld pool morphology. Additionally, grain size and morphology were shown to change across the thickness direction of the struts (from the bottom inclined surface to the top inclined surface). The spatial variation in grain size was reflected by changes in hardness through the thickness of each strut. The 0.5 mm struts exhibited more significant grain elongation in the strut direction and larger sub-grain solidification cell diameters than their thicker counterparts. The larger sub-grain solidification cell diameters in the 0.5 mm samples resulted in correspondingly lower hardness values when compared to samples of higher thicknesses.

36 MATERIALS SCIENCE↗

Additional Analysis of the 2H-Evaporator Wall Scale Sample HTF-17-57

Savannah River National Laboratory previously analyzed scale samples from both the wall and cone sections of the 242-16H Evaporator prior to chemical cleaning. The samples were analyzed for uranium and plutonium isotopes required for a Nuclear Criticality Safety Assessment of the scale removal process. The analysis of the scale samples found the material to contain crystalline nitrated cancrinite and clarkeite and significant amounts of mercury. Savannah River Remediation subsequently requested additional analyses on the samples. Inspection of the sample bottles revealed that no sample remained of the cone scale (HTF-17-56) while approximately 4 g of the wall scale sample (HTF-17-57) remained. The wall sample was subsequently ground with a mortar and pestle, at which time it was discovered that the sample contained a significant amount of liquid, metallic mercury. The portion of the sample that was not mercury was approximately 3 g. This portion of the sample was analyzed to determine the concentrations of selected radionuclides. The following radionuclide concentrations were measured: <9.6E+02 dpm/g H-3, 2.9E+02 dpm/g C-14, 5.6E+03 dpm/g Tc-99, and 1.6E+02 dpm/g I-129. Blank samples were also analyzed to evaluate sample contamination from the Shielded Cells environment. All blank sample results were below detectable limits. Due to the limited sample size and the anticipated low levels of the target radionuclides, no replicate sample analysis was conducted.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Mid-Atlantic US observations of radiocarbon in CO 2 : fossil and biogenic source partitioning and model evaluation

Accurately quantifying regional anthropogenic CO 2 fluxes is fundamental to improving our understanding of the carbon cycle and for creating effective carbon mitigation policies, and the radiocarbon to total carbon ratio in atmospheric CO 2 (Δ 14 CO 2 ) is a robust tracer of fossil fuel CO 2 that can discriminate between biogenic and fossil fuel CO 2 sources. NASA's Atmospheric Carbon and Transport-America (ACT-America) airborne mission between 2016 and 2019 aimed to improve the accuracy of regional greenhouse gas flux estimates, through refining our understanding and characterization of fluxes and flux uncertainties in models. Δ 14 CO 2 observations from 26 flights are presented for examining seasonal CO 2 source partitioning in the Mid-Atlantic USA. Observed variability in boundary layer CO 2 at timescales ranging from intra-day to seasonal was largely driven by biogenic CO 2 (CO 2bio ) variability that ranged from −19.7 ppm in summer to 16.2 ppm in fall, while fossil fuel CO 2 (CO 2ff ) variability remained at 3.3±2.0 ppm. Carbonyl sulfide uptake was well-correlated with CO 2bio uptake, and examining this relationship, as well as that between CO 2 and CO 2bio variability reinforces the seasonal extent of gross primary productivity response throughout ACT-America. We use airborne Δ 14 CO 2 flask sampling alongside in situ carbon monoxide measurements to calculate high-frequency CO 2ff and evaluate the magnitude and diurnal variability of modeled CO 2ff , deducing likely transport errors in an example flight. Although ACT-America CO 2ff signals were attenuated due to the broad source regions sampled, results illustrate the value of Δ 14 CO 2 sampling and observation-based methodologies for regional CO 2 flux attribution, evaluation and improvement of modeled CO 2 .

Baier, Bianca C. [National Oceanic and Atmospheric↗

Rarefied piezometric uptake apparatus and method for measuring gaseous uptake

A rarefied piezometric uptake apparatus and method for measuring gaseous uptake for large solid samples with little or no sample preparation. Past systems and methods require extensive sample preparation. The method includes providing a rarefied piezometric uptake apparatus having a dosing chamber and uptake chamber in an improved selective fluid communication. The apparatus and method improve the measurement of gaseous uptake into solid samples resulting in improved prediction of gas migration through solid samples such as geologic formations.

Paul, Matthew J.↗

Splat Quenching as a High Throughput Rapid Solidification Testing Method for Developing Additive Manufacturing Alloys

Splat quenching as a high throughput rapid solidification screening tool is evaluated. Samples were made using known alloys (SS316, IN625, Ti-5553) to evaluate and establish the microstructures for a variety of alloy systems as well as the predicted cooling rates. The samples are inductively heated and levitated prior to being struck between two platens that produce a high contact pressure and a thin sample resulting in cooling rates on the order of 10 6 to 10 7 K/s. Process parameters were evaluated with analytical models in addition to numerical simulations to provide an effect of process variables such as substrate material, melt superheat, and platen velocity on the resulting solidification. The splat thickness was found to be controlled by platen velocity, melt superheat, as well as the feedstock volume. The sample thickness is the key controlling factor for varying the average cooling rate experienced by the splat quenched sample. The splat quenching techniques can reach regions of rapid solidification space that meet and exceed laser and electron beam techniques across the sample. In conclusion, the results of the study provide a useful foundation in understanding the splat quenching technique and its potential as a low effort tool to explore rapid solidification effects on alloys.

Alloy Design↗

An adaptive sampling augmented Lagrangian method for stochastic optimization with deterministic constraints

The primary goal of this paper is to provide an efficient solution algorithm based on the augmented Lagrangian framework for optimization problems with a stochastic objective function and deterministic constraints. Our main contribution is combining the augmented Lagrangian framework with adaptive sampling, resulting in an efficient optimization methodology validated with practical examples. To achieve the presented efficiency, here we consider inexact solutions for the augmented Lagrangian subproblems, and through an adaptive sampling mechanism, we control the variance in the gradient estimates. Furthermore, we analyze the theoretical performance of the proposed scheme by showing equivalence to a gradient descent algorithm on a Moreau envelope function, and we prove sublinear convergence for convex objectives and linear convergence for strongly convex objectives with affine equality constraints. The worst-case sample complexity of the resulting algorithm, for an arbitrary choice of penalty parameter in the augmented Lagrangian function, is $\mathscr{O}$(ϵ -3-δ ) , where ϵ > 0 is the expected error of the solution and δ > 0 is a user-defined parameter. If the penalty parameter is chosen to be $\mathscr{O}$(ϵ -1 ), we demonstrate that the result can be improved to $\mathscr{O}$(ϵ -2 ) , which is competitive with the other methods employed in the literature. Moreover, if the objective function is strongly convex with affine equality constraints, we obtain $\mathscr{O}$(ϵ -1 log(1/ϵ)) complexity. Finally, we empirically verify the performance of our adaptive sampling augmented Lagrangian framework in machine learning optimization and engineering design problems, including topology optimization of a heat sink with environmental uncertainty.

97 MATHEMATICS AND COMPUTING↗

Status of the MicroBooNE Low Energy Excess Search

MicroBooNE is a neutrino experiment that utilizes a liquid argon time projection chamber (LArTPC) located on-axis in the Booster Neutrino Beam (BNB) at Fermilab. One of the experiment’s main goals is to search for excess low-energy electromagnetic-like events as seen by the MiniBooNE experiment, located just downstream of MicroBooNE in the BNB. As MicroBooNE nears the completion of its first single-electron-like and single-photon-like searches, these proceedings present the status of MicroBooNE's low-energy excess search as of early summer 2020. In addition to presenting an overview of the approach to these analyses, we showcase results from $\pi^0$ calibrations and $e$/$\gamma$ separation, and sample results from sidebands aimed at validating the analysis' progress outside the low-energy signal region.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Superconductivity in WBe 2

WBe 2 , which occurs in space group 194, with hexagonal symmetry P6 3 /mmc, is prepared by arc-melting at temperatures above 2200 C, where Be vapor loss is significant. This study is motivated by recent work on MoB 2 and WB 2 , both superconductors (T c =32 and 17 K respectively) under high (∼70 GPa) pressure. In order to avoid the known Be-rich superconducting phases (WBe 13 and WBe 22 ) in the complex phase diagram, both known to be superconducting at 4.1 K, the sample was prepared with a slight (∼5 %) excess of W. The resultant sample, prepared using high purity (99.999 %) Be, is essentially single phase WBe 2 , with some spread in its superconducting properties due to the known homogeneity range. (WBe 2 forms in space group 194 between approximately W 1.02 Be 1.98 and W 0.88 Be 2.12 .) Characterization was carried out with x-ray diffraction, electrical resistivity, ρ, in zero and applied magnetic fields, and specific heat. The resistivity in zero and applied fields and specific heat data indicate that our sample of WBe 2 is a bulk superconductor at ambient pressure with a T c onset in ρ at 1.05 K, and T c (ρ→0) at ∼0.86 K. Furthermore, there is no signature of superconductivity in ρ at 4.1 K, indicating successful avoidance of WBe 13 and WBe 22 . The ρ data in field indicate an upper critical field of approximately 400 gauss.

Electrical transport↗

Microstructure Alignment Effects from Engineered Cooling during Additive Manufacturing of Alnico Magnets from Prealloyed Powder

Alnico is a rare-earth free; permanent magnet (PM) which maintains its saturation magnetization while at temperatures up to 550°C but lacks the coercivity and energy product needed for a wide range of demanding applications. With an optimal set of processing and manufacturing techniques, Alnico could replace Dy-free Nd-Fe-B magnets in certain applications if the microstructure is textured in a $\langle$001$\rangle$ direction. Additive manufacturing (AM) of near-net-shape magnets may provide such texture. To investigate the possibility, directed-energy deposition (DED) in conjunction with an actively cooled substrate was used to build samples with a compositionally modified, gas-atomized, Alnico 8 alloy. The resulting samples were solutionized and quenched, followed by magnetic annealing and a heat treatment. Magnetic properties and microstructures are compared to previous work.

36 MATERIALS SCIENCE↗

SARS-CoV-2 RNA in Wastewater Settled Solids Is Associated with COVID-19 Cases in a Large Urban Sewershed

Wastewater-based epidemiology may be useful for informing public health response to viral diseases like COVID-19 caused by SARS-CoV-2. Here, we quantified SARS-CoV-2 RNA in wastewater influent and primary settled solids in two wastewater treatment plants to inform the preanalytical and analytical approaches and to assess whether influent or solids harbored more viral targets. The primary settled solids samples resulted in higher SARS-CoV-2 detection frequencies than the corresponding influent samples. Likewise, SARS-CoV-2 RNA was more readily detected in solids using one-step digital droplet (dd)RT-PCR than with two-step RT-QPCR and two-step ddRT-PCR, likely owing to reduced inhibition with the one-step ddRT-PCR assay. We subsequently analyzed a longitudinal time series of 89 settled solids samples from a single plant for SARS-CoV-2 RNA as well as coronavirus recovery (bovine coronavirus) and fecal strength (pepper mild mottle virus) controls. SARS-CoV-2 RNA targets N1 and N2 concentrations correlated positively and significantly with COVID-19 clinically confirmed case counts in the sewershed. Together, the results demonstrate that measuring SARS-CoV-2 RNA concentrations in settled solids may be a more sensitive approach than measuring SARS-CoV-2 in influent.

54 ENVIRONMENTAL SCIENCES↗