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At least 361 records · Page 20

Analysis of Harrell Monosodium Titanate Lot #46000908120

Monosodium titanate (MST) for use in the Actinide Removal Process (ARP) must be qualified and verified in advance. A single qualification sample for each batch of material is sent to SRNL for analysis, as well as a statistical sampling of verification samples. The original Harrell Industries Lot #46000908120 qualification and 16 verification samples received in October 2012 failed to meet the specification for weight percent solids. All of the pails sampled and tested contained less than 15 wt % MST solids. The lot was returned to the vendor, and in February 2014 a new qualification sample and set of 16 verification samples were received from this lot. The new lot met each of the selected specification requirements that were tested and, consequently, the material is acceptable for use in the ARP process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Mercury Source Zone Identification using Soil Vapor Sampling and Analysis

Development and demonstration of reliable measurement techniqes that can detect and help quantify the nature and extent of elemental mercury (Hg(0)) in the subsurface are needed to reduce certainties in the decision making process and increase the effectiveness of remedial actions. We conducted field tests at the Y-12 National Security Complex (NSC) in Oak Ridge, TN, to determine if sampling and analysis of Hg(0) vapors in the shallow subsurface (<0.3 m depth) can be used to as an indicator of the location and extent of Hg(0) releases in the subsurface. We constructed a rigid PVC pushprobe assembly, which was driven into the ground. Soil gas samples were collected through a sealed inner tube of the assembly and analyzed immediately in the field with a Lumex and/or Jerome Hg(0) analyzer. Time-series sampling showed that Hg vapor concentrations were fairly stable over time suggesting that the vapor phase Hg(0) was not being depleted and that sampling results were not dependent on the soil gas purge volume. Hg(0) vapor data collected at over 200 pushprobe locations at 3 different release sites correlated well to areas of known Hg(0) contamination. Vertical profiling of Hg(0) vapor concentrations conducted at 2 locations provided information on the vertical distribution of Hg(0) contamination in the subsurface. We concluded from our studies that soil gas sampling and analysis can be conducted rapidly and inexpensively at a large scale to help identify areas contaminated with Hg(0).

Watson, David B↗

Experimental and Phenomenological Investigations of the MiniBooNE Anomaly

This thesis covers a range of experimental and theoretical efforts to elucidate the origin of the $4.8\sigma$ MiniBooNE low energy excess (LEE). We begin with the follow-up MicroBooNE experiment, which took data along the BNB from 2016 to 2021. This thesis specifically presents MicroBooNE's search for $\nu_e$ charged-current quasi-elastic (CCQE) interactions consistent with two-body scattering. The two-body CCQE analysis uses a novel reconstruction process, including a number of deep-learning-based algorithms, to isolate a sample of $\nu_e$ CCQE interaction candidates with $75\%$ purity. The analysis rules out an entirely $\nu_e$-based explanation of the MiniBooNE excess at the $2.4\sigma$ confidence level. We next perform a combined fit of MicroBooNE and MiniBooNE data to the popular $3+1$ model; even after the MicroBooNE results, allowed regions in $\Delta m^2$-$\sin^2 2_{\theta_{\mu e}}$ parameter space exist at the $3\sigma$ confidence level. This thesis also demonstrates that the MicroBooNE data are consistent with a $\overline{\nu}_e$-based explanation of the MiniBooNE LEE at the $<2\sigma$ confidence level. Next, we investigate a phenomenological explanation of the MiniBooNE excess combining the $3+1$ model with a dipole-coupled heavy neutral lepton (HNL). It is shown that a 500 MeV HNL can accommodate the energy and angular distributions of the LEE at the $2\sigma$ confidence level while avoiding stringent constraints derived from MINER$\nu$A elastic scattering data. Finally, we discuss the Coherent CAPTAIN-Mills experiment--a 10-ton light-based liquid argon detector at Los Alamos National Laboratory. The background rejection achieved from a novel Cherenkov-based reconstruction algorithm will enable world-leading sensitivity to a number of beyond-the-Standard Model physics scenarios, including dipole-coupled HNLs.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Analysis of Pitting Corrosion on Wrought and Additively Manufactured 316L Stainless Steel in Atmospheric Environments

Additive manufacturing of metal components enables rapid fabrication of complex geometries. However, metal additive manufacturing also introduces new morphological and microstructural characteristics which might be detrimental to component performance. Here we report the pitting corrosion properties of wrought and additively manufactured 316L stainless steel after atmospheric exposure to coastal environments and laboratory-created environments. Qualitative visualization in combination with quantitative analysis of resulting pits provided an in-depth understanding of pitting differences between wrought and additively manufactured 316L stainless steel and between coastal and laboratory-based exposure. Optical and scanning electron microscopy were utilized for visualization, while white light interferometry measured pits across approximately 5mm x 5mm areas on each sample. Post-processing of the interferometry data enables quantification of pitting attack for each sample in terms of both pit depth and pit volume. The pitting analysis introduced herein offers a new technique to compare pitting attack between different manufacturing processes and materials.

36 MATERIALS SCIENCE↗

Summary Report for the Environmental Protection Agency MERL/FRMAC/RAP Mission Alignment Exercise held at the Savannah River Site on June 9-13 2014

From June 9th thru June 13th 2014, members of the Federal Radiological Monitoring and Assessment Center (FRMAC), the Environmental Protection Agency (EPA) and the Department of Energy Radiological Assistance Program (DOE RAP) Region-3 participated in a joint nuclear incident emergency response exercise at the Savannah River Site (SRS) near Aiken, South Carolina. The purpose of this exercise was to strengthen the interoperability relationship between the FRMAC, RAP, and the EPA Mobile Environmental Radiation Laboratory (MERL) stationed in Montgomery, Alabama. The exercise was designed to allowed members of the DOE RAP Region-3 team to collect soil, water, vegetation and air samples from SRS and submit them through an established FRMAC hotline. Once received and processed through the hotline, FRMAC delivered the samples to the EPA MERL for sample preparation and laboratory radiological analysis. Upon completion of laboratory analysis, data was reviewed and submitted back to FRMAC via an electronic data deliverable (EDD). As part of the exercise, an evaluation was conducted to identify gaps and potential improvements in each step of the processes. Additionally, noteworthy practices and potential future areas of interoperability between FRMAC and EPA were acknowledged. The exercise also provided a unique opportunity for FRMAC personnel to observe EPA sample receipt and sample preparation processes and to gain familiarity with the MERL laboratory instrumentation and radiation detection capabilities. The observations and lessons-learned from this exercise will be critical for developing a more efficient, integrated response for future interactions between the FRMAC and EPA assets.

54 ENVIRONMENTAL SCIENCES↗

Enabling Microscale Processing: Combined Raman and Absorbance Spectroscopy for Microfluidic On-Line Monitoring

Microfluidics have many potential applications including characterization of chemical processes on a reduced scale, spanning the study of reaction kinetics using on-chip liquid–liquid extractions, sample pretreatment to simplify off-chip analysis, and for portable spectroscopic analyses. The use of in situ characterization of process streams from laboratory-scale and microscale experiments on the same chemical system can provide comprehensive understanding and in-depth analysis of any similarities or differences between process conditions at different scales. A well-characterized extraction of Nd(NO 3 ) 3 from an aqueous phase of varying NO 3– (aq) concentration with tributyl phosphate (TBP) in dodecane was the focus of this microscale study and was compared to an earlier laboratory-scale study utilizing counter current extraction equipment. Here, we verify that this same extraction process can be followed on the microscale using spectroscopic methods adapted for microfluidic measurement. Concentration of Nd (based on UV–vis) and nitrate (based on Raman) was chemometrically measured during the flow experiment, and resulting data were used to determine the distribution ratio for Nd. Extraction distributions measured on the microscale were compared favorably with those determined on the laboratory scale in the earlier study. Both micro-Raman and micro-UV–vis spectroscopy can be used to determine fundamental parameters with significantly reduced sample size as compared to traditional laboratory-scale approaches. This leads naturally to time, cost, and waste reductions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

High temperature polymer degradation: Rapid IR flow-through method for volatile quantification

Accelerated aging of polymers at elevated temperatures often involves the generation of volatiles. These can be formed as the products of oxidative degradation reactions or intrinsic pyrolytic decomposition as part of polymer scission reactions. A simple analytical method for the quantification of water, CO 2 , and CO as fundamental signatures of degradation kinetics is required. Here, we describe an analytical framework and develops a rapid mid-IR based gas analysis methodology to quantify volatiles that are contained in small ampoules after aging exposures. The approach requires identification of unique spectral signatures, systematic calibration with known concentrations of volatiles, and a rapid acquisition FTIR spectrometer for time resolved successive spectra. Furthermore, the volatiles are flushed out from the ampoule with dry N2 carrier gas and are then quantified through spectral and time integration. This method is sufficiently sensitive to determine absolute yields of ~50 μg water or CO 2 , which relates to probing mass losses of less than 0.01% for a 1 g sample, i.e. the early stages in the degradation process. Such quantitative gas analysis is not easily achieved with other approaches. Our approach opens up the possibility of quantitative monitoring of volatile evolution as an avenue to explore polymer degradation kinetics and its dependence on time and temperature.

36 MATERIALS SCIENCE↗

Air pollution from aircraft

A model which predicts nitric oxide and carbon monoxide emissions from a swirl can modular combustor is discussed. A detailed analysis of the turbulent fuel-air mixing process in the swirl can module wake region is reviewed. Hot wire anemometry was employed, and gas sampling analysis of fuel combustion emissions were performed.

Heywood, J. B.↗

Crack Detection in High-Velocity Oxygen-Fuel-Sprayed Al{sub 59.2}Cu{sub 25.5}Fe{sub 12.3}B{sub 3} Quasicrystalline Coatings Using Piezoelectric Active Sensors

Quasicrystals have received some attention in recent years regarding their potential usefulness as low friction and wear resistant materials. When quasicrystalline (QC) coatings are exposed to different levels of external loading or are subjected to thermal stresses, crack nucleation, and propagation become life-limiting factors. In this investigation, Al{sub 59.2}Cu{sub 25.5}Fe{sub 12.3}B{sub 3} QC coatings were deposited onto AISI-A36 steel substrates using the high-velocity oxygen-fuel (HVOF) technique. The coatings were deposited at different oxygen-to-fuel ratios. To characterize the integrity of the coatings, the active piezoceramic excitation technique was applied to detect the propagation of cracks during three-point bending tests. The piezoelectric transducer signal was processed using wavelet transformation analysis. The results revealed that the coated samples displayed different densities of cracks depending on the oxygen-to-fuel. The crack density was found higher for coatings formed using a slightly oxidizing flame. The opening of the pre-existing cracks in the coating was the main reason of signal attenuation during piezoelectric excitation. The HVOF-sprayed AlCuFeB quasicrystalline coating, with thickness between 150 and 180 μm, withstands a flexural stress as high as 340 MPa. To the best of our knowledge, this study is the first that provides a quantitative assessment of the viability of QC coatings in mechanical applications in spite of their intrinsic brittleness.

36 MATERIALS SCIENCE↗

Excipient screening by lyophilization provides insights into spray drying formulations for nanoparticle vaccines

Nanoparticles have shown great promise as delivery platforms in the development of tunable and safe vaccines. Nanolipoprotein particles (NLPs), also known as nanodiscs, are discoidal nanoparticles composed of a lipid bilayer stabilized at their periphery by apolipoproteins. Under the right conditions, the NLP self-assembly process is highly customizable in terms of lipids and apolipoprotein constituents, allowing for tunable physical and chemical characteristics. This flexibility allows a wide range of vaccine antigens and adjuvants to be incorporated onto the NLP platform for tailored vaccine design. The stability of NLPs during long term storage is a very important factor in developing a vaccine delivery platform suitable for widespread global use. When stored in a solution for extended periods of time, NLPs dissociate into their corresponding lipids and protein constituents, leading to particle degradation. Proper stabilization of NLPs can often be achieved by lyophilization (i.e. freeze-drying), a method widely used for various applications including pharmaceuticals. This process, however, can be damaging to particles without the presence of lyoprotectants or excipients that help maintain particle stability during lyophilization. Another method used to stabilize vaccines and pharmaceuticals is spray drying, a process that converts liquid formulations into dry powders through controlled heating and airflow. While spray drying is rapid, scalable, and cost-effective, lyophilization is typically a gentler process that better retains biomolecule structure and function. Both processes use excipients for particle stabilization, so lyophilization can be used as a surrogate to test stability of NLPs, to down-select formulations that may withstand the harsher conditions of spray drying. To screen different formulations, NLPs were synthesized and purified to homogeneity by size exclusion chromatography (SEC) and samples were prepared with a wide range of lyoprotectants and/or excipients. To assess the protective effects of excipients on NLPs upon spray drying, both pre- and post-lyophilized samples were analyzed by SEC. To assess the protective effects upon heating (encountered during the spray drying process), NLP samples were incubated at elevated temperatures prior to SEC analysis. The lyoprotectants and excipients evaluated in this study had different efficiencies in protecting NLPs during lyophilization and heating tests. Trehalose, for example, exhibits stabilization on NLPs both upon lyophilization and heating whereas leucine accelerated NLP dissociation. Although some lyoprotectants are effective by themselves, different combinations can decrease the stabilization of NLPs. Shelf-stable vaccines that do not require cold-chain storage are essential for global accessibility and our findings provide fundamental insight into how to advance NLP-based vaccines for these applications.

Serrano, Litzay J [Lawrence Livermore National Lab↗

Mixed Element Microparticle Characterization by Electron Probe Microanalysis

Abstract Microparticle compositional characterization for nuclear forensics has traditionally been achieved by “gold-standard” destructive analytical techniques such as large geometry-secondary ion mass spectrometry and fission track-thermal ionization mass spectrometry, but long processing times and total sample consumption eliminate the option of subsequent analysis by other methods. Electron probe microanalysis has long been widely employed for rapid, nondestructive, micrometer-scale compositional measurements and imaging in fields such as material science and geology and may therefore need to be reevaluated as an alternative tool for microparticle analysis for the nuclear forensics community. This study presents the use of electron probe microanalysis for imaging and quantitative characterization of homogeneous microparticles utilizing a calibration curve based on high-precision quadrupole-inductively coupled plasma-mass spectrometry analyses. Samples of opportunity synthesized at Savannah River National Laboratory, nickel-doped cerium oxide microparticles, were selected as analogs for plutonium-doped uranium oxide microparticles. Positive detection and accurate quantification of variable amounts of nickel dopant down to trace levels (10s of parts per million) suggest applicability of this technique to other mixed element systems (e.g., actinides). Quantitative single-particle characterization via electron probe microanalyzer may thus provide a high fidelity, nondestructive complement to techniques currently in use.

Riche, Alexis T. (ORCID:0009000121978126)↗

Application of X-ray microcomputed tomography in the characterization of irradiated nuclear fuel and material specimens

X-ray microcomputed tomography (µCT) was applied in characterizing the internal structures of a number of irradiated materials, including carbon-carbon fibre composites, nuclear-grade graphite and tristructural isotropic-coated fuel particles. Local cracks in carbon-carbon fibre composites associated with their synthesis process were observed with µCT without any destructive sample preparation. Pore analysis of graphite samples was performed quantitatively, and qualitative analysis of pore distribution was accomplished. It was also shown that high-resolution µCT can be used to probe internal layer defects of tristructural isotropic-coated fuel particles to elucidate the resulting high release of radioisotopes. Layer defects of sizes ranging from 1 to 5 µm and up could be isolated by to-mography. As an added advantage, µCT could also be used to identify regions with high densities of radioisotopes to deter-mine the proper plane and orientation of particle mounting for further analytical characterization, such as materialographic sectioning followed by optical and electron microscopy. Lastly, in fully ceramic matrix fuel forms, despite the highly absorbing matrix, characterization of tristructural isotropic-coated particles embedded in a silicon carbide matrix was accomplished usingµCT and related advanced image analysis techniques.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

SOLAr Critical Infrastructure Energization (SOLACE): Leveraging Distributed Energy Resources to Provide Local Power

This document is a technical report based on a large-scale DOE-funded project conducted between 2019 and 2022. The project, called SOLAr Critical infrastructure Energization (SOLACE), is aimed at leveraging distributed energy resources (DERs) to provide local power to communities, feeders, or other regions. The project included a particular focus on high-value critical loads such as municipal water supply, telecommunication hubs, and disaster shelters. The key developments of the project were: (1) A comprehensive pre-event power system analysis methodology that identifies and characterizes the viable local power options. (2) A DMS-based example control system for activating and operating the local power solution during a time of crisis. (3) Grid-forming inverter technology to enable isolated local power operation and black-starting. (4) Cyber-security considerations for isolated systems when wider-area communication may be offline. This report describes the overall process that identifies and assesses the viable DER-based local power solutions for a given facility, region, or community. The report documents the process, including the key analysis steps, tools required, data requirements, and recommended pass/fail criteria for each step. It also provides a sample implementation of this process through a test case. Finally, it provides details of how a viable pre-event plan can be selected and activated at go-time when an event has occurred.

14 SOLAR ENERGY↗

Apollo 16: Core 60004 - Preliminary study of less than 1 mm fines

The article studies the possible variation of mineralogy as a function of both grain size and depth within the core of less than 1 mm fines, for the core section 60004 from Apollo 16. Twelve samples of the fines were dry sieved. The grain size analysis showed a bimodal distribution for all samples, indicating a competing process of grain size degeneration and agglutinate formation. Approximately 99% of the minerals in the samples examined consisted of plagioclase feldspar, pyroxene and olivine, with plagioclase the dominant phase. The various minerals were analyzed, using standard electron microprobe techniques, as a function of size range for each sample, and the representative analyses are presented. Several types of glass were also analyzed, ranging in color from orange through yellow and green to colorless. The investigation of the chemical variations of mineral and lithic clasts from the top and the bottom of the core suggests that although minor variations are present, the regolith was derived from fairly homogeneous sources.

Meyer, H. O. A.↗

Nitrogen on Mars: Insights from Curiosity

Recent detection of nitrate on Mars indicates that nitrogen fixation processes occurred in early martian history. Data collected by the Sample Analysis at Mars (SAM) instrument on the Curiosity Rover can be integrated with Mars analog work in order to better understand the fixation and mobility of nitrogen on Mars, and thus its availability to putative biology. In particular, the relationship between nitrate and other soluble salts may help reveal the timing of nitrogen fixation and post-depositional behavior of nitrate on Mars. In addition, in situ measurements of nitrogen abundance and isotopic composition may be used to model atmospheric conditions on early Mars.

Stern, J. C.↗

Production of Carbon Nanomaterials and Sorbents from Domestic U.S. Coal (Final Report)

The main goal of this project was to produce high-value carbon nanomaterials and carbon sorbents from domestic coal resources in a cost-effective manner. Four types of domestic coal samples were processed through a combination of deashing, devolatilization, oxidation, reduction, and activation treatments to produce graphene oxide (GO), reduced graphene oxide (RGO), and activated carbon (AC). The precursors and developed materials were extensively characterized by various methods to investigate the impact of the coal feedstock type on the yield and quality of each product. A commercial graphite-based GO sample was included in the experimental work as the baseline material for comparison with the coal-based materials developed in this work. The performed work also included a technoeconomic analysis and cost estimation for a plant processing 20 tons/day coal, a market evaluation for the graphene materials, and a technology gap analysis. A simple process by concentrated nitric acid oxidation is used to oxidize coal precursors for the production of GO. Fine oxidized coal particles that were separated from larger oxidized coal particles had significantly higher oxygen contents and were identified as coal-based GO samples. Coarse oxidized coal particles were used as precursors for production of AC. Based on the Raman spectroscopy results, coal-based GO samples exhibited G and D bands similar to those of graphite-based GO samples. X-ray photoelectron spectroscopy revealed that coal-based GO samples had surface oxygen contents of ~26-35% that were higher than the oxygen contents of graphite-based GO samples. Larger particles of oxidized coal samples were activated under different conditions to produce high surface area functionalized AC. Prepared materials had surface areas exceeding 1,500 m 2 /g and pore volumes more than 1 cm 3 /g with different pore size distributions. Reduced graphene oxide samples were prepared by thermal reduction of both coal-based and graphite-based GO samples at 170-2800 ºC. Coal-based and graphite-based RGO samples exhibited similar carbon contents, Raman spectra, and XRD profiles. Heat treatment above 1500 ºC shifted RGO to synthetic graphite. Among anthracite, bituminous, subbituminous, and lignite coals tested, anthracite was the best precursor to produce carbon nanomaterials exhibiting properties similar to those of graphite-based materials. Anthracite-based carbon nanomaterials also had the highest production yields. Technoeconomic analysis estimated the production cost of GO and RGO for anthracite-based samples at about 2,600 and 4,200 $/ton, respectively, which is about two orders of magnitude lower than the current estimated price of graphite-based materials. Several gaps to further develop the proposed technology were identified and discussed that include process and equipment optimization, process integration, need for additional bench- and pilot-scale experiments, and other items to reduce the scale up risk. Market analysis reports suggested a compound annual growth rate of 40% for graphene and related materials. Short-term applications include composites, inks, and coatings. However, energy storage applications appear to be the dominant potential long-term applications. Different applications of coal-based GO and RGO need to be explored and clear metrics and standards for each application need to be developed.

01 COAL, LIGNITE, AND PEAT↗

Petrologic Comparison of High- and Low-Titanium Basalt Clasts Derived From ANGSA Core 73001

Volatile elements and compounds significantly influence the properties and behavior of magma, including ascent and eruptive processes. Basalts record a complicated history of the volatile species inherent to their parental magma, and the processes, such as degassing, that change these volatile inventories. On the Moon, outstanding questions remain concerning the behavior of magmatic volatiles and their roles in the evolution of lunar magmas and the formation of mare basalts. As part of the Apollo Next Generation Sample Analysis (ANGSA) program, we are investigating the petrogenesis of two basalt clasts collected from the recently processed Apollo 17 drive tube, 73001. Our team is studying the petrology of the two basalt clasts in 2D and 3D. Recent work has highlighted the utility of coupling traditional 2D methods with 3D measurements to better understand the crystallization and degassing histories of lunar lava flows. We are also investigating the volatile inventory of the samples through in situ studies of volatile-bearing phases, like apatite, to understand the eruptive signatures and degassing histories of low-titanium and high-titanium lunar basalts. At the upcoming conference, we will present the first detailed study of the 2D and 3D mineralogy, textures, 3D vesiculation, and chemistry of these basalt clasts to shed light on their magmatic, volcanic, and post-eruptive histories.

Basalt↗