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All sourcesNASA NTRSDOE OSTI
DOE OSTI2016

Observations and Modeling of the Green Ocean Amazon 2014/15: Transmission Electron Microscopy Analysis of Aerosol Particles Field Campaign Report

During two Intensive Operational Periods (IOP), we collected samples at 3-hour intervals for transmission electron microscopy analysis. The resulting transmission electron microscopy images and compositions were analyzed for the samples of interest. Further analysis will be done especially for the plume of interest. We found solid spherical organic particles from rebounded samples collected with Professor Scot Martin’s group (Harvard University). Approximately 30% of the rebounded particles at 95% relative humidity were spherical organic particles. Their sources and formation process are not known, but such spherical particles could be solid and will have heterogeneous chemical reactions. We observed many organic particles that are internally mixed with inorganic elements such as potassium and nitrogen. They are either homogeneously mixed or have inorganic cores with organic aerosol coatings. Samples collected from the Manaus, Brazil, pollution plume included many nano-size soot particles mixed with organic material and sulfate. Aerosol particles from clean periods included organic aerosol particles, sulfate, sea salt, dust, and primary biogenic aerosol particles. There was more dust, primary biogenic aerosol, and tar balls in samples taken during IOP1 than those taken during IOP2. Many dust particles were found between March 2 and 3.

spherical organic particles, Manaus pollution plum↗
DOE OSTI2022

An independent analysis of bias sources and variability in wind plant pre-construction energy yield estimation methods

The wind resource assessment community has long had the goal of reducing the bias between wind plant pre-construction energy yield assessment (EYA) and the observed annual energy production (AEP). This comparison is typically made between the 50% probability of exceedance (P50) value of the EYA and the long-term corrected operational AEP (hereafter OA P50), and is known as the P50 bias. The industry has critically lacked an independent analysis of bias reduction investigated across multiple consultants to identify the greatest sources of uncertainty and variance in the EYA process and the best opportunities for uncertainty reduction. The present study addresses this gap by benchmarking consultant methodologies against each other and against operational data at a scale not seen before in industry collaborations. We consider data from 10 wind plants and evaluate discrepancies between eight consultancies in the steps taken from estimates of gross to net energy. Consultants tend to overestimate the gross energy produced at the turbines and then compensate by further overestimating downstream losses, leading to a mean P50 bias near zero, still with significant variability among the individual wind plants. Within our data sample, we find that consultant estimates of all loss categories, except environmental losses, tend to reduce the project-to-project variability of the P50 bias. The disagreement between consultants, however, remains flat throughout the addition of losses. Finally, we find that differences in consultants’ estimates of project performance can lead to differences up to $10/MWh in the levelized cost of energy for a wind plant.

Todd, Austin C.↗
DOE OSTI2015

Timing gamma-ray pulsars with the Fermi large area telescope: Timing noise and astrometry

We have constructed timing solutions for 81 γ-ray pulsars covering more than five years of Fermi data. The sample includes 37 radio-quiet or radio-faint pulsars which cannot be timed with other telescopes. These timing solutions and the corresponding pulse times of arrival are prerequisites for further study, e.g., phase-resolved spectroscopy or searches for mode switches. Many γ-ray pulsars are strongly affected by timing noise (TN), and we present a new method for characterizing the noise process and mitigating its effects on other facets of the timing model. We present an analysis of TN over the population using a new metric for characterizing its strength and spectral shape, namely, its time-domain correlation. The dependence of the strength on ν and ν-dot is in good agreement with previous studies. We find that noise process power spectra S(f) for unrecycled pulsars are steep, with strong correlations over our entire data set and spectral indices S(f)∝f{sup −α} of α ∼ 5–9. One possible explanation for these results is the occurrence of unmodeled, episodic “microglitches.” Finally, we show that our treatment of TN results in robust parameter estimation, and in particular we measure a precise timing position for each pulsar. We extensively validate our results with multi-wavelength astrometry, and using our updated position, we firmly identify the X-ray counterpart of PSR J1418−6058.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2015

Identification and Mitigation of Generated Solid By-Products during Advanced Electrode Materials Processing

A scalable, solid-state elevated temperature process was developed to produce high capacity carbonaceous electrode materials for energy storage devices via decomposition of starch-based precursor in an inert atmosphere. The fabricated carbon-based architectures are useful as an excellent electrode material for lithium-ion, sodium-ion and lithium-sulfur batteries. This article focuses on the study and analysis of the formed nanometer-sized byproducts during the lab-scale production of carbonaceous electrode materials in the process design phase. The complete material production process was studied by operation, namely during heating, holding the reaction at elevated temperature, followed by cooling. The unknown downstream particles in the process exhaust were collected and characterized via aerosol and liquid suspensions, and they were quantified using direct-reading instruments for number and mass concentrations. The airborne emissions were collected on polycarbonate filters and TEM grids using the Tsai diffusion sampler (TDS) for characterization and further analysis. Released byproduct aerosols collected in a deionized (DI) water trap were analyzed using a Nanosight real time nanoparticle characterization system and the aerosols emitted post water suspension were collected and characterized. Individual particles in the nanometer size range were found in exhaust aerosols, however, crystal structured aggregates were formed on the sampling substrate after a long-term sampling of emitted exhaust. After characterizing the released aerosol byproducts, methods were also identified to mitigate possible human and environmental exposures upon the industrial implementation of such a process.

25 ENERGY STORAGE↗
DOE OSTI2025

Machine learning for domain transfer between simulated and experimental 2D X-ray diffraction patterns using generative adversarial networks

X-ray diffraction (XRD) is a well-established technique for analyzing materials at an atomic level. Dynamic compression experiments (DCE), in which materials are subject to extreme pressures, can provide fundamental understanding to pressure-induced phase transitions and compression of the crystal lattice. The analysis of XRD patterns from highly compressed samples is non-trivial given the sparsity of data, high experimental costs, and the fact that the data is often marred with X-ray background and other artifacts. While accurate computational frameworks exist, they solve the forward problem—from structures and orientations to XRD patterns. Solving the inverse problem for 2D experimental diffraction patterns is currently a complex manual process of matching and comparing experimentally observed patterns to computationally generated ones. Machine learning is a promising tool for automating the matching process but often requires data-intensive architectures. Here, in this study, we use a CycleGAN to translate the domain of limited experimental data to a domain in which there is readily available simulated data. This domain shift allows data-intensive machine learning models that have only been trained on simulated XRD patterns to be used in the analysis of experiments.

Brozak, Samantha Jean [Sandia National Laboratorie↗
DOE OSTI2014

Characterization of Used Nuclear Fuel with Multivariate Analysis for Process Monitoring

The Multi-Isotope Process (MIP) Monitor combines gamma spectroscopy and multivariate analysis to detect anomalies in various process streams in a nuclear fuel reprocessing system. Measured spectra are compared to models of nominal behavior at each measurement location to detect unexpected changes in system behavior. In order to improve the accuracy and specificity of process monitoring, fuel characterization may be used to more accurately train subsequent models in a full analysis scheme. This paper presents initial development of a reactor-type classifier that is used to select a reactor-specific partial least squares model to predict fuel burnup. Nuclide activities for prototypic used fuel samples were generated in ORIGEN-ARP and used to investigate techniques to characterize used nuclear fuel in terms of reactor type (pressurized or boiling water reactor) and burnup. A variety of reactor type classification algorithms, including k-nearest neighbors, linear and quadratic discriminant analyses, and support vector machines, were evaluated to differentiate used fuel from pressurized and boiling water reactors. Then, reactor type-specific partial least squares models were developed to predict the burnup of the fuel. Using these reactor type-specific models instead of a model trained for all light water reactors improved the accuracy of burnup predictions. The developed classification and prediction models were combined and applied to a large dataset that included eight fuel assembly designs, two of which were not used in training the models, and spanned the range of the initial 235U enrichment, cooling time, and burnup values expected of future commercial used fuel for reprocessing. Error rates were consistent across the range of considered enrichment, cooling time, and burnup values. Average absolute relative errors in burnup predictions for validation data both within and outside the training space were 0.0574% and 0.0597%, respectively. The errors seen in this work are artificially low, because the models were trained, optimized, and tested on simulated, noise-free data. However, these results indicate that the developed models may generalize well to new data and that the proposed approach constitutes a viable first step in developing a fuel characterization algorithm based on gamma spectra.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2016

Evaluating the lingering effect of livestock grazing on functional potentials of microbial communities in Tibetan grassland soils

Background and aims: Livestock grazing is a widely practiced land-use regime that can impose lingering effects on global biogeochemical cycles. Yet, elucidating the mechanisms of related eco-processes, which are largely mediated by the microbial community, remains challenging. Methods: In this work, we collected soil samples from two Tibetan grassland sites subjected to grazing in winter followed by a 3-month recovery. We then evaluated functional potentials of microbial communities via a metagenomic tool known as GeoChip 4.0. Results: Significant alterations were detected in post-grazing grassland soils, and further analysis showed that plant diversity was the best indicator of alterations in functional potentials. Relative abundances of labile C degradation genes decreased at the 3400-m site, but those of recalcitrant C degradation genes increased, which could be explained by the higher soil recalcitrant C input owing to their being substantially more forbs species at this site. Nitrification genes decreased at both sites, probably owing to increased soil moisture conducive to oxygen-limiting conditions. Relative abundance of denitrification genes increased at the 3200-m site, concomitant with increased N 2 O emissions. Conclusions: These findings demonstrated that functional gene compositions of the microbial community were altered in post-grazing grassland soils, and linked to soil biogeochemical processes.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2018

MicroRNA-21 promotes wound healing via the Smad7-Smad2/3-Elastin pathway

Highlights: • MicroRNA-21 promotes wound healing. • Smad7 is the target of microRNA-21. • MicroRNA-21 promotes wound healing process via targeting TGF-β pathway. Wound healing is regulated by a complex network of cells, molecules, and cytokines, as well as microRNAs (miRNAs). miRNAs were confirmed to influence the wound healing process, and miR-21, an important member of the miRNA family, was also shown to regulate wound healing. The aim of the present study was to investigate the role of miR-21 in the wound healing process and the possible underlying cell signaling pathways. We isolated GMSCs from WT and miR-21-KO mouse gingiva. Flow cytometric analysis and immunocytofluorescense staining were used to identify the GMSCs acquired from WT and miR-21-KO mice. RT-PCR, western blot analysis and immunohistofluorescence staining were performed to examine the expression of extracellular matrix components and key proteins of cell signaling pathways. TargetScan and pmiR-RB-REPORT vectors were used to verify that Smad7 was a direct target of miR-21. Compared to WT mice, miR-21-KO mice showed slower wound healing. RT-PCR and western blot analysis indicated that Elastin expression was downregulated in miR-21-deficient samples. We confirmed that Smad7 was a direct target of miR-21. miR-21 knockout resulted in increased expression of Smad7 and impaired phosphorylation of the Smad2/3 complex. The expression of the Smad7-Smad2/3-Elastin axis in palate tissues sections acquired from WT and miR-21-KO mice showed the same trend. Based on all these results, we demonstrated that miR-21 promoted the wound healing process via the Smad7-Smad2/3-Elastin pathway.

60 APPLIED LIFE SCIENCES↗
DOE OSTI2020

Y-12 Groundwater Protection Program Groundwater and Surface Water Sampling and Analysis Plan (CY 2021)

This plan provides a description of the groundwater and surface water quality monitoring activities planned for calendar year (CY) 2021 at the U.S. Department of Energy Y-12 National Security Complex (Y-12) that will be managed by the Y-12 Groundwater Protection Program (GWPP). Groundwater and surface water monitoring is performed by the GWPP. Groundwater and surface water monitoring will be performed in three hydrogeologic regimes at Y-12: the Bear Creek Hydrogeologic Regime (Bear Creek Regime), the Upper East Fork Poplar Creek Hydrogeologic Regime (East Fork Regime), and the Chestnut Ridge Hydrogeologic Regime (Chestnut Ridge Regime). The Bear Creek and East Fork regimes are located in Bear Creek Valley and the Chestnut Ridge Regime is located south of Y-12. Additional surface water monitoring will be performed north of Pine Ridge along the boundary of the Oak Ridge Reservation. The following sections of this report provide details regarding the CY 2021 groundwater and surface water monitoring activities. Section 2 describes the monitoring locations in each regime and the processes used to select the sampling locations. A description of the field measurements and laboratory analytes is provided in Section 3. Sample collection methods and procedures are described in Section 4, and Section 5 lists the documents cited for more detailed operational and technical information. The narrative sections of the report reference several appendices. Figures (maps and diagrams) and tables (excluding a data summary table presented in Section 4) are in Appendix A and Appendix B, respectively. Groundwater Monitoring Schedules (when issued throughout CY 2021) will be inserted in Appendix C, and addenda to this plan (if issued) will be inserted in Appendix D. Laboratory requirements (bottle lists, holding times, etc.) are provided in Appendix E, and an approved Waste Management Plan is provided in Appendix F. Modifications to the CY 2021 monitoring program may be necessary during implementation. Changes in programmatic requirements may alter the analytes specified for selected monitoring wells or may add or remove wells from the planned monitoring network. Each modification to the monitoring program will be approved by the Y-12 GWPP manager and documented as an addendum to this sampling and analysis plan.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2016

Improved accuracy of quantitative parameter estimates in dynamic contrast-enhanced CT study with low temporal resolution

Purpose: A previously proposed method to reduce radiation dose to patient in dynamic contrast-enhanced (DCE) CT is enhanced by principal component analysis (PCA) filtering which improves the signal-to-noise ratio (SNR) of time-concentration curves in the DCE-CT study. The efficacy of the combined method to maintain the accuracy of kinetic parameter estimates at low temporal resolution is investigated with pixel-by-pixel kinetic analysis of DCE-CT data. Methods: The method is based on DCE-CT scanning performed with low temporal resolution to reduce the radiation dose to the patient. The arterial input function (AIF) with high temporal resolution can be generated with a coarsely sampled AIF through a previously published method of AIF estimation. To increase the SNR of time-concentration curves (tissue curves), first, a region-of-interest is segmented into squares composed of 3 × 3 pixels in size. Subsequently, the PCA filtering combined with a fraction of residual information criterion is applied to all the segmented squares for further improvement of their SNRs. The proposed method was applied to each DCE-CT data set of a cohort of 14 patients at varying levels of down-sampling. The kinetic analyses using the modified Tofts’ model and singular value decomposition method, then, were carried out for each of the down-sampling schemes between the intervals from 2 to 15 s. The results were compared with analyses done with the measured data in high temporal resolution (i.e., original scanning frequency) as the reference. Results: The patients’ AIFs were estimated to high accuracy based on the 11 orthonormal bases of arterial impulse responses established in the previous paper. In addition, noise in the images was effectively reduced by using five principal components of the tissue curves for filtering. Kinetic analyses using the proposed method showed superior results compared to those with down-sampling alone; they were able to maintain the accuracy in the quantitative histogram parameters of volume transfer constant [standard deviation (SD), 98th percentile, and range], rate constant (SD), blood volume fraction (mean, SD, 98th percentile, and range), and blood flow (mean, SD, median, 98th percentile, and range) for sampling intervals between 10 and 15 s. Conclusions: The proposed method of PCA filtering combined with the AIF estimation technique allows low frequency scanning for DCE-CT study to reduce patient radiation dose. The results indicate that the method is useful in pixel-by-pixel kinetic analysis of DCE-CT data for patients with cervical cancer.

61 RADIATION PROTECTION AND DOSIMETRY↗
DOE OSTI2020

Astrophysical Insights into Radial Velocity Jitter from an Analysis of 600 Planet-search Stars

Radial velocity (RV) detection of planets is hampered by astrophysical processes on the surfaces of stars that induce a stochastic signal, or “jitter,” which can drown out or even mimic planetary signals. Here, we empirically and carefully measure the RV jitter of more than 600 stars from the California Planet Search sample on a star by star basis. As part of this process, we explore the activity–RV correlation of stellar cycles and include appendices listing every ostensibly companion-induced signal we removed and every activity cycle we noted. We then use precise stellar properties from Brewer et al. to separate the sample into bins of stellar mass and examine trends with activity and with evolutionary state. We find that RV jitter tracks stellar evolution and that in general, stars evolve through different stages of RV jitter: the jitter in younger stars is driven by magnetic activity, while the jitter in older stars is convectively driven and dominated by granulation and oscillations. We identify the “jitter minimum”—where activity-driven and convectively driven jitter have similar amplitudes—for stars between 0.7 and 1.7 M {sub ⊙} and find that more-massive stars reach this jitter minimum later in their lifetime, in the subgiant or even giant phases. Finally, we comment on how these results can inform future RV efforts, from prioritization of follow-up targets from transit surveys like TESS to target selection of future RV surveys.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2019

The Effect of Zinc on the Structural, Electrical, and Mechanical Properties of YBCO-123 Superconducting Nanoparticles Prepared by an Acetate-Based Sol-Gel Process

In this study, zinc (Zn)-doped YBaCuO (YBCO)-123-based high-temperature superconducting samples were produced using the sol-gel method, which is commonly used for preparing nanosize materials. Zn ions were substituted by Cu ions (YBa{sub 2}Cu{sub 3-x}Zn{sub x}O), and Zn doping effects on structural, electrical, and mechanical properties of the YBCO-123 superconductors were examined in detail. Undoped sample was prepared under same conditions. X-ray diffraction analysis (XRD) was used to determine phase analysis and lattice parameters of the superconducting samples. To analyze the microstructure properties, scanning electron microscope (SEM) measurements were performed. Resistivity and microhardness measurements were also carried out for superconducting and mechanic properties, respectively. Vickers microhardness, young modulus, fracture toughness, and yield strength values of the samples were calculated. Microhardness measurements were analyzed using the Kick’s law, proportional sample resistance (PSR) model, EPD model, the Hays-Kendall (HK) approach, and indentation-induced cracking (IIC) model.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2022

Chemical Cartography with APOGEE: Mapping Disk Populations with a 2-process Model and Residual Abundances

We apply a novel statistical analysis to measurements of 16 elemental abundances in 34,410 Milky Way disk stars from the final data release (DR17) of APOGEE-2. Building on recent work, we fit median abundance ratio trends [X/Mg] versus [Mg/H] with a 2-process model, which decomposes abundance patterns into a "prompt" component tracing core-collapse supernovae and a "delayed" component tracing Type Ia supernovae. For each sample star, we fit the amplitudes of these two components, then compute the residuals Δ[X/H] from this two-parameter fit. The rms residuals range from ~0.01–0.03 dex for the most precisely measured APOGEE abundances to ~0.1 dex for Na, V, and Ce. The correlations of residuals reveal a complex underlying structure, including a correlated element group comprised of Ca, Na, Al, K, Cr, and Ce and a separate group comprised of Ni, V, Mn, and Co. Selecting stars poorly fit by the 2-process model reveals a rich variety of physical outliers and sometimes subtle measurement errors. Residual abundances allow for the comparison of populations controlled for differences in metallicity and [α/Fe]. Relative to the main disk (R = 3–13 kpc), we find nearly identical abundance patterns in the outer disk (R = 15–17 kpc), 0.05–0.2 dex depressions of multiple elements in LMC and Gaia Sausage/Enceladus stars, and wild deviations (0.4–1 dex) of multiple elements in ω Cen. The residual abundance analysis opens new opportunities for discovering chemically distinctive stars and stellar populations, for empirically constraining nucleosynthetic yields, and for testing chemical evolution models that include stochasticity in the production and redistribution of elements.

79 ASTRONOMY AND ASTROPHYSICS↗
DOE OSTI2017

Laser-driven hydrothermal process studied with excimer laser pulses

Previously, we discovered [Mariella et al., J. Appl. Phys. 114, 014904 (2013)] that modest-fluence/modest-intensity 351-nm laser pulses, with insufficient fluence/intensity to ablate rock, mineral, or concrete samples via surface vaporization, still removed the surface material from water-submerged target samples with confinement of the removed material, and then dispersed at least some of the removed material into the water as a long-lived suspension of nanoparticles. We called this new process, which appears to include the generation of larger colorless particles, “laser-driven hydrothermal processing” (LDHP) [Mariella et al., J. Appl. Phys. 114, 014904 (2013)]. Now, we report that we have studied this process using 248-nm and 193-nm laser light on submerged concrete, quartzite, and obsidian, and, even though light at these wavelengths is more strongly absorbed than at 351 nm, we found that the overall efficiency of LDHP, in terms of the mass of the target removed per Joule of laser-pulse energy, is lower with 248-nm and 193-nm laser pulses than with 351-nm laser pulses. Given that stronger absorption creates higher peak surface temperatures for comparable laser fluence and intensity, it was surprising to observe reduced efficiencies for material removal. We also measured the nascent particle-size distributions that LDHP creates in the submerging water and found that they do not display the long tail towards larger particle sizes that we had observed when there had been a multi-week delay between experiments and the date of measuring the size distributions. This is consistent with transient dissolution of the solid surface, followed by diffusion-limited kinetics of nucleation and growth of particles from the resulting thin layer of supersaturated solution at the sample surface.

36 MATERIALS SCIENCE↗
DOE OSTI2013

3D Reconstruction of Biological Organization and Mineralization in Sediment Attached Biofilms During Uranium Bioremediation

Of central interest in this study were microbial communities attached to sediment particles and in associated groundwater. Are the communities similar? What do the organisms look like and how do they associated with each other? Research was conducted on samples collected from the Department of Energy's (DOE) Rifle Integrated Field Research Challenge (IFRC) site in Rifle, Colorado, USA. This site served first as a test case for in situ bioremediation via biostimulation, and more recently as a location for studying the role of microbial communities in the carbon and other linked biogeochemical cycles. We addressed the question of the nature of planktonic to sediment-attached microbial communities using field and laboratory experimental studies with a range of methods that provide 2- and 3-dimensional topological information coupled to information about chemical speciation, organism type, and activity levels. The research leveraged data from metagenomics and proteomics analyses that obtained through parallel work at the Rifle site in the context of the IFRC. In this project we integrated characterization methods with extensive genomic sequence information and associated environmental data to better understand the processes that occur within groundwater and sediment-attached communities. Notable is the range of characterization methods, including scanning transmission x-ray microscopy (STXM), micro-EXAFS/XANES and microdiffraction and 2D and 3D cryo-electron tomographic analysis, and high-resolutino transmission electron microscope (HRTEM) analysis to characterize these natural microbial communities. A cryo-TEM work was unique because samples for electron microscopic characterization were cryo-plunged directly on site immediately after sampling. This step minimizes post-collection alterations, including cell damages and change of redox state. Among many achievements documented in publications listed at the end of this report, we highlight the following: 1) The development of a platform for routine correlative cryogenic microscopy and spectroscopy with samples prepared on-site. 2) The determination of which organisms dominate planktonic and biofilm communities in the subsurface. 3) Identification of microorganism-mineral associations and discovery of a novel mechanism that sustains activity of iron-reducing bacteria. 4) The detection of bacteria from the OP11-OD1-WWE3 (etc.) radiation and elucidation of their remarkable structural organization by cryog-TEM cryo-electron tomograhpy (cryo-ET). 5) Extensive analysis of biofilms and documentation of the association of cells and Se minerals. 6) The comparison of expressed c-type cytochromes between pure cultures of G. bemidjiensis and related field populations, provided insight into possible molecular mechanisms for U(VI) reduction in the aquifer. At least sixteen publications will result from this project (partial support), which provide both graduate student and post doctoral training.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2023

Laser Ablation Plasmas and Spectroscopy for Nuclear Applications

The development of measurement methodologies to detect and monitor nuclear-relevant materials remains a consistent and significant interest across the nuclear energy, nonproliferation, safeguards, and forensics communities. Optical spectroscopy of laser-produced plasmas is becoming an increasingly popular diagnostic technique to measure radiological and nuclear materials in the field without sample preparation, where current capabilities encompass the standoff, isotopically resolved and phase-identifiable (e.g., UO and UO[Formula: see text]) detection of elements across the periodic table. These methods rely on the process of laser ablation (LA), where a high-powered pulsed laser is used to excite a sample (solid, liquid, or gas) into a luminous microplasma that rapidly undergoes de-excitation through the emission of electromagnetic radiation, which serves as a spectroscopic fingerprint for that sample. This review focuses on LA plasmas and spectroscopy for nuclear applications, covering topics from the wide-area environmental sampling and atmospheric sensing of radionuclides to recent implementations of multivariate machine learning methods that work to enable the real-time analysis of spectrochemical measurements with an emphasis on fundamental research and development activities over the past two decades. Background on the physical breakdown mechanisms and interactions of matter with nanosecond and ultrafast laser pulses that lead to the generation of laser-produced microplasmas is provided, followed by a description of the transient spatiotemporal plasma conditions that control the behavior of spectroscopic signatures recorded by analytical methods in atomic and molecular spectroscopy. High-temperature chemical and thermodynamic processes governing reactive LA plasmas are also examined alongside investigations into the condensation pathways of the plasma, which are believed to serve as chemical surrogates for fallout particles formed in nuclear fireballs. Laser-supported absorption waves and laser-induced shockwaves that accompany LA plasmas are also discussed, which could provide insights into atmospheric ionization phenomena from strong shocks following nuclear detonations. Furthermore, the standoff detection of trace radioactive aerosols and fission gases is reviewed in the context of monitoring atmospheric radiation plumes and off-gas streams of molten salt reactors. Finally, concluding remarks will present future outlooks on the role of LA plasma spectroscopy in the nuclear community.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2022

A study of in situ reduction of MoO 3 to MoO 2 by X-ray Photoelectron Spectroscopy

Results from X-ray Photoelectron Spectroscopy (XPS) of molybdenum oxide samples are presented to elucidate how Mo (VI) oxide evolves to Mo (IV) oxide upon heating of a MoO 3 sample. XPS data analysis techniques based on manipulation of spectra treated as vectors are shown and allow insights into intermediate phases of Mo oxide which suggest how the original oxide changes under the influence of heat but also supports an interpretation of as-received tetravalent Mo powders as multivalent materials. In particular, several new spectral components were observed and assigned to the Magnéli phase as well as MoO 3 domains that have been modified by the presence of X-rays or temperature. Finally, these assignments comprise a new method of data processing where sample modification is used to inform XPS data interpretation and differ from previous work where the linear relationship of the binding energy of molybdenum oxides has been used.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2018

Determining Coal Ash Impacts on Radium and Thorium Background Levels in Soil Using Rare Earth Element Analyses - 18604

One challenge at large remediation sites contaminated with radiological materials is differentiating between low-level site-related contamination and NORM. This is because sites contaminated with radiological materials, such as thorium processing and mining and milling facilities, often generate wastes that contain contaminants that are similar to NORM deposits. For sites in urban areas, this issue is further compounded due to the presence of historic industrial fill (historic fill) containing materials such as fly ash, coal ash, and red brick, that exhibit elevated radioactivity levels. These materials often have activity levels near, or even well above, a site's cleanup goal. At a large Superfund Site in the eastern US (Site), many of the suspected Site-related fill areas are commingled with coal and fly ash. As the cleanup criteria for the radionuclides of concern (ROC), radium (Ra) and thorium (Th), is 5 pico-Curies per gram above background, a four-pronged approach was developed to determine if the coal and fly ash are impacting the background levels of the ROCs. This evaluation included a review of boring logs to visually confirm the presence of historic fill, as well as coal fragments and coal ash; a literature review to establish the typical concentrations of Ra and Th found in coal and fly ash from US sources; the use of rare earth analyses to establish chemical signatures for non-Site related historic fill containing coal ash versus Site-related fill; and a quantitative analysis of Site-related data to determine if the radioactivity levels in historic fill containing coal were elevated. Soil samples were collected from two locations at the Site; fill areas containing coal ash that were not suspected to be impacted by Site activities, as well as fill areas containing coal ash that were associated with the former processing facility. These samples were analyzed for rare earth elements (REE), as well as Ra-228 and Th-232 and the ratios of lanthanum, cerium, and neodymium to Ra-228 and Th-232 were established for each sample. Based on a comparison of these data, a strong correlation was established between the rare earth/thorium decay chain ratios and the classification of material as either Site or non-Site related. These data were used to develop a higher background activity for fill areas containing non-Site related NORM. While the cleanup level defined in the Record of Decision remained unchanged, the higher background derived from the fly ash/coal ash material, as identified by REE analyses, resulted in higher project screening levels, which ensured that excavation activities did not 'chase' material that was not Site-related. To date, use of the coal ash background level has saved millions of dollars in cleanup costs since non-Site related contamination is not being remediated. Use of this approach to determine the appropriate background level for a site is relatively straightforward since it relies on visual observation of the soil for coal and fly ash, along with REE analyses, which is an inexpensive, quick, and established analytical method for soil samples. As long as a good rare earth profile of both contaminated and natural (in this case fly ash and coal ash) material can be established, the results can be quite definitive, which could result in significant volume reduction by minimizing the amount of material excavated and disposed of. This will lead to cost and time savings for what could be an otherwise costly and potentially complex excavation. Anyone performing environmental remediation of NORM contaminated sites may benefit from this paper and presentation. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗