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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Updated uranium reference material 231 Pa/ 235 U consensus model ages for nuclear forensics

Radiochronometry provides the model age of nuclear materials, which is useful for understanding the production history of materials found outside of regulatory control. Certified reference materials (CRMs) are important for radiochronometry to increase confidence in measurement quality; however, the absence of 231 Pa/ 235 U CRMs necessitates that nuclear forensic laboratories measure the 231 Pa/ 235 U model ages of preexisting uranium reference materials. Here, in this work, new consensus 231 Pa/ 235 U model ages are reported from three nuclear forensic laboratories for three reference materials using current analytical methods. These updated consensus values can be used for quality control of 231 Pa/ 235 U model age measurements.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

Sample screening of uranium ore concentrates using portable spectrophotometers: investigating the correlation between visible colors and chemical signatures

A research collaboration between the Japan Atomic Energy Agency and the Department of Energy’s National Nuclear Security Administration examined nuclear forensic signatures and analytical methods for tracing the origins of uranium ore concentrates (UOCs). Here, this study focuses on utilizing portable spectrophotometers capable of reflectance measurements in the visible light spectrum as a potential rapid screening tool for nuclear forensics analysis. Unlike laboratory-based near-infrared spectroscopy or digital image analysis, this research investigated the potential to correlate visible color measurements with key nuclear forensics signatures using seven types of UOC samples with known origins and three UOC certified reference materials. Results demonstrated that distinct color groups, quantified using CIELAB values, correlated with major uranium compounds. Furthermore, the findings indicated that trace elements can influence the UOC colors, providing additional insights into material characteristics. Although this approach requires further validation across a broader range of UOC species, this study demonstrated that simple colorimetric analysis using visible spectrophotometry, which does not require complex sample preparation or data processing, can serve as a practical and novel rapid tool for preliminary screening and attribution in nuclear forensics investigations.

and nuclear chemistry↗
DOE OSTI2019

Influence of argon flow rate on structural and optical properties of transparent Nb{sub 2}O{sub 5} thin films

Transparent niobium pentoxide (Nb{sub 2}O{sub 5}) thin films deposited on glass substrates by RF sputtering at different argon (Ar) flow rate were contrastively studied. Analytical methods such as X-ray fluorescence, Fourier-transform infrared spectroscopy and field emission scanning electron microscope were utilized to investigate the morphological surface and structural properties of Nb{sub 2}O{sub 5} thin films deposited at different Ar flow rate. UV–Vis–NIR and photoluminescence (PL) spectroscopy were used to explore the optical properties of Nb{sub 2}O{sub 5} thin films deposited at different Ar flow rate. The allowed optical band gap (E{sub g}{sup d}) of the Nb{sub 2}O{sub 5} thin films varies from 3.88 to 3.80 eV with increasing Ar flow rate from 30 to 90 sccm. The PL of the Nb{sub 2}O{sub 5} thin films showed strong emission peak around 400 nm. The real values of the refractive index are increase with increasing Ar flow rate. Optical quantities related to the optical constants of Nb{sub 2}O{sub 5} thin films thin films such as single oscillator parameters and third-order nonlinear susceptibility were assessed.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Radial Inertia Effect on Dynamic Compressive Response of Polymeric Foam Materials

Polymeric foams have been extensively used in shock isolation applications because of their superior shock or impact energy absorption capability. However, as a type of soft condensed matter, the highly nonlinear, heterogeneous, and dissipative behavior of polymeric foams may result in an ineffective mitigation or isolation to shock/blast loading. To meet certain desired shock mitigation or isolation requirements, the polymeric foams need to be experimentally characterized to obtain their intrinsic material response. However, radial inertia during dynamic compression has become a severe issue and needs to be fully understood. In this study, we developed an analytical method to calculate the additional stress induced by radial inertia in a polymeric foam specimen. The radial inertia is generally caused by Poisson’s effect and associated with three different mechanisms – axial strain acceleration, large deformation, and Poisson’s ratio change. In conclusion, the effect of Poisson’s ratio change during deformation on radial inertia was specifically investigated for hyperelastic foam materials, and verified with experimental results obtained from Kolsky compression bar tests on a silicone foam.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Evaluation of dried blood spot sampling for verification of exposure to chemical threat agents

Abstract Purpose Exposure to chemical threat agents (CTAs), including nerve agents, the vesicating agent sulfur mustard, and opioids, remains a significant threat to warfighter and civilian populations. Definitive analytical methods to verify exposure to CTAs require shipping refrigerated or frozen biomedical samples to reference laboratories for analysis. Logistical and financial burdens arise as the transport of biomedical samples is subject to strict restrictions and complex packaging, which, if done incorrectly, can lead to sample deterioration. The use of dried blood spot (DBS) sampling could provide operational improvements for collecting, storing, and shipping important forensic samples. Therefore, this effort focuses on developing DBS techniques with Mitra® 30-µL volumetric absorptive microsampling (VAMS®) devices for use in CTA exposure verification. Methods VAMS® devices were loaded and dried with human whole blood that was exposed to the metabolites pinacolyl methylphosphonic acid (PMPA), ethyl methylphosphonic acid (EMPA), 1,1’sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE), norfentanyl, norcarfentanil, norsufentanil, and norlofentanil. Following extraction from the VAMS® devices, metabolites were detected using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The methods were validated for performance by assessing sensitivity, precision, accuracy, and recovery. Results These methods were sensitive to 1 ng/mL for SBMSE, 0.5 ng/mL for PMPA, EMPA, and norfentanyl; 0.1 ng/mL for norlofentanil, and 0.05 ng/mL for norsufentanil and norcarfentanil. All methods met acceptable precision and accuracy criteria with favorable recovery. Conclusions These results demonstrated the utility of VAMS® in stabilizing human whole blood and show promise as an improved collection method for verification of exposure to various CTAs.

Toxicology↗
DOE OSTI2021

Long-Term Creep-Rupture Behavior of Alloy Inconel 740/740H

To explore potential application of Ni-based alloys for power generation at the higher temperatures and pressures needed to achieve high thermal to electrical-energy conversion efficiency, an extensive creep-rupture dataset covering up to 875 °C and almost 70,000 h for Inconel 740/740H was analyzed using Larson–Miller parameter and Wilshire approaches. The results were used to assess the relative effectiveness of the two analytical methods, both in describing the experimental data and, because of the breadth of the dataset, using analyses of its shorter-time data to make creep lifetime predictions for much more extended times, which were then directly compared to the measured rupture times. The respective methods were also used to predict creep-limited lifetimes relevant to power production (that is, 100,000 h or greater). Despite the complexity of the precipitation-strengthened Inconel 740/740H alloy and the generalized parametric approach of these methodologies, the predictions based on such were reasonably accurate when the entire dataset was analyzed. However, when the analysis was confined to only data for conditions yielding creep-rupture times < 5,000 h( about 65 % of the entire dataset), the Wilshire correlation yielded better prediction for longer time lifetimes due to the inherent instability of the specific Larson–Miller formalism used in this analysis when extrapolated significantly outside its analysis range.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Deformational Features and Microstructure Evolution of Copper Fabricated by a Single Pass of the Elliptical Cross-Section Spiral Equal-Channel Extrusion (ECSEE) Process

The objectives of this work are to study the deformational feature, textures, microstructures, and dislocation configurations of ultrafine-grained copper processed by the process of elliptical cross-section spiral equal-channel extrusion (ECSEE). The deformation patterns of simple shear and pure shear in the ECSEE process were evaluated with the analytical method of geometric strain. The influence of the main technical parameters of ECSEE die on the effective strain distribution on the surface of ECSEE-fabricated samples was examined by the finite element simulation. The high friction factor could improve the effective strain accumulation of material deformation. Moreover, the pure copper sample fabricated by ECSEE ion shows a strong rotated cube shear texture. The refining mechanism of the dislocation deformation is dominant in copper processed by a single pass of ECSEE. The inhomogeneity of the micro-hardness distribution on the longitudinal section of the ECSEE-fabricated sample is consistent with the strain and microstructure distribution features.

36 MATERIALS SCIENCE↗
DOE OSTI2019

Corrosion Fatigue Behaviors of Type 316 LN Cold-Worked Stainless Steels in Acidified Chloride Environment

The effect of cold work (CW) on the microstructure and corrosion fatigue (CF) resistance of 316 LN stainless steel (SS) using microscopic, electrochemical and surface analytical methods was investigated. The CF resistance increases with CW. The fractographs revealed that the crack growth zone was minimum for the base metal as compared to CW SS. Fatigue-tested sample revealed a slip offset was high for as-received, while not much significant difference for 5 and 20% CW SS at low mean stress levels. The presence of NH{sub 4} improved passivity by the formation of nitrate ions that inhibits anodic dissolution.

36 MATERIALS SCIENCE↗
DOE OSTI2013

High-Definition Differential Ion Mobility Spectrometry with Resolving Power up to 500

As the resolution of analytical methods improve, further progress tends to be increasingly limited by instrumental parameter instabilities that could be ignored before. This is now the case with differential ion mobility spectrometry (FAIMS), where fluctuations of the voltages and gas pressure have become critical. A new high-definition generator for FAIMS compensation voltage reported here provides a stable and accurate output than can be scanned with negligible steps. This reduces the spectral drift and peak width, thus improving the resolving power (R) and resolution. The gain for multiply-charged peptides that have narrowest peaks is up to ~40%, and R ~ 400 - 500 is achievable using He/N2 or H2/N2 gas mixtures.

Environmental Molecular Sciences Laboratory↗
DOE OSTI2019

Computational Removal of Undesired Mass Spectral Features Possessing Repeat Units via a Kendrick Mass Filter

Polymers are a common component of chemical background which complicates data analysis and can impair interpretation. Undesired chemical background cannot always be addressed via pre-analytical methods, chromatography, or existing data processing methods. The Kendrick mass filter (KMF) is presented for the computational removal of undesired signals present in MS{sup 1} spectra. The KMF is analogous to mass defect filtering but utilizes homology information via Kendrick mass scaling in combination with chromatographic retention time and the number of observed signals. The KMF is intended to assist in situations in which current data processing methods to remove background, e.g., blank subtraction, are either not possible or effective. The major parameters affecting KMF were investigated using PEG 400 and NIST standard reference material 1950 (metabolites in human plasma). Further exploration of the KMF performance was tested using an extract of a swab known to contain polymers. An illustrative real-world example of skin analysis with polymeric signal is discussed. The KMF is also able to provide a high-level view of the compositionality of data regarding the presence of signals with repeat units and indicate the presence of different polymers. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗
DOE OSTI2017

A HISTORICAL PERSPECTIVE OF NUCLEAR THERMAL HYDRAULICS

The nuclear thermal-hydraulics discipline was developed following the needs for nuclear power plants (NPPs) and, to a more limited extent, research reactors (RR) design and safety. As in all other fields where analytical methods are involved, nuclear thermal-hydraulics took benefit of the development of computers. Thermodynamics, rather than fluid dynamics, is at the basis of the development of nuclear thermal-hydraulics together with the experiments in complex two-phase situations, namely, geometry, high thermal density, and pressure.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2017

Understanding the Performance of Automotive Catalysts via Spatial Resolution of Reactions inside Honeycomb Monoliths

By directly resolving spatial and temporal species distributions within operating honeycomb monolith catalysts, spatially resolved capillary inlet mass spectrometry (SpaciMS) provides a uniquely enabling perspective for advancing automotive catalysis. Specifically, the ability to follow the spatiotemporal evolution of reactions throughout the catalyst is a significant advantage over inlet-and-effluent-limited analysis. Intracatalyst resolution elucidates numerous catalyst details including the network and sequence of reactions, clarifying reaction pathways; the relative rates of different reactions and impacts of operating conditions and catalyst state; and reaction dynamics and intermediate species that exist only within the catalyst. These details provide a better understanding of how the catalyst functions and have basic and practical benefits; e.g., catalyst system design; strategies for on-road catalyst state assessment, control, and on-board diagnostics; and creating robust and accurate predictive catalyst models. Moreover, such spatiotemporally distributed data provide for critical model assessment, and identification of improvement opportunities that might not be apparent from effluent assessment; i.e., while an incorrectly formulated model may provide correct effluent predictions, one that can accurately predict the spatiotemporal evolution of reactions along the catalyst channels will be more robust, accurate, and reliable. In such ways, intracatalyst diagnostics comprehensively enable improved design and development tools, and faster and lower-cost development of more efficient and durable automotive catalyst systems. Beyond these direct contributions, SpaciMS has spawned and been applied to enable other analytical techniques for resolving transient distributed intracatalyst performance. This chapter focuses on SpaciMS applications and associated catalyst insights and improvements, with specific sections related to lean NOx traps, selective catalytic reduction catalysts, oxidation catalysts, and particulate filters. The objective is to promote broader use and development of intracatalyst analytical methods, and thereby expand the insights resulting from this detailed perspective for advancing automotive catalyst technologies.

Partridge Jr, William↗
DOE OSTI2017

Tailoring the response of Autonomous Reactivity Control (ARC) systems

The Autonomous Reactivity Control (ARC) system was developed to ensure inherent safety of Generation IV reactors while having a minimal impact on reactor performance and economic viability. In this study we present the transient response of fast reactor cores to postulated accident scenarios with and without ARC systems installed. Using a combination of analytical methods and numerical simulation, the principles of ARC system design that assure stability and avoids oscillatory behavior have been identified. A comprehensive transient analysis study for ARC-equipped cores, including a series of Unprotected Loss of Flow (ULOF) and Unprotected Loss of Heat Sink (ULOHS) simulations, were performed for Argonne National Laboratory (ANL) Advanced Burner Reactor (ABR) designs. With carefully designed ARC-systems installed in the fuel assemblies, the cores exhibit a smooth non-oscillatory transition to stabilization at acceptable temperatures following all postulated transients. To avoid oscillations in power and temperature, the reactivity introduced per degree of temperature change in the ARC system needs to be kept below a certain threshold the value of which is system dependent, the temperature span of actuation needs to be as large as possible.

ARC↗
DOE OSTI2019

Black holes with MDRs and Bekenstein–Hawking and Perelman entropies for Finsler–Lagrange–Hamilton Spaces

New geometric and analytic methods for generating exact and parametric solutions in generalized Einstein–Finsler like gravity theories and nonholonomic Ricci soliton models are reviewed and developed. We show how generalizations of the Schwarzschild–(anti) de Sitter metric can be constructed for modified gravity theories with arbitrary modified dispersion relations, MDRs, and Lorentz invariance violations, LIVs. Such theories can be geometrized on cotangent Lorentz bundles (phase spaces) as models of relativistic Finsler–Lagrange–Hamilton spaces. There are considered two general classes of solutions for gravitational stationary vacuum phase space configurations and nontrivial (effective) matter sources or cosmological constants. Such solutions describe nonholonomic deformations of conventional higher dimension black hole, BH, solutions with general dependence on effective four dimensional, 4-d, momentum type variables. For the first class, we study physical properties of Tangherlini like BHs in phase spaces with generic dependence on an energy coordinate/parameter. We investigate also BH configurations on base spacetime and in curved cofiber spaces when the BH mass and the maximal speed of light determine naturally a cofiber horizon. For the second class, the solutions are constructed with Killing symmetry on an energy type coordinate. There are analyzed the conditions when generalizations of Bekenstein–Hawking entropy (for solutions with conventional horizons) and/or Grigory Perelman’s W-entropy (for more general generic off-diagonal solutions) can be defined for phase space stationary configurations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2017

Feasibility study of offshore wind turbines with hybrid monopile foundation based on centrifuge modeling

The support structure of an offshore wind turbine (OWT) accounts for up to 25% of the capital cost; therefore, investigations into reliable and efficient foundations are critical for the offshore wind turbine industry. This paper describes an innovative hybrid monopile foundation for OWTs, which is an optimization of the original monopile foundation with broader applications. The behavior of OWTs with the hybrid monopile foundation in service conditions are investigated under lateral cyclic loadings, by considering the effects of wind, waves, and ice. A series of centrifuge tests are conducted in order to analyze these behaviors in detail, and OWT models with the original single-pile as well as wheel-only foundations are tested for comparison. Based on these tests, the accumulated lateral displacement and stiffness during cyclic loadings are presented, and the results indicate that the hybrid foundation exhibits a larger cyclic capacity than the other foundations. The influence of the cycle numbers, cyclic loading characteristics, and soil properties is examined during the tests; furthermore, the effects of these factors on the model deformation responses are illustrated. This study proposes the first analytical method for quantitatively estimating the cyclic lateral displacement of the new hybrid foundation in service conditions, and a degradation coefficient is recommended based on the test results. This method aims to provide a simple approach to predicting responses of OWTs with hybrid monopile foundations in service conditions.

17 WIND ENERGY↗
DOE OSTI2025

Comparison of measurement techniques and sorption of radium-226 in low and high salinity aqueous samples

Human activities have the potential to redistribute radium (Ra) in the marine environment in a manner that may necessitate monitoring or management of subsequent human or environmental exposures. There is therefore a need to identify accurate and accessible techniques for Ra measurement in high salinity samples and to describe the distribution of Ra in estuarine and marine environments, but most efforts in these areas have focused on low salinity matrices. In addition, rapid and reliable measurements are crucial for time-sensitive samples such as short-lived isotopes or emergency situations. The objective of this study is to describe the limits of detection, cost, and relative ease for measurement of Ra in both low and high salinity aqueous samples via three analytical methods: liquid scintillation counting (LSC), high purity germanium (HPGe) gamma spectrometry, and inductively coupled plasma mass spectrometry (ICP-MS). To contextualize these measurements for real-world scenarios, the partitioning of 226 Ra to substrates relevant to the marine environment was also characterized. Although HPGe detection with solid phase extraction had the lowest limit of detection for low salinity samples (0.27 Bq L −1 ), poor 226 Ra recovery for high salinity samples and high materials costs make this method prohibitive for many users. Limits of detection for high salinity samples were lower for LSC (1.28 Bq L −1 ) than for ICP-MS without dilution (11.4 Bq L −1 ), but significant and unexpected degradation of the high salinity LSC standards was observed after six months. Furthermore, our preferred measurement method for high salinity Ra samples is ICP-MS with sample dilution as necessary to reduce matrix effects.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2025

A worldwide aerosol phenomenology: Elemental and organic carbon in PM 2.5 and PM 10

Elemental carbon (EC), organic carbon (OC), and particulate matter (PM) concentrations in the inhalable (PM 10 ) and fine (PM 2.5 ) size fractions are measured worldwide, albeit with different analytical methods. These measurements from many researchers were collected and analyzed for Africa, America, Asia, and Europe for 2012–2019. EC/PM, OC/PM, and OC/EC ratios were examined based on region, site type, and season to infer potential sources and impacts. These analyses demonstrate that carbonaceous materials are important PM constituents throughout the world. Mean EC/PM ratios were lowest in PM 10 in Sahelian Africa and Europe (∼0.01), highest (>0.07) in PM 2.5 at urban sites in North America, South America, and Japan. Mean OC/PM ratios were lowest in PM 10 in the Sahel (∼0.06) and in PM 2.5 in China and Thailand (0.10), and highest in central and eastern Europe (∼0.3) and North America (∼0.4). OC/EC ratios were elevated in western and northern Europe, and at regional background sites in North America. EC/PM increased with PM 10 in Thailand, while OC/PM increased with higher PM mass in Thailand, India, and North America, highlighting the specific contribution of carbonaceous aerosols to PM pollution in these regions. At European and North American background sites, OC/EC ratios increased with PM mass. Higher OC/EC ratios in dry periods indicate influence of wildfires, prescribed burns, and secondary aerosol formation. Elevated wintertime EC/PM ratios coincide with residential heating in temperate climate zones.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2017

One-step construction of a molybdenum disulfide/multi-walled carbon nanotubes/polypyrrole nanocomposite biosensor for the ex-vivo detection of dopamine in mouse brain tissue

Highlights: • Ex vivo dopamine detection in mouse brain tissues of Parkinson's disease model. • Nanocomposite constructed by one-step electrochemical approach. • The synergetic performance enhancement of the sensor by nanocomposite. We developed a new strategy for construction of a biosensor for the neurotransmitter dopamine. The biosensor was constructed by one-step electrochemical deposition of a nanocomposite in aqueous solution at pH 7.0, consisting of molybdenum disulfide, multi-walled carbon nanotubes, and polypyrrole. A series of analytical methods was performed to investigate the surface characteristics and the improved electrocatalytic effect of the nanocomposite, including cyclic voltammetry, electrochemical impedance spectroscopy, field-emission scanning electron microscopy, atomic force microscopy, and Raman spectroscopy. The constructed biosensor showed high sensitivity (1.130 μAμM{sup −1}cm{sup −2}) with a dynamic linearity range of 25–1000 nM and a detection limit of 10 nM. Additionally, the designed sensor exhibited strong anti-interference ability and satisfactory reproducibility. The practical application of the sensor was manifested for the ex vivo determination of dopamine neurotransmitters using brain tissue samples of a mouse Parkinson's disease model.

60 APPLIED LIFE SCIENCES↗