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At least 19 records

Ambient ion focusing from a field-free region to a detector: enhanced signal for explosives and drug detection with mass spectrometry

This study demonstrates ion focusing at ambient pressure and increased ion signal by creating a voltage gradient from a field-free region to a detector, thereby improving the detection of chemicals, such as explosives and drugs. At ambient pressure, ion loss and resulting signal reduction pose challenges that limit detection sensitivity in analytical instruments. Techniques to increase sensitivity, such as atmospheric flow tube-mass spectrometry (AFT-MS), extend ion-molecule reaction times but result in significant overall ion loss due to diffusion. Ion manipulation techniques, though challenging at ambient pressure, can mitigate these losses by concentrating ions toward the detector inlet. Using SIMION, ion trajectories were modeled with a voltage gradient applied between a flow tube and a detector, revealing ion focusing at ambient pressure. Experimental verification with an atmospheric flow tube employed both mass spectrometry and Faraday plate detectors to measure ion beam profiles across varying flow rates, tube diameters, and voltage gradients. Application of a voltage gradient effectively directed ions to the axial center of the flow tube, narrowed ion beam width, and increased signal intensity by 5 to 10 times compared to conditions without a voltage gradient. This ion focusing approach shows promise for improving sensitivity in ambient-pressure instruments. This technique has the potential to enhance detection levels in security and forensic applications, with particular benefits for field-portable devices used at checkpoints to identify explosives and drugs.

ambient pressure

Neutron detector development for high-rate neutron reflectometry at the Second Target Station of Oak Ridge National Laboratory

The Second Target Station (STS) at the Oak Ridge National Laboratory Spallation Neutron Source (SNS) is expected to produce a neutron source that is the brightest in the world, having a significantly higher peak brightness compared to the First Target Station (FTS), where the reflectometry instruments already fall short of being able to handle the highest available flux by a factor of ~100. The neutron reflectometers at the SNS FTS are not suitable for the reflectometers planned for the SNS STS because of its unprecedentedly high peak brightness and the already limited capabilities of these instruments at high count rates. Furthermore, the high rate instruments that are now under development are expected to underperform with regard to gamma sensitivity, meaning that signal-to-noise will be reduced and they will be unable to measure weaker reflectance phenomena in the presence of the significant prompt gamma flash at SNS. To address these challenges, we conducted research to advances associated instruments, techniques, and capabilities for the SNS STS reflectometers. More specifically, we investigated the development of a scalable, 2-D positive-sensitive, pixelated, scintillator-based neutron detector module based on a newly developed scintillator. The work has potential for impact on future neutron reflectometry instruments and neutron science performed at the SNS STS. In particular, the improved background rejection capability of the developed detector could extend the available experimental dynamic Q range, allowing it to measure weak reflectance phenomena.

reflectometry, radiation instrumentation, neutron

Demystifying Piecewise and Localized Scatter Correction Methods

Multiplicative scatter is a common source of noise in near-infrared spectroscopy and other related instrumental techniques. A wide variety of methods are commonly used for the correction of multiplicative scatter. However, the majority of such methods assume that the parameters that describe the scatter are constant throughout the measured spectrum, which is often not the case. This work investigates a family of methods that perform scatter correction using local regions of neighboring wavelengths in order to better account for wavelength-dependent scattering. The methods in question are piecewise standard normal variate, localized standard normal variate, piecewise multiplicative scatter correction, and localized multiplicative scatter correction. This work describes the theoretical and algorithmic foundations of the family of local region-based scatter correction methods and compares their application and optimization at a qualitative and quantitative level using several datasets.

NIR spectroscopy

Rare Earth Element Detection and Quantification in Coal and Rock Mineral Matrices

As global demand for rare earth elements (REEs) increases, maintaining the production and supply chain is critical. Technologies capable of being used in the field and in situ in the subsurface for rapid REE detection and quantification facilitates the efficient mining of known resources and exploration of new and unconventional resources. Laser-induced breakdown spectroscopy (LIBS) is a promising technique for rapid elemental analysis both in the laboratory and in the field. Multiple articles have been published evaluating LIBS for detection and quantification of REEs; however, REEs in their natural deposits have not been adequately studied. In this work, detection and quantification of two REEs, La and Nd, have been studied in both synthetic and natural mineral matrices at concentrations relevant to REE extraction. Measurements were performed on REE-containing rock and coal samples (natural and synthetic) utilizing different LIBS instruments and techniques, specifically a commercial benchtop instrument, a custom benchtop instrument (single- and double-pulse modes), and a custom LIBS probe currently being developed for in situ, subsurface, borehole wall detection and quantification of REEs. Plasma expansion, emission intensity, detection limits, and double-pulse signal enhancement were studied. The limits of detection (LOD) were found to be 10/14 ppm for La and 15/25 ppm for Nd in simulated coal/rock matrices in single-pulse mode. Signal enhancement of 3.5 to 6-fold was obtained with double-pulse mode as compared to single-pulse operation.

La detection

Nonintrusive Diagnostic Strategies for Arcjet Stream Characterization

In the previous lecture, the issues related to arcjet flow modeling were introduced, and the limitations of conventional instrumentation in addressing these issues were discussed. The general level of understanding of the arcjet flows was seen to preclude the use of arcjets as aerothermodynamic test facilities beyond the current role in aerothermal material testing, despite their long test duration capability. In this section, the focus will be on new developments in spectroscopic instrumentation and techniques that can be brought to bear on the fundamental problem of arcjet stream characterization. Although a wide selection of arcjet facilities were introduced in the previous section, the discussion of nonintrusive diagnostic instrumentation will be restricted to the large-scale, segmented, constricted-arc heater facilities that are most widely used in thermal protection material testing for aerospace applications. After a brief review of the important features of arcjet flows, the topic of nonintrusive, optical diagnostics is introduced with a discussion of some of the basic aspects of radiative transitions. The lecture is then organized into two sections covering emission measurements and laser-induced fluorescence measurements. Emission measurements are presented next for different regions of arcjet flows, while the fluorescence measurements are presented for the free stream region only. Summaries are given for each of the two main sections, and observations on arcjet characterization by optical diagnostics in general are given at the end.

Douglas G Fletcher

Opportunities to Intercalibrate Radiometric Sensors from International Space Station

Highly accurate measurements of Earth's thermal infrared and reflected solar radiation are required for detecting and predicting long-term climate change. Consideration is given to the concept of using the International Space Station to test instruments and techniques that would eventually be used on a dedicated mission, such as the Climate Absolute Radiance and Refractivity Observatory (CLARREO). In particular, a quantitative investigation is performed to determine whether it is possible to use measurements obtained with a highly accurate (0.3%,with 95%confidence) reflected solar radiation spectrometer to calibrate similar, less accurate instruments in other low Earth orbits. Estimates of numbers of samples useful for intercalibration are made with the aid of yearlong simulations of orbital motion. Results of this study support the conclusion that the International Space Station orbit is ideally suited for the purpose of intercalibration between spaceborne sensors.

Intercalibrate

The Aeolus-Earth DWTS Heliophysics Mission

The Aeolus-Earth Mission (DWTS-Helio) is a recently selected NASA Heliophysics investigation that will apply the innovative Doppler Wind Temperature Sounder (DWTS) technique to the Space Atmosphere Interaction Region (SAIR) at ~105-180 km. The technique, invented by Gordley & Marshall (2011), applies the Doppler Scanning with Gas Filter (DSGF) technique using a cryo-cooled MWIR radiometer to view the limb of the atmosphere from LEO (orbital velocity creates the Doppler shifts required by the technique). For this implementation of DWTS, a Nitric Oxide (NO) low pressure gas cell is used. The limb of the atmosphere is observed from a spacecraft at orbital velocity, and as an observed air volume passes through the field of view, this velocity creates a set of Doppler-shifted images. These images are used to create Doppler Integrated Pass (DIP) signals, from which atmospheric temperature and wind profiles are extracted (it may be considered a converse of the successful in-flight calibration of gas cells used for the HALOE instrument). The technique is relative, removing the need for absolute radiances, and the signal-to-noise ratio for this technique is high, resulting in good measurement precision. Different gas cells can be used to create different altitude coverage and may be combined to measure a more continuous altitude range. For example, using a NO cell captures the lower atmosphere from 30-50km as well as the SAIR, while using the 13 isotopologue of CO2 would capture 50-120km. Due to the desired data volume as well as power and thermal considerations, this initial Aeolus-Earth flight will be more suited for a ‘hosted’ payload on an Orbital Maneuvering Vehicle platform instead of the ‘free-flyer’ option originally investigated. Lastly, the technique is sufficiently powerful that a two-channel system could produce full Mars atmosphere data not currently possible.

DWTS

Spatiotemporal Studies of Soluble Inorganic Nanostructures with X‐rays and Neutrons

This Review addresses the use of X-ray and neutron scattering as well as X-ray absorption to describe how inorganic nanostructured materials assemble, evolve, and function in solution. We first provide an overview of techniques and instrumentation (both large user facilities and benchtop). We review recent studies of soluble inorganic nanostructure assembly, covering the disciplines of materials synthesis, processes in nature, nuclear materials, and the widely applicable fundamental processes of hydrophobic interactions and ion pairing. Reviewed studies cover size regimes and length scales ranging from sub-Ångström (coordination chemistry and ion pairing) to several nanometers (molecular clusters, i.e. polyoxometalates, polyoxocations, and metal-organic polyhedra), to the mesoscale (supramolecular assembly processes). Reviewed studies predominantly exploit 1) SAXS/WAXS/SANS (small- and wide-angle X-ray or neutron scattering), 2) PDF (pair-distribution function analysis of X-ray total scattering), and 3) XANES and EXAFS (X-ray absorption near-edge structure and extended X-ray absorption fine structure, respectively). While the scattering techniques provide structural information, X-ray absorption yields the oxidation state in addition to the local coordination. Our goal for this Review is to provide information and inspiration for the inorganic/materials science communities that may benefit from elucidating the role of solution speciation in natural and synthetic processes.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Micromechanical response of SiC-OPyC layers in TRISO fuel particles

Tristructural isotropic (TRISO)–coated particle fuel is a proposed fuel for multiple advanced reactor concepts. The performance of the particle depends on whether the silicon carbide (SiC) layer remains intact to prevent the release of metallic and gaseous fission products. Mechanical fracture of the SiC layer is a potential failure mode under various fuel configurations and operating environments, including the potential transmission of matrix-originating cracks through TRISO particles. Furthermore, this study uses instrumented indentation techniques on cross-sectioned surrogate particles to examine the mechanical stability of the critical interface between SiC and the outer pyrolytic carbon (OPyC) layer. The observed behavior at the interface is rationalized by examining the radially dependent fracture behavior of the SiC layer and performing a numerical analysis to quantify the residual stresses that develop during the processing and cross-sectioning of the as-fabricated particle. Characterizing the SiC-OPyC interface of surrogate TRISO particles using nanoindentation provides unique insight into the interface's room-temperature residual stress and mechanical stability. The modeling efforts were used to investigate the experimental procedure further, and the results are presented herein to validate this fuel form's potential mechanical failure modes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

A systematic exploration of the hydrolysis products of the uranium trioxide polymorphs and their optical vibrational spectra

Study of the uranium trioxide (UO 3 )-water system is complex with inconclusive results and limited details in the literature. The UO 3 system is home to at least seven structural polymorphs and an amorphous phase. The proposed hydrolysis products of UO 3 are just as numerous, yet investigations of these alteration products are sporadic and generally antiquated, thus requiring systematic investigations. Recent developments in the understanding of UO 3 phase space, aided by improvements in analytical and computational techniques, necessitate more modern investigations into the uranyl hydroxide family and their naturally occurring mineral counterparts. We present findings from a systematic investigation of the products formed via hydrothermal reactions of common UO 3 polymorphs and discuss how the equatorial coordination of the uranyl/uranyl-like ions within the UO 3 precursors leads to differences in the optical vibrational spectra of the resulting hydrolysis products. The hypo-stochiometric nature of α-UO 2 (OH) 2 allows for the formation of multiple unique uranyl sites and a distortion of the unit cell to a lower symmetry. This study provides, for the first time, an analysis of β-UO 2 (OH) 2 using modern techniques and instrumentation (Raman/infrared spectroscopy and powder x-ray diffraction) and lays a foundation for future time-dependent investigations into the structural dependence of the hydrolysis kinetics of the UO 3 phases. In conclusion, given the prevalence of UO 3 at both ends of the nuclear fuel cycle, an understanding of its behavior with water has applications ranging from nuclear forensics to waste management and environmental transport.

Uranium trioxide

Delving into the depths of NGC 3783 with XRISM II. Cross-calibration of X-ray instruments used in the large, multi-mission observational campaign

Context. Accurate X-ray spectroscopic measurements are fundamental for deriving basic physical parameters of the most abundant baryon components in the Universe. The plethora of X-ray observatories currently operational enables a panchromatic view of the high-energy emission of celestial sources. However, uncertainties in the energy-dependent calibration of the instrument transfer functions (e.g. the effective area, energy redistribution, or gain) can limit - and historically, did limit - the accuracy of X-ray spectroscopic measurements. Aims. We revised the status of the cross-calibration among the scientific payload on board four operation missions: Chandra, NuSTAR, XMM-Newton, and the recently launched XRISM. XRISM carries the micro-calorimeter Resolve, which yields the best energy resolution at energies ≥2 keV. For this purpose, we used the data from a 10-day-long observational campaign targeting the nearby active galactic nucleus NGC 3783, carried out in July 2024. Methods. We present a novel model-independent method for assessing the cross-calibration status that is based on a multi-node spline of the spectra with the highest-resolving power (XRISM/Resolve in our campaign). We also estimated the impact of the intrinsic variability of NGC 3783 on the cross-calibration status due to the different time coverages of participating observatories and performed an empirical reassessment of the Resolve throughput at low energies. Results. Based on this analysis, we derived a set of energy-dependent correction factors of the observed responses, enabling a statistically robust analysis of the whole spectral dataset. They will be employed in subsequent papers describing the astrophysical results of the campaign. Aims. We revised the status of the cross-calibration among the scientific payload on board four operation missions: Chandra, NuSTAR, XMM-Newton, and the recently launched XRISM. XRISM carries the micro-calorimeter Resolve, which yields the best energy resolution at energies ≥2 keV. For this purpose, we used the data from a 10-day-long observational campaign targeting the nearby active galactic nucleus NGC 3783, carried out in July 2024. Methods. We present a novel model-independent method for assessing the cross-calibration status that is based on a multi-node spline of the spectra with the highest-resolving power (XRISM/Resolve in our campaign). We also estimated the impact of the intrinsic variability of NGC 3783 on the cross-calibration status due to the different time coverages of participating observatories and performed an empirical reassessment of the Resolve throughput at low energies. Results. Based on this analysis, we derived a set of energy-dependent correction factors of the observed responses, enabling a statistically robust analysis of the whole spectral dataset. They will be employed in subsequent papers describing the astrophysical results of the campaign.

Active Galactic Nuclei, individual: NGC 3783

A Space Servicing Telerobotics Technology Demonstration

Supervised telerobotic controls provide the key to successful remote servicing, as demonstrated in the telerobot testbed of the jet propulsion laboratory. Such advanced techniques and systems are specially applicable to ground-remote operations for servicing tasks, which are to be performed remotely in space and to be operated under human supervision from the ground. Laboratory demonstrations have successfully proven the utility of such techniques and systems. Instrumental to the success of supervised robotic operations are the techniques called object designate and relative target. In addition, a technique called universal camera calibration was also applied in the telerobot testbed. Generalized compliant control techniques were used in the robotic removal and insertion operations. These techniques were proven successful in task situations where preprogrammed automation cannot be adequately exercised due to errors, changes, or omission in the worksite data base.

Edwin P Kan

DICER: A new instrument at LANSCE to constrain neutron capture rates on radionuclides

With very few exceptions, direct measurements of neutron capture rates on radionuclides have not been possible. A number of indirect methods have been pursued such as the surrogate method, the γ-ray strength function method, the Oslo method and the β-Oslo method. Substantial effort has been devoted to quantify the usually large systematic errors that accompany the results from these techniques. A new instrument has been developed at the Los Alamos Neutron Science Center (LANSCE) to provide more accurate data on several radionuclides relevant to nuclear criticality safety, radiochemical diagnostics, astrophysics, nuclear forensics and nuclear security, by measuring the transmission of neutrons through radioactive samples and studying resonance properties. The Device for Indirect Capture on Radionuclides (DICER) and associated radionuclide production at the Isotope Production Facility (IPF), both at LANSCE, as well radioactive sample fabrication, have been under development the last few years. A description of the new apparatus, data on a few mid-weight stable isotopes and efforts on radionuclide measurements will be presented.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

Preface to the Proceedings of the 25th Topical Conference on High-Temperature Plasma Diagnostics

The 25th Topical Conference on High-Temperature Plasma Diagnostics (HTPD 2024) was held in Asheville, NC, USA, at the Renaissance Asheville Downtown Hotel from 21 to 25 April 2024. This biennial conference brings together scientists and engineers from a variety of fields, including magnetic confinement fusion, inertial confinement fusion, space plasmas, astrophysics, and industrial applications, to discuss mutual problems in the development of instrumentation and experimental techniques for the characterization of high-temperature plasmas. As the 25th meeting, HTPD 2024 represents ∼50 years of ongoing international collaboration on these topics.

Biewer, Theodore [ORNL] (ORCID:0000000174563509)

New developments in structure-property and amorphous materials research at the upgraded 16-BM-B Paris-Edinburgh press station at HPCAT

Beamline 16-BM-B of the High-Pressure Collaborative Access Team (HPCAT) at the Advanced Photon Source (APS) provides a Paris-Edinburgh press program to probe the structure and properties of crystalline and amorphous materials up to 12 GPa at room temperature or 7 GPa at 2000°C. During the recent APS upgrade, 16-BM-B undertook major improvements to its instrumentation and measurement techniques. The upgrade includes the addition of a 1.2 m horizontal “condenser” mirror and a new variable-sized collimation system, the combination of which decreases the acquisition time for energy dispersive X-ray diffraction measurements by a factor of 10 when compared to pre-upgrade measurements. The addition of a new Ge energy-sensitive detector and DANTE (XGLab) digital pulse processor allows for processing the increased diffraction counts with minimal deadtime. In addition to upgraded beamline components, new techniques are being developed for eventual release to the user community, including electrical resistivity and tomography measurements.

APS upgrade

Benchtop Autonomous Electrochemical Characterization System for Combinatorial Thin-Film Solid Oxide Electrodes

The design of materials for electrochemical energy conversion is complicated by a vast search space of candidate materials and multifaceted property requirements: multicarrier conductivity, stability, and catalytic activity are all necessary but rarely intersect. Although self-driving laboratories are rapidly rising to address such material optimization problems, the required infrastructure for integrated, large-scale robotic facilities can be cost-prohibitive. Here we develop and evaluate a closed-loop measurement system for efficient screening of proton-conducting oxide electrodes for ceramic fuel cells and electrolyzers, building on top of an existing benchtop instrument and integrating techniques for rapid impedance measurement and automated analysis. This system exemplifies a “minimum viable” self-driving implementation that can deliver substantial benefits with relatively simple infrastructure. Combinatorial thin-film microelectrode libraries are characterized with a recently developed joint time-domain and frequency-domain impedance measurement technique, which provides an order-of-magnitude acceleration relative to conventional impedance spectroscopy. The distribution of relaxation times is extracted from impedance data and analyzed without human intervention. These results feed an active learning and Bayesian optimization process that learns to predict electrochemical impedance as a function of material composition, measurement temperature, oxygen partial pressure, and electrical bias, which further reduces the screening time by tenfold with optimized experimental sequences. We apply this system to Ba⁡(Co,Fe,Zr,Y)⁢O 3−𝛿 combinatorial libraries and evaluate its effectiveness for learning material property trends and optimizing expensive-to-evaluate properties such as activation energy. This offers insights into key methodological aspects of practical autonomous experimentation, including surrogate model validation, cost-aware acquisition functions, and high-throughput data interpretation. Our results demonstrate the efficacy of the system for rapidly gathering information, but also highlight real-world experimental challenges of thin-film degradation and numerical instability in surrogate models.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

A Quantum Leap for Dynamic Radiography

Dynamic radiography techniques have been instrumental in advancing the National Nuclear Security Administration's (NNSA) mission since WWII. This paper explores the transformative potential of quantum information science (QIS) to revolutionize dynamic radiography through enhanced image processing, tomographic reconstruction, statistics and uncertainty quantification (UQ), and artificial intelligence integration. By leveraging quantum algorithms to extract previously inaccessible information from existing datasets, this interdisciplinary approach promises unprecedented insights at the intersection of dynamic imaging, artificial intelligence, and quantum information technologies.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND

Droplet Entrainment in Steam Supply System of Water-Cooled Small Modular Reactors: Experiment and Modeling Approaches

Droplet entrainment in steam-flow is a prominent phenomenon that needs adequate safety and risk analysis of postulated transient and accident scenarios—including experimental investigation and representative modeling and simulation (M&S)—for small modular reactor (SMR) system design and demonstration. This study identifies knowledge gaps by evaluating experimental and computational fluid dynamics modeling approaches to support early-stage reactor system design, testing, and model evaluation. Previous studies reported in the literature for steam-flow entrainment primarily focused on gigawatt capacity pressurized water reactor (PWR) systems. However, entrainment phenomena are even more prominent for PWR-type SMRs due to their more compact integrated designs, which need further research and development. To fill the research gaps, this study provides insight by specifying the phenomena of interest by leveraging the lessons learned from past research, adopting advanced M&S techniques and advanced instrumentation and control. The findings and recommendations are applicable for evaluating steam-flow entrainment models and for designing integral effect test and separate effect test facilities for gaining reactor design approvals.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS