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DOE OSTI2025

Unraveling Dimensional Tuning: From 2D to 3D in Covalent Organic Frameworks for Enhanced 2e – Oxygen Reduction Reaction

Covalent organic frameworks (COFs) with a two-dimensional (2D) topology have recently emerged as promising catalyst systems for the electrosynthesis of hydrogen peroxide (H 2 O 2 ) from oxygen (O 2 ). However, designing 2D catalysts to achieve higher H 2 O 2 selectivity presents a significant challenge because of the extensive layer stacking and the aggregated active sites located in the basal planes. It results in lower atom utilization, which requires attention. In this study, we present two functionally similar COFs: one with a 2D rhombus topology (2D@BT_TPA-COF) and another with a three-dimensional (3D) noninterpenetrated pts topology (3D@BT_TPA-COF). Both COFs were utilized for the 2e – oxygen reduction reaction (2e – ORR). Tunning the dimensionality from 2D to 3D resulted in an increase in H 2 O 2 selectivity from approximately ~56% to approximately ~96% (at 0.4 V) and a rise in the turnover frequency (TOF) from 0.05 to 0.08 s –1 at 0.3 V. Nonaggregated active site distribution over 3D topology, featuring higher active site exposure, provides better access to the O 2 /electrolyte and facilitates electron transfer leading to higher 2e – ORR activity and selectivity compared to the 2D counterpart.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Esterification of 3-quinuclidinol, a marker for the incapacitant BZ, for analysis by EI-GC-MS in OPCW test matrices

The analysis by EI-GC-MS of 3-quinuclidinol (3Q), a marker for the riot control and incapacitating agent quinuclinidyl benzilate (BZ), using several, new acylation strategies is described. After evaluating and optimizing conditions for the acylations, these were tested on their ability to successfully derivatize 3Q in three different matrices featured in the 44th Organisation for the Prohibition of Chemical Weapons (OPCW) proficiency test (PT). As 3Q is a highly polar compound, the work here describes acylation strategies that generate 3Q analogs with superior gas chromatographic profiles relative to the underivatized material. The acyl groups studied in this work included acetyl, benzoyl, pentafluorobenzoyl and the bis(3,5-trifluoromethyl)benzoyl. The acylated 3Q products provide sharp, detectable peaks with significantly different retention times from that of the unmodified 3Q. Thus, the retention times for acetyl-, benzoyl-, pentafluorobenzoyl- and 3,5-bis(trifluoromethyl)benzoyl-3Q were determined to be 15.9, 24.9, 22.8 and 22.1 min respectively, in stark contrast to the unmodified 3Q which provides a sharp peak with a retention time centered at ~ 13.5 min only at high concentrations (> 10 µg/mL or µg/g) while a broad peak (RT ~ 15–15.5 min) at low concentrations (< 5 µg/mL or µg/g). The developed protocol was used to derivatize 3Q in three separate matrices. The first two matrices were liquid samples featured during the 44th OPCW PT at two separate concentrations in each (5 and 50 µg/mL). The last matrix was a soil sample featured in the same 44th OPCW PT wherein the 3Q had been spiked at a 12 µg/g concentration. The approach involves the extraction of 3Q from all matrices followed by its acylation resulting in a second reportable analytical method for an OPCW PT. The presented derivatization strategies should find wide applicability particularly in laboratories involved with the analysis of this chemical weapon agent degradation product and those participating in the yearly OPCW PTs.

3-quinuclidinol↗

DOE OSTI2024

Photodetachment photoelectron spectroscopy shows isomer-specific proton-coupled electron transfer reactions in phenolic nitrate complexes

The oxidation of phenolic compounds is one of the most important reactions prevalent in various biological processes, often explicitly coupled with proton transfers (PTs). Quantitative descriptions and molecular-level understanding of these proton-coupled electron transfer (PCET) reactions have been challenging. This work reports a direct observation of PCET in photodetachment (PD) photoelectron spectroscopy (PES) of hydrogen-bonded phenolic (ArOH) nitrate (NO 3 - ) complexes, in which a much slower rising edge provides a spectroscopic signature to evidence PCET. Electronic structure calculations unveil the PCET processes to be isomer-specific, occurred only in those with their HOMOs localized on ArOH, leading to charge-separated transient states ArOH •+ ·NO 3 - triggered by ionizing phenols while simultaneously promoting PT from ArOH •+ to NO 3 - . Importantly, this study showcases that gas-phase PD-PES is a generic means enabling to identify PCET reactions with explicit structural and binding information.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Finite Bubble Statistics Constrain Late Cosmological Phase Transitions

We consider first order cosmological phase transitions (PTs) happening at late times below standard model temperatures T PT ≲ GeV. The inherently stochastic nature of bubble nucleation and the finite number of bubbles associated with a late-time PT lead to superhorizon fluctuations in the PT completion time. We compute how such fluctuations eventually source curvature fluctuations with universal properties, independent of the microphysics of the PT dynamics. Using cosmic microwave background (CMB) and large scale structure measurements, we constrain the energy released in a dark-sector PT. For 0.1 eV ≲ T PT ≲ keV this constraint is stronger than both the current bound from additional neutrino species Δ⁢N eff , and in some cases, even CMB-S4 projections. Future measurements of CMB spectral distortions and pulsar timing arrays will also provide competitive sensitivity for keV ≲ T PT ≲ GeV.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2025

Medium Voltage Testbed for Comparing Advanced Power Line Sensors vs. Transformers with Electrical Grid Events

Electrical utilities have relied upon potential transformers (PTs) and current transformers (CTs) for very accurate metering and to provide reliable signals for protective relays. These devices measure phase voltages and currents and are commissioned by electrical engineers. PTs/CTs can detect and react to various electrical anomalies that could adversely affect electrical grid operations. Less expensive alternative sensing technologies offer the possibility of wider deployment, particularly in grids that employ distributed energy resources. In this work, the performance of an advanced medium-voltage sensor is compared with that of a reference PT and a CT and experimentally evaluated for different power grid scenarios on an advanced outdoor power line sensor testbed at the U.S. Department of Energy’s Oak Ridge National Laboratory. The sensor is based on a capacitive divider for voltage monitoring and a Rogowski coil with an integrator for current monitoring. This study simulated a power grid model based on a utility circuit at the Riverside EPB of Chattanooga. The simulation circuit was created with MATLAB/Simulink software and was integrated into an RT-LAB project to run with the OP4510 real-time simulator at the OPLST. During the tests, the real-time simulations were run for 40 s, and the signal to record the test event with the power meter was set at 30 s for the event-trigger circuit. The advanced outdoor power line sensor testbed has a real-time simulator that is used to generate transient scenarios (e.g., electrical faults, capacitor bank operation, and service restoration), while the analog signals are recorded by the same high-resolution power meter. The behaviors of analog signals, harmonic components, total harmonic distortion, and crest factors are assessed for this power line sensor and compared with those of the reference PT/CT because of the absence of testing standards for advanced outdoor power line sensors. The results showed that this OPLS technology responded identically to the PT and CT under all conditions.

Piesciorovsky, Emilio [ORNL]↗

NASA NTRS1978

SEC sensor parametric test and evaluation system

This system provides the necessary automated hardware required to carry out, in conjunction with the existing 70 mm SEC television camera, the sensor evaluation tests which are described in detail. The Parametric Test Set (PTS) was completed and is used in a semiautomatic data acquisition and control mode to test the development of the 70 mm SEC sensor, WX 32193. Data analysis of raw data is performed on the Princeton IBM 360-91 computer.

Source record↗

NASA NTRS1993

Ti-bearing oxide minerals in lunar meteorite Y793169 with the VLT affinity

Lunar meteorite, Yamato 793169 previously classified as a VLT mare basalt contains considerable amounts of Ti-bearing oxides in the mesostasis area (2 vol. percent). Mineralogical study of these oxides revealed that they are isolated grains of ilmenite, ulvospinel and chromite, which are formed at the last stage of crystallization. Ti/(Ti+Al+Cr) and Cr/(Cr+Al) versus Fe/(Mg+Fe) variations of these phases are not in the same trends as in the low Ti pigeonite basalts of Apollo 12 and 15 in spite of its higher TiO2 contents. Among four lunar meteorites proposed to be samples of mare regions of the Moon, EET87521 and Y793274 are breccias rich in lunar mare components, but Y793169 and A881757 are crystalline rocks composed of Fe-rich pigeonite and plagioclase with affinity to the VLT basalts, despite their higher bulk TiO2 contents than the limit for VLT. Polished think sections (PTS) Y793169,51-3 and A881757,51-4 (Asuka-31) supplied by the National Institute of Polar Research (NIPR) were investigated. Both samples were allocated as parts of two consortium studies. Mineral chemistries and textures were examined by an electron probe micro-analyzer (EPMA) and scanning electron microscope (SEM), JEOL 840A with X-ray chemical map analysis (CMA) utilities. Modal abundances of minerals in Y793169 were obtained from colored backscattered electron (BSE) image of SEM for a particular mineral by a computer and by point analysis for minerals with a similar BSE intensity.

Takeda, Hiroshi↗

NASA NTRS1994

Inhomogeneous distribution of materials in lodranites-acapulcoites and IAB irons and their common formation processes

The two-dimensional chemical mapping analysis (CMA) techniques of EPMA and XRF were applied to a new polished thin section (PTS) of EET84302,28, Acapulco and a 5x3 cm slice of Caddo County to find heterogeneous regional distribution of low temperature fractions in the lodranite-acapulcoite groups and silicate inclusions in the IAB irons. A region richer in metal-plagioclase was found in EET84302,28 and Caddo County. The mineralogy of EET84302,28 is not much different from coarse-grained, metal-rich acapulcoite-like mineral assemblage in EET84302,19, which has chromite-orthopyroxene segregation. Nearly uniform Mg/Fe ratios of silicates modified by reduction at regional oxygen fugacity and large difference in modal abundances of minerals in this meteorite group can be explained by regional concentration of materials when the source materials were partly melted.

Takeda, Hiroshi↗

NASA NTRS1995

Development of a Deltoid Shoulder Muscle Model for Rhesus Monkey Spaceflight Studies

The acromiodeltoid shoulder muscle was demonstrated to be a suitable model for spaceflight studies. The muscle contains a mixture of fast and slow fibers, permitting analysis of muscle fiber type specific changes. Two biopsy sites per muscle were identified that provided samples not degraded by the biopsy procedure. Both sites contained sufficient numbers fibers for determining changes in fiber type percentages and size. There was adequate bilateral symmetry regarding fiber type composition in the left and right muscles such that a total of four times points can be compared. The ESOP cage did not cause atrophy of deltoid muscle fibers; this means that microgravity-induced atrophy should be detectable. As expected, muscle excision stimulated muscle IgM and IgG muscle autoantibody production. Nonrestrained control animals suppressed this response whereas restrained monkeys showed an abnormally pronounced response indicative a compromised immune system. The presence of ESOP cage-induced changes in the immune response may mask spaceflight-induced effects. The ESOP cage modified the dominant hand operation of the PTS. These results demonstrate the importance of high fidelity ground based controls.

Riley, Danny A.↗

NASA NTRS1999

Petrology and Geochemistry of a Mg- and Al-Rich Orthopyroxenite Xenolith in the EETA79001 Shergottite: Implications for Mars Crustal Evolution

EETA79001 is a Mars meteorite (SNC) consisting of multiple rock types, including two basalt types, olivine and pyroxene xenocrysts, and ultramafic xenoliths. This study is focused on the petrology and geochemistry of one orthopyroxenite xenolith in PTS 68, designated X-1. It consists of chemically homogeneous orthopyroxene cores with exceptionally high Mg/Fe (mg#=85) and Al. Cores are permeated by minute high-Si+Al glassy inclusions, some with augite microlites. Magnesian core areas are mantled by more Fe-rich orthopyroxene rims grading to pigeonite away from cores. The xenolith is transected by cross-cutting shear planes, some of pre-incorporation origin. Major and minor element composition and variation suggest that core areas are primarily igneous, crystallized from a high temperature mafic melt. However, nearly constant mg# across cores suggest metamorphic equilibration. Si+Al inclusions may result from, among other processes, exsolution of feldspathic material during subsolidus cooling, or may be solid materials (alkali feldspar) poikilitically enclosed by growing igneous orthopyroxene crystals. Late reaction with more fractionated melts produced Fe-rich mantles, the whole assemblage later cut by tectonic micro-shear planes. Raw electron microprobe data produced during this study are available on request from the author.

Berkley, John L.↗

NASA NTRS2005

Mineralogy and Petrology of New Antarctic Nakhlite MIL 03346

Among the approx.1300 meteorites returned from Antarctica by the 2003-2004 ANSMET expedition was a 715g nakhlite, MIL 03346, recovered from the Miller Range. Samples of this meteorite were distributed to investigators on December 16, 2004. We were allocated PTS MIL 03346,63,100. This abstract is our preliminary report on the mineralogy and petrology of this important new sample.

McKay, G.↗

NASA NTRS2001

Acoustic Issues in Human Spaceflight

NASA is concerned about acute effect of sound on crew performance on International Space Station (ISS), and is developing strategies to assess and reduce acute, chronic, and delayed effects of sound. High noise levels can cause headaches, irritation, fatigue, impaired sleep, headache, and tinnitus and have resulted in an inability to hear alarms. Speech intelligibility may be more impaired for crew understanding non-native language in a noisy environment. No hearing loss occurred, but significant effects on crew performance and communication occurred. Permanent Threshold Shifts (PTS) have not been observed in the US shuttle program. Russian specification for noise in spacecraft is 60 dBA (awake) and 50 dBA (asleep) while the U.S. noise specification on ISS is NC 50 (awake) and NC 40 (asleep) with a 85 dBA hazard limit. Background noise levels of ISS modules have measured 56-69 dBA. Treadmill exercise operations measure 77 dBA. Alarms are required to be 20 dBA above ambient. Hearing protection is recommended when noise exceeds 60 dB 24 hour Leq. Countermeasures include hearing protection and design/ engineering controls. Advanced composite materials with excellent low frequency attenuation properties could be applied as a barrier protection around noisy equipment, or used on personal protective equipment worn by the crew. Hearing protection countermeasures include foam ear inserts, passive muff headsets, and active noise reduction headsets. Oto-acoustic emissions (OAE) could be used to monitor effectiveness of hearing protection countermeasures and tailor hearing protection countermeasures to individual crewmembers. Micro-gravity, vibration, toxic fumes, air quality/composition, stress, temperature, physical exertion or some combination of the above factors may have interacted with moderate long-term noise exposure to cause significant hearing loss. Longitudinal studies will need to address what co-morbidity factors, such as radiation, toxicology, microgravity effects (fluid shift), aging, are involved with hearing loss.

Clark, Jonathan B.↗

NASA NTRS2013

Transmission Electron Microscopy of Iron Metal in Almahata Sitta Ureilite

Almahata Sitta (AS) is a polymict breccia mainly composed of variable ureilite lithologies with small amounts of chondritic lithologies [1]. Fe metal is a common accessory phase in ureilites, but our earlier study on Fe metals in one of AS fragments (#44) revealed a unique mineralogy never seen in other ureilites [2,3]. In this abstract we report detailed transmission electron microscopy (TEM) on these metal grains to better understand the thermal history of ureilites. We prepared FIB sections of AS#44 by JEOL JIB-4000 from the PTS that was well characterized by SEM-EBSD in our earlier study [2]. The sections were then observed by STEM (JEOL JEM- 2100F). One of the FIB sections shows a submicron-sized symplectic intergrown texture composed of Fe metal (kamacite), Fe carbide (cohenite), Fe phosphide (schreibersite), and Fe sulfide (troilite). Each phase has an identical SAED pattern in spite of its complex texture, suggesting co-crystallization of all phases. This is probably caused by shock re-melting of pre-existing metal + graphite to form a eutectic-looking texture. The other FIB section is mostly composed of homogeneous Fe metal (93 wt% Fe, 5 wt% Ni, and 2 wt% Si), but BF-STEM images exhibited the presence of elongated lathy grains (approx. 2 microns long) embedded in the interstitial matrix. The SAED patterns from these lath grains could be indexed by alpha-Fe (bcc) while interstitial areas are gamma-Fe (fcc). The elongated alpha-Fe grains show tweed-like structures suggesting martensite transformation. Such a texture can be formed by rapid cooling from high temperature where gamma-Fe was stable. Subsequently alpha-Fe crystallized, but gamma-Fe remained in the interstitial matrix due to quenching from high temperature. This scenario is consistent with very rapid cooling history of ureilites suggested by silicate mineralogy.

Mikouchi, T.↗

NASA NTRS2016

LAVA Pressure Transducer Trade Study

The Regolith and Environment Science and Oxygen and Lunar Volatile Extraction (RESOLVE) payload will transport the (LAVA) subsystem to hydrogen-rich locations on the moon supporting NASA's in-situ resource utilization (ISRU) programs. There, the LAVA subsystem will analyze volatiles that evolve from heated regolith samples in order to quantify how much water is present. To do this, the system needs resilient pressure transducers (PTs) to calculate the moles in the gas samples. The PT trade study includes a comparison of newly-procured models to a baseline unit with prior flight history in order to determine the PT model with the best survivability in flight-forward conditions.

Trade Study↗

NASA NTRS2017

Lunar Advanced Volatile Analysis Subsystem: Pressure Transducer Trade Study

In Situ Resource Utilization (ISRU) is a key factor in paving the way for the future of human space exploration. The ability to harvest resources on foreign astronomical objects to produce consumables and propellant offers potential reduction in mission cost and risk. Through previous missions, the existence of water ice at the poles of the moon has been identified, however the feasibility of water extraction for resources remains unanswered. The Resource Prospector (RP) mission is currently in development to provide ground truth, and will enable us to characterize the distribution of water at one of the lunar poles. Regolith & Environment Science and Oxygen & Lunar Volatile Extraction (RESOLVE) is the primary payload on RP that will be used in conjunction with a rover. RESOLVE contains multiple instruments for systematically identifying the presence of water. The main process involves the use of two systems within RESOLVE: the Oxygen Volatile Extraction Node (OVEN) and Lunar Advanced Volatile Analysis (LAVA). Within the LAVA subsystem, there are multiple calculations that depend on accurate pressure readings. One of the most important instances where pressure transducers (PT) are used is for calculating the number of moles in a gas transfer from the OVEN subsystem. As a critical component of the main process, a mixture of custom and commercial off the shelf (COTS) PTs are currently being tested in the expected operating environment to eventually down select an option for integrated testing in the LAVA engineering test unit (ETU).

Kang, Edward Shinuk↗

NASA NTRS2019

Restore-L Intern Final Report

Every year, approximately 20 satellites are retired because their propellants are exhausted. Primarily limited by fuel, the satellites are usually fully functioning otherwise. The lifetimes of satellites can be extended with the capability of refueling. Not only would refueling extend satellite lifetime, it would also provide future satellites flexibility to prioritize other elements of their missions. Restore-L is a Goddard Space Flight Center Satellite Servicing Projects Division mission with the primary objectives of developing tools, technologies, and techniques to extend the lifetime of satellites - even if they were not designed to be serviced in or- bit. Equipped with five key servicing technology elements, the Restore-L Servicing Vehicle will demonstrate industry-changing satellite servicing technologies. The primary goal of the Restore-L mission is to rendezvous with, grasp, refuel, and relocate a government-owned satellite to extend its lifetime. The Propellant Transfer Subsystem (PTS) is required to deliver measured amounts of fuel to the client satellite in a safe manner.

Negi, Abhay↗

NASA NTRSDate not supplied

Coherence Analysis of the Space Launch System using Unsteady Pressure Sensitive Paint

Transonic buffet forces are a major source of unsteady loading on launch vehicles, thus requiring accurate estimation for efficient vehicle design. The state of the art in modeling these unsteady loads utilizes wind-tunnel tests where the fluctuating pressures are measured by pressure transducers (PTs) at discrete locations on a rigid buffet model. These pressures are then integrated over the surface of the vehicle to yield a series of orthogonal centerline loads called buffet forcing functions (BFFs). Typically, the PT layout aims at resolving the pressure correlation along the longitudinal axis of the vehicle. As a result, the distribution of azimuthal correlation and its impact on the estimated BFFs are not well known. To fill these gaps, extremely high-spatial-resolution uPSP data were collected for three different configurations of the Space Launch System in the NASA Ames Research Center 11-Foot Transonic Unitary Plan Wind Tunnel. The spatio-temporal behavior of the pressure correlation on these vehicles is analyzed and flow features of interest are investigated. It is shown that terminal shocks interacting with turbulence are a source of increased azimuthal coherence, especially when the shock develops at a junction. Vortex shedding off the forward attachment hardware that connects the core stage to the solid rocket boosters (SRBs) is the most severe buffet environment on the vehicle. The associated fluctuating pressures are shown to be highly coherent as far as the vehicle tail and up to 40 degrees away from the boosters. For selected areas of the vehicle, factoring the azimuthal coherence into the attenuation of discrete-measurements-based BFFs results in under prediction relative to the BFFs obtained from full integration of the uPSP data.

buffet↗

NASA NTRSDate not supplied

Evaluating Sensory Augmentation as A Non-Pharmaceutical Tool to Mitigate Motion Sickness and Enhance Sensorimotor Task Performance: A Pilot Study Using Simulated Capsule Wave Motion

Wave motion during capsule recovery operations can result in motion sickness and performance decrements exacerbating reentry sickness following long duration spaceflight. The purpose of this pilot study was (1) to validate a capsule wave motion simulation as a platform to evaluate motion sickness countermeasures and (2) to evaluate a sensory augmentation belt providing vibrotactile feedback of gravitational upright. Ten healthy subjects ages 38.0 ± 10.1 (6M|4F) were exposed to complex wave motions on a six degree-of-freedom platform that included pitch, roll, and heave at provocative stimulus frequencies (0.1-0.25 Hz) while seated in an illuminated cabin deprived of external visual cues. Subjects reported acute symptoms for up to three consecutive 15 min trials or until they reached a motion sickness endpoint of 8 pts on the Pensacola Diagnostic Index (PDI). Five subjects were randomly assigned to the Sensory Augmentation (SA) group while the other five served as controls (CN group). Based on a Motion Sickness Susceptibility Questionnaire, the two groups had similar motion sickness histories (susceptibility percentile ranking of CN group = 27.5 ± 63.6 in the CN group versus 27.5 ± 37.0 in the SA group, median ± IQR). The vibrotactile feedback consisted of a single array of 8 electromechanical tactors positioned around the torso on an adjustable belt (Engineering Acoustics, Inc) that utilized an integrated inertial measurement unit (IMU) to indicate the direction of upright (e.g., subject’s back tactor on during forward tilt). During each wave motion trial subjects performed a battery of four different tasks: tracking Earth vertical using a joystick with and without a secondary task (Paced Auditory Serial Addition Test), an eye-hand target acquisition task on a cabin-fixed tablet, and the psychomotor vigilance test (PVT). All ten subjects reported varying levels of motion sickness with 6 of 10 reaching a symptom endpoint. Interestingly, subjects anecdotally reported that engagement in the joystick tracking task was less provocative than tasks involving the cabin-fixed tablet or periods of no activity. Sensory augmentation appeared to delay symptom onset, with 2 of 5 subjects reaching an endpoint within the first 15 min trial in the CN group versus none in the SA group (PDI after 15 min = 6.0 ± 2.5 in the CN group versus 3.4 ± 2.5 in the SA group, mean ±std). Sensory augmentation also improved performance on the joystick tracking task at lower stimulus frequencies (0.1 Hz in roll and 0.2 Hz in pitch). Both CN and SA groups maintained a consistent level of performance on the eye-hand target acquisition and PVT throughout the baseline (no motion) and wave motion periods. Our results validated that the simulated capsule wave motion paradigm provides an effective motion sickness stressor. This paradigm is currently being used to investigate the efficacy of intranasal scopolamine to mitigate motion sickness. Sensory augmentation using vibrotactile feedback appears to improve spatial awareness and delay symptom onset during complex passive motion. One advantage of this portable belt design is that it incorporates all tactor drive and IMU circuitry and therefore could continue to be worn by crewmembers and serve as a balance aid during egress and ambulation with recovery operations.

A M Bollinger↗