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DOE OSTI2024

Formation of uranium disulfide from a uranium thioamidate single-source precursor

A single-source-precursor approach was developed to synthesize uranium-based materials outside of the typically-studied oxides. This approach allows for shorter reaction times, milder reaction conditions, and control over the chemicals present in synthesis. To this end, the first homoleptic uranium thioamidate complex was synthesized as a precursor for US 2 materials. Pyrolysis of the thioamidate results in decomposition via an alkene elimination pathway and formation of γ-US 2 , which has historically been hard to access without the need for a secondary sulfur source. Despite the oxophilicity of uranium, the method successfully forms US 2 without the inclusion of oxygen in the bulk final product. These findings are supported by simultaneous thermal analysis, elemental analysis, powder X-ray diffraction, and uranium L 3 -edge X-ray absorption fine-structure spectroscopy. This work represents the first example of a single-source precursor approach to target and synthesize actinide materials other than the oxides.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS1975

Passenger comfort response times as a function of aircraft motion

The relationship between a passenger's response time of changes in level of comfort experienced as a function of aircraft motion was examined. The aircraft used in this investigation was capable of providing a wide range of vertical and transverse accelerations by means of direct lift flap control surfaces and side force generator surfaces in addition to normal control surfaces. Response times to changes in comfort were recorded along with the passenger's rating of comfort on a five point scale. In addition, a number of aircraft motion variables including vertical and transverse accelerations were also recorded. Results indicate some relationship between human comfort response times to reaction time data.

Rinalducci, E. J.↗

NASA NTRSDate not supplied

The Influence of Self-Reported Distractions on the Psychomotor Vigilance Task (PVT) in Laboratory and Field Environments

Introduction: The Psychomotor Vigilance Task (PVT) is a measure of vigilant attention that is commonly used in laboratory environments to assess the neurobehavioral impact of sleep loss and circadian misalignment. The PVT has been increasing in popularity for use in field environments; however, the potential for distraction is higher in the field compared to the lab. It is unclear how distractions experienced by individuals taking the PVT in the real world may influence reaction time metrics. We investigated the influence of self-reported distraction on PVT outcomes across laboratory and field environments. Methods: We examined PVT data from five studies including short (n=36 participants, 3799 PVTs) and long-haul (n=75 participants, 3283 PVTs) airline personnel, control center personnel (n=5 participants, 96 PVTs), and healthy individuals who participated in a study involving at-home and laboratory assessments (n=12 participants, 486 and 310 PVTs). Individuals in all of the studies were asked to complete the five-minute NASA PVT at least three times daily. Participants were asked to indicate the number of distractions they experienced immediately after each PVT. Mean PVT reaction time (RT) and number of distractions were computed for each study and overall. Results: Participants reported more distractions in field environments compared to the lab (short-haul=1.29 +/- 1.48, long-haul=0.66 +/- 1.07, control-center=1.20 +/- 1.37, at-home=0.86 +/- 1.36, laboratory=0.46 +/- 1.07) Across all studies, we found that PVT RT slowed as self-reported distractions increased (all studies combined: 0 distractions=PVT RT 274.4ms; 1=284.6ms; 2=302.9ms; 3=321.2ms; >4=409.3ms). These findings were similar for healthy participants completing PVTs at home (0 distractions=287.1ms; 1=309.9ms; 2=328.3ms; 3=369.8ms; >4=385.1ms) but were less consistent during in-lab assessments (0 distractions=278.7ms; 1=316.2ms; 2=396.2ms; 3=370.4ms; >4=354.4ms). These findings were similar for other PVT outcomes. Conclusion: Participants reported more distractions in field environments compared to the laboratory. Our findings suggest that the number of distractions that individuals report experiencing while taking a PVT increases the reaction time registered by the device. Researchers should collect information about distractions during the PVT and should be aware that distractions may influence the recorded PVT reaction time.

behavior↗

NASA NTRSDate not supplied

Extinction of the Stagnation Point Diffusion Flame: Effect of Conductive Heat Loss into Solid Interior

The planned microgravity experiment Growth and Extinction Limit (GEL) is designed to study the material flammability and extinction of thermally thick solid with an emphasis to quantify the effect of conductive heat loss into the solid interior by measuring the in-depth temperature profile. To obtain a more detailed understanding of the extinction phenomena, a previously developed one-dimensional axisymmetric stagnation-point diffusion flame model is expanded to account for the excessive heat loss into the solid beyond the steady burning state. This is important because for thick solids, this is important because the burning period can have a long and slow solid transient with a quasi-steady gas -phase. A non-dimensional excessive conductive heat loss parameter Ψ is defined in the paper and extensive numerical computations have been performed to determine the extinction boundary and the characteristics of near-limit flames. The classical U-shaped flammability boundary in the oxygen vs. stretch rate plot now becomes a series of U-shaped boundaries as a function of Ψ. For a given oxygen ambient, extinction boundary is a function of Ψ. The boundary consists of a blowoff branch and a radiative quenching branch. This is similar to the steady burning flammability boundary (Ψ =0) in the oxygen vs stretch rate plot. Extensive computed data including flame and pyrolysis temperatures, burning rate, flame standoff distance, and reaction rate are presented along the extinction boundaries. In particular, we note that the non-dimensional gas reaction rate is the ratio of diffusion reaction time to the reaction diffusion time, so it has the classical Damhkoler number character. By examining the maximum non-dimensional reaction rates, we observe that along the extinction boundaries, they are approximate constant across the entire range of stretch rates (from quenching to blow-off). These critical values are of the order unity but may vary in different oxygen ambient. The implication will be discussed in the presentation together with the near-limit flame structures.

Chengyao Li↗

NASA NTRS1982

The effects of reduced oxygen and of carbon monoxide on performance in a mouse pole-jump apparatus

The effects on reaction time and behavior were studied for exposure to reduced oxygen concentrations in the presence and absence of carbon monoxide. Tests were run with Swiss Webster mice in a pole-jump apparatus. The results show that reaction times increase gradually with a decrease in oxygen (O2) to 10 percent O2. Below 10 percent O2 reaction times increase dramatically and performance is degraded almost immediately. At carbon monoxide (CO) concentrations of 500 ppm and reduced O2 levels, reaction times are increased even more. At CO concentrations of 1000 ppm, performance is nearly completely degraded even without reduced oxygen levels.

Cagliostro, D. E.↗

NASA NTRS1997

Effects of Orientation on Recognition of Facial Affect

The ability to discriminate facial features is often degraded when the orientation of the face and/or the observer is altered. Previous studies have shown that gross distortions of facial features can go unrecognized when the image of the face is inverted, as exemplified by the 'Margaret Thatcher' effect. This study examines how quickly erect and supine observers can distinguish between smiling and frowning faces that are presented at various orientations. The effects of orientation are of particular interest in space, where astronauts frequently view one another in orientations other than the upright. Sixteen observers viewed individual facial images of six people on a computer screen; on a given trial, the image was either smiling or frowning. Each image was viewed when it was erect and when it was rotated (rolled) by 45 degrees, 90 degrees, 135 degrees, 180 degrees, 225 degrees and 270 degrees about the line of sight. The observers were required to respond as rapidly and accurately as possible to identify if the face presented was smiling or frowning. Measures of reaction time were obtained when the observers were both upright and supine. Analyses of variance revealed that mean reaction time, which increased with stimulus rotation (F=18.54, df 7/15, p (is less than) 0.001), was 22% longer when the faces were inverted than when they were erect, but that the orientation of the observer had no significant effect on reaction time (F=1.07, df 1/15, p (is greater than) .30). These data strongly suggest that the orientation of the image of a face on the observer's retina, but not its orientation with respect to gravity, is important in identifying the expression on the face.

Cohen, M. M.↗

NASA NTRS2010

A Flight-Calibrated Methodology for Determination of Cassini Thruster On-Times for Reaction Wheel Biases

The Cassini spacecraft, the largest and most complex interplanetary spacecraft ever built, continues to undertake unique scientific observations of planet Saturn, Titan, Enceladus, and other moons of the ring world. In order to maintain a stable attitude during the course of its mission, this three-axis stabilized spacecraft uses two different control systems: the Reaction Control System (or RCS) and the Reaction Wheel Assembly (RWA) control system. In the course of its mission, Cassini performs numerous reaction wheel momentum biases (or unloads) using its reaction control thrusters. The use of the RCS thrusters often imparts undesired velocity changes (delta Vs) on the spacecraft and it is crucial for Cassini navigation and attitude control teams to be able to, quickly but accurately, predict the hydrazine usage and delta V vector in Earth Mean Equatorial (J2000) inertial coordinates for reaction wheel bias events, without actually having to spend time and resources simulating the event in a dynamic or hardware-in-the-loop simulation environments. The flight-calibrated methodology described in this paper, and the ground software developed thereof, are designed to provide the RCS thruster on-times, with acceptable accuracy and without any form of dynamic simulation, for reaction wheel biases, along with the hydrazine usage and the delta V in EME-2000 inertial frame.

Reaction Control System↗

NASA NTRS1975

Conspicuity of target lights: The influence of flash rate and brightness

The stimulus characteristics of lights that might aid a pilot to see and avoid, by alerting him to a potential threat were studied. The relative conspicuity of foveally equated, point-source, steady and flashing lights of several brightnesses, seen against a star background was examined. From the subject's viewpoint, these target lights could appear anywhere within a large (40 deg horizontal by 35 deg vertical) field of view. The lights appeared at random time intervals while the subject was periodically distracted by a simulated cockpit task. The results indicate that correct target detection increases and reaction time decreases with increased target intensity. Steady lights are missed more frequently and acquired more slowly than flashing lights, but no significant differences are found among the wide range of flash rates employed. The intensity of the light has a greater effect on both detection and reaction time to steady lights than to flashing lights. These results are compared with results of other researchers who used targets which appeared at fixed locations. The longest reaction times were recorded to lights which appeared either at the extremes or at the very center of the visual field.

Connors, M. M.↗

DOE OSTI2020

Non-catalytic oxidative depolymerization of lignin in perfluorodecalin to produce phenolic monomers

We demonstrate for the first time non-catalytic, oxidative cracking with molecular oxygen (O 2 ) to depolymerize native lignin into oxygenated phenolic monomers. Maximum monomer yield of 10.5 wt% was achieved at 250 °C after only 10 min of reaction and included vanillin, syringaldehyde, vanillic acid, and syringic acid. High rates of oxidation are attributed to the use of perfluorodecalin as solvent. Perfluorodecalin is a perfluorocarbon (PFC), characterized by their chemical stability and exceptionally high solubility for O 2 . Monomer yields were typically five-fold higher in perfluorodecalin compared to solvents more commonly employed in lignin conversion, such as methanol, butanol, acetonitrile, and ethyl acetate. Phenolic monomer production in perfluorodecalin favors high temperatures and short reaction times to prevent further oxidation of the produced monomers. Lignin oil obtained under oxidative conditions in perfluorodecalin showed lower molecular weight and smaller polydispersity compared to other solvents. Increasing the reaction time further decreased the molecular weight, while increasing reaction time in an inert atmosphere increased the molecular weight of the lignin oil. High concentrations of O 2 in perfluorodecalin not only increased lignin depolymerization but suppressed undesirable condensation reactions. Depolymerization is likely initiated by thermally induced homolytic cleavage of ether linkages in lignin to form phenoxy and carbon-based radicals. These radicals bind with O 2 as a radical scavenger and further react to form phenolic monomeric products rather than repolymerizing to large oligomers. The PFC process was scaled from 5 mL to 250 mL without any loss of yield. Because most organic compounds are not soluble in perfluorodecalin, recycling is easily achieved via liquid–liquid separation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2010

A Flight-Calibrated Methodology for Determination of Cassini Thruster On-Times for Reaction Wheel Biases

This paper describes a methodology for accurate and flight-calibrated determination of the on-times of the Cassini spacecraft Reaction Control System (RCS) thrusters, without any form of dynamic simulation, for the reaction wheel biases. The hydrazine usage and the delta V vector in body frame are also computed from the respective thruster on-times. The Cassini spacecraft, the largest and most complex interplanetary spacecraft ever built, continues to undertake ambitious and unique scientific observations of planet Saturn, Titan, Enceladus, and other moons of Saturn. In order to maintain a stable attitude during the course of its mission, this three-axis stabilized spacecraft uses two different control systems: the RCS and the reaction wheel assembly control system. The RCS is used to execute a commanded spacecraft slew, to maintain three-axis attitude control, control spacecraft's attitude while performing science observations with coarse pointing requirements, e.g. during targeted low-altitude Titan and Enceladus flybys, bias the momentum of reaction wheels, and to perform RCS-based orbit trim maneuvers. The use of RCS often imparts undesired delta V on the spacecraft. The Cassini navigation team requires accurate predictions of the delta V in spacecraft coordinates and inertial frame resulting from slews using RCS thrusters and more importantly from reaction wheel bias events. It is crucial for the Cassini spacecraft attitude control and navigation teams to be able to, quickly but accurately, predict the hydrazine usage and delta V for various reaction wheel bias events without actually having to spend time and resources simulating the event in flight software-based dynamic simulation or hardware-in-the-loop simulation environments. The methodology described in this paper, and the ground software developed thereof, are designed to provide just that. This methodology assumes a priori knowledge of thrust magnitudes and thruster pulse rise and tail-off time constants for eight individual attitude control thrusters, the spacecraft's wet mass and its center of mass location, and a few other key parameters.

Earth Mean Equatorial↗

DOE OSTI2021

Facile microwave synthesis of zirconium metal-organic framework thin films on gold and silicon and application to sensor functionalization

Zirconium-based metal-organic frameworks, including UiO-66 and related frameworks, have become the focus of considerable research in the area of chemical warfare agent (CWA) decontamination. However, little work has been reported exploring these metal-organic frameworks (MOFs) for CWA sensing applications. For many sensing approaches, the growth of high-quality thin films of the active material is required, and thin film growth methods must be compatible with complex device architectures. Several approaches to synthesize thin films of UiO-66 have been described but many of these existing methods are complex or time consuming. In this work, we describe the development of a simple and rapid microwave assisted synthesis of oriented UiO-66 thin films on unmodified silicon (Si) and gold (Au) substrates. Thin films of UiO-66 and UiO-66-NH 2 can be grown in as little as 2 min on gold substrates and 30 min on Si substrates. The film morphology and orientation are characterized and the effects of reaction time and temperature on thin film growth on Au are investigated. Both reaction time and temperature impact the overgrowth of protruding discrete crystallites in the thin film layer but, surprisingly, no strong correlation is observed between film thickness and reaction time or temperature. We also briefly describe the synthesis of Zr/Ce solid solution thin films of UiO-66 on Au and report the first synthesis of a solid solution thin film MOF. Finally, we demonstrate the utility of the microwave method for the facile functionalization of two sensor architectures, plasmonic nanohole arrays and microresonators, with UiO-66 thin films.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Experimental-based mechanistic study and optimization of hydrothermal liquefaction of anaerobic digestates

Valorization of agricultural and food waste digestates is crucial for sustainable waste management to reduce environmental impacts and improve the economics of commercial farms. Hydrothermal liquefaction (HTL) of anaerobic digestates was evaluated to recover resources by converting them into carbon-dense biocrude oil and a nutrient-rich HTL aqueous phase (HTL-AP) coproduct. The effects of HTL temperature (280–360 °C), reaction time (10–50 min), feedstock pH (2.5–8.5), digestate salt content (1–5 wt%), and digestate cellulose-to-lignin ratio (0.2–1.8) on energy and nutrient recovery were systematically investigated in a set of well-designed experiments following a half-fractional central composite protocol. Response surface analysis combined with HTL product characterization and comparative literature study produced a comprehensive reaction pathway for HTL of anaerobic digestates. Moreover, this analysis revealed the importance of acidic feedstocks (pH 3.00–5.53), high reaction temperatures (337–360 °C), and reaction times <45 or 45–50 min for digestates with Cel/Lig >1 or <1, for maximizing the energy recovered in biocrude (high carbon yield and low heteroatom content) and the amounts of P, NH 3 –N, and Mg distributed in the HTL-AP. Acidic conditions catalyzed biocrude production, inhibited the Maillard reaction (lowering the nitrogen content in biocrude), and partitioned nutrients into the HTL-AP. Higher reaction temperatures coupled with longer reaction times activated hydro-denitrogenation and deoxygenation reactions to improve biocrude quality. Finally, this work provides not only validated methods to achieve targeted resource recovery for specific feedstock compositions using HTL, but also a comprehensive mechanistic understanding of the HTL of biomass waste for controlling target product characteristics.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1975

Development of a chemiluminescent and bioluminescent system for the detection of bacteria in wastewater effluent

Automated chemiluminescent and bioluminescent sensors were developed for continuous monitoring of microbial levels in wastewater effluent. Development of the chemiluminescent system included optimization of reagent concentrations as well as two new techniques which will allow for increased sensitivity and specificity. The optimal reagent concentrations are 0.0025 M luminol and 0.0125 M sodium perborate in 0.75N sodium hydroxide before addition of sample. The methods developed to increase specificity include (1) extraction of porphyrins from bacteria collected in a filter using 0.1N NaOH - 50 percent Ethanol, and (2) use of the specific reaction rate characteristics for the different luminol catalysts. Since reaction times are different for each catalyst, the reaction can be made specific for bacteria by measuring only the light emission from the particular reaction time zone specific for bacteria. Developments of the bioluminescent firefly luciferase system were in the area of flow system design.

Thomas, R. R.↗

NASA NTRS2010

DVA as a Diagnostic Test for Vestibulo-Ocular Reflex Function

The vestibulo-ocular reflex (VOR) stabilizes vision on earth-fixed targets by eliciting eyes movements in response to changes in head position. How well the eyes perform this task can be functionally measured by the dynamic visual acuity (DVA) test. We designed a passive, horizontal DVA test to specifically study the acuity and reaction time when looking in different target locations. Visual acuity was compared among 12 subjects using a standard Landolt C wall chart, a computerized static (no rotation) acuity test and dynamic acuity test while oscillating at 0.8 Hz (+/-60 deg/s). In addition, five trials with yaw oscillation randomly presented a visual target in one of nine different locations with the size and presentation duration of the visual target varying across trials. The results showed a significant difference between the static and dynamic threshold acuities as well as a significant difference between the visual targets presented in the horizontal plane versus those in the vertical plane when comparing accuracy of vision and reaction time of the response. Visual acuity increased proportional to the size of the visual target and increased between 150 and 300 msec duration. We conclude that dynamic visual acuity varies with target location, with acuity optimized for targets in the plane of rotation. This DVA test could be used as a functional diagnostic test for visual-vestibular and neuro-cognitive impairments by assessing both accuracy and reaction time to acquire visual targets.

Wood, Scott J.↗

DOE OSTI2025

Sustainable potassium sorbate production from triacetic acid lactone in food-grade solvents

This study advances the production of potassium sorbate (KS) from triacetic acid lactone (TAL) utilizing food-grade solvents, ethanol (EtOH) and isopropyl alcohol (IPA). Here, we have previously demonstrated the route to produce KS from TAL in tetrahydrofuran (THF) as the main solvent, but the use of THF is associated with environmental and health risks especially for food applications. The process employs a catalytic approach in food-grade solvents and includes three main steps: hydrogenation, etherification and hydrolysis, and ring-opening hydrolysis to produce KS from TAL. In the synthesis of KS from TAL, the use of IPA leads to higher yields and reduced reaction times compared to EtOH. As a result, the overall reaction time in IPA was reduced to 35.7 h, compared to 42.1 h in our previous study using THF and EtOH, while achieving a comparable KS yield of 84% from TAL. The synthesized KS exhibits a trans-2, trans-4 geometrical configuration, identical to that of commercially available KS. Through techno-economic analysis (TEA) and life cycle assessment (LCA), we estimated full-scale production of KS from sugarcane with the developed process in IPA could achieve a minimum product selling price (MPSP) of $\$8.27$ per kg with a range of $\$7.06$–10.16 per kg [5th–95th percentiles from 6000 Monte Carlo simulations] and a carbon intensity (CI) of 13.7 [9.6–18.6] kg CO 2 -eq per kg. This study highlights the synthesis of KS from TAL using food-grade solvents, demonstrating improved economic viability and environmental sustainability compared to our previous research (MPSP of $\$9.68$ per kg [$\$8.47$–11.45 per kg] and CI of 16.2 [12.0–21.2] kg CO 2 -eq per kg), as the total required reaction decreases while achieving the comparable overall yield of KS from TAL.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Data for "Sustainable Potassium Sorbate Production from Triacetic Acid Lactone in Food-Grade Solvents"

This study advances the production of potassium sorbate (KS) from triacetic acid lactone (TAL) utilizing food-grade solvents, ethanol (EtOH) and isopropyl alcohol (IPA). We have previously demonstrated the route to produce KS from TAL in tetrahydrofuran (THF) as the main solvent, but the use of THF is associated with environmental and health risks especially for food applications. The process employs a catalytic approach in food-grade solvents and includes three main steps: hydrogenation, etherification and hydrolysis, and ring-opening hydrolysis to produce KS from TAL. In the synthesis of KS from TAL, the use of IPA leads to higher yields and reduced reaction times compared to EtOH. As a result, the overall reaction time in IPA was reduced to 35.7 h, compared to 42.1 h in our previous study using THF and EtOH, while achieving a comparable KS yield of 84% from TAL. The synthesized KS exhibits a trans-2, trans-4 geometrical configuration, identical to that of commercially available KS. Through techno-economic analysis (TEA) and life cycle assessment (LCA), we estimated full-scale production of KS from sugarcane with the developed process in IPA could achieve a minimum product selling price (MPSP) of $8.27 per kg with a range of $7.06–10.16 per kg [5th–95th percentiles from 6000 Monte Carlo simulations] and a carbon intensity (CI) of 13.7 [9.6–18.6] kg CO2-eq per kg. This study highlights the synthesis of KS from TAL using food-grade solvents, demonstrating improved economic viability and environmental sustainability compared to our previous research (MPSP of $9.68 per kg [$8.47–11.45 per kg] and CI of 16.2 [12.0–21.2] kg CO2-eq per kg), as the total required reaction decreases while achieving the comparable overall yield of KS from TAL.

bioproducts↗

DOE OSTI2020

Production of levulinic acid and biocarbon electrode material from corn stover through an integrated biorefinery process

To overcome the inefficient biomass conversion, waste generation, and lack of co-production in biorefineries, an integrated process was proposed for the conversion of corn stover into levulinic acid and biocarbon electrode material. Corn stover was pretreated through hydrothermal process using 0.45 wt% K 2 CO 3 which removed 76 wt% lignin and 85 wt% xylan while preserving 83 wt% glucan. This was followed by acid hydrolysis to produce levulinic acid at varying H 2 SO 4 concentrations and reaction time in a batch reactor at 190 °C. At a reaction time of 5 min in 2 wt% H 2 SO 4 , 35.8 wt% and 30 wt% glucan in raw and pretreated corn stover was converted to levulinic acid, respectively. The residue from acid hydrolysis was converted into biocarbon for supercapacitor electrodes via a two-step thermal activation process which showed a specific capacitance of 120 F g -1 . The proposed integrated biorefinery concept provides multiple value-added products for a greater financial and environmental sustainability.

09 BIOMASS FUELS↗

NASA NTRS1972

New reaction tester accurate within 56 microseconds

Testing device measures simple and disjunctive reaction time of human subject to light stimuli. Tester consists of reaction key, logic card, panel mounted neon indicators, and interconnecting wiring. Device is used for determining reaction times of patients undergoing postoperative neurological therapy.

Brown, H.↗