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NASA NTRS1993

Test Would Quantify Combustion Oxygen From Different Sources

Proposed isotope-enrichment scheme enables determination of contributions of dual sources of oxygen for combustion. Liquid oxygen or other artificial stream enriched with O(18) to about 1 percent by weight. Combustion products analyzed by mass spectrometer to measure relative abundances of H2O(18) and H2O(16). From relative abundances of water products measured, one computes relative contribution of oxygen extracted from stream compared to other source of oxygen in combustion process. Used to determine contributions of natural oxygen in air and liquid oxygen supplied in separate stream mixed with air or sent directly into combustion chamber.

Tapphorn, Ralph M.↗

DOE OSTI2016

Mechanism of conductivity relaxation in liquid and polymeric electrolytes: Direct link between conductivity and diffusivity

Combining broadband impedance spectroscopy, differential scanning calorimetry, and nuclear magnetic resonance we analyzed charge and mass transport in two polymerized ionic liquids and one of their monomeric precursors. In order to establish a general procedure for extracting single-particle diffusivity from their conductivity spectra, we critically assessed several approaches previously employed to describe the onset of diffusive charge dynamics and of the electrode polarization in ion conducting materials. Based on the analysis of the permittivity spectra, we demonstrate that the conductivity relaxation process provides information on ion diffusion and the magnitude of cross-correlation effects between ionic motions. A new approach is introduced which is able to estimate ionic diffusivities from the characteristic times of conductivity relaxation and ion concentration without any adjustable parameters. Furthermore, this opens the venue for a deeper understanding of charge transport in concentrated and diluted electrolyte solutions.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2019

A unified form of low-energy nodal electronic interactions in hole-doped cuprate superconductors

Using angle resolved photoemission spectroscopy measurements of Bi 2 Sr 2 CaCu 2 O 8+δ over a wide range of doping levels, we present a universal form for the non-Fermi liquid electronic interactions in the nodal direction in the exotic normal state phase. It is described by a continuously varying power law exponent versus energy and temperature (hence named a Power Law Liquid or PLL), which with doping varies smoothly from a quadratic Fermi Liquid in the overdoped regime, to a linear Marginal Fermi Liquid at optimal doping, to a non-quasiparticle non-Fermi Liquid in the underdoped regime. The coupling strength is essentially constant across all regimes and is consistent with Planckian dissipation. Using the extracted PLL parameters we reproduce the experimental optics and resistivity over a wide range of doping and normal-state temperature values, including the T* pseudogap temperature scale observed in the resistivity curves. This breaks the direct link to the pseudogapping of antinodal spectral weight observed at similar temperature scales and gives an alternative direction for searches of the microscopic mechanism.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2023

Pertechnetate/perrhenate–capped Zr/Hf–Dihydroxide Dimers: Elucidating Zr–TcO 4 Co–Mobility in the Nuclear Fuel Cycle

Spent nuclear fuel contains heavy element fission products that must be separated for effective reprocessing for a safe and sustainable nuclear fuel cycle. 93 Zr and 99 Tc are high-yield fission products that co-transport in liquid-liquid extraction processes. Here we seek atomic-level information of this co-extraction process, as well as fundamental knowledge about Zr IV (and Hf IV ) aqueous speciation in the presence of topology-directing ligands such as pertechnetate (TcO 4 – ) and non-radioactive surrogate perrhenate (ReO 4 – ). In this context, we show that the flat tetrameric oxyhydroxyl-cluster [M IV 4 (OH) 8 (H 2 O) 16 ] 8+ (and related polymers) is dissociated by perrhenate/pertechnetate to yield isostructural dimers, M 2 (OH) 2 (XO 4 – ) 6 (H 2 O) 6 • 3H 2 O (M=Zr/Hf IV ; X=Re/Tc VII ), elucidated by single-crystal X-ray diffraction. We used these model compounds to understand the pervasive 93 Zr- 99 Tc coextraction with further speciation studies in water, nitric acid, and tetrabutylphosphate (TBP) -kerosene; where the latter two media are relevant to nuclear fuel reprocessing. SAXS (small angle X-ray scattering), compositional evaluation, and where experimentally feasible, ESI-MS (electrospray ionization mass spectrometry) showed that perrhenate/pertechnetate influence Zr/Hf IV -speciation in water. Here, in Zr-XO 4 solvent extraction studies to simulate fuel reprocessing, we provide evidence that TcO 4 – enhances extraction of Zr IV , and compositional analysis of the extracted metal-complexes (Zr-ReO 4 study) is consistent with the crystallized Zr IV 2 (OH) 2 (Re VII O 4 – ) 6 (H 2 O) 6 •dimer.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2020

Directional self-locomotion of active droplets enabled by nematic environment

Active matter comprised of self-propelled interacting units holds a major promise for the extraction of useful work from its seemingly chaotic dynamics. Streamlining active matter is especially important at microscale, where the viscous forces prevail over inertia and transport requires a non-reciprocal motion. Here we report that microscopic active droplets representing aqueous dispersions of swimming bacteria Bacillus subtilis become unidirectionally motile when placed in an inactive nematic liquid crystal medium. Random motion of bacteria inside the droplet is rectified into a directional self-locomotion of the droplet by the polar director structure that the droplet creates in the surrounding nematic through anisotropic molecular interactions at its surface. Droplets without active swimmers show no net displacement. The trajectory of the active droplet can be predesigned by patterning the molecular orientation of the nematic. As a result, the effect demonstrates that broken spatial symmetry of the medium can be the reason for and the means to control directional microscale transport.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2021

Design and production of the high voltage electrode grids and electron extraction region for the LZ dual-phase xenon time projection chamber

The dual-phase xenon time projection chamber (TPC) is a powerful tool for direct-detection experiments searching for WIMP dark matter, other dark matter models, and neutrinoless double-beta decay. Successful operation of such a TPC is critically dependent on the ability to hold high electric fields in the bulk liquid, across the liquid surface, and in the gas. Careful design and construction of the electrodes used to establish these fields is therefore required. We present the design and production of the LUX-ZEPLIN (LZ) experiment's high-voltage electrodes, a set of four woven mesh wire grids. Grid design drivers are discussed, with emphasis placed on design of the electron extraction region. Here, we follow this with a description of the grid production process and a discussion of steps taken to validate the LZ grids prior to integration into the TPC.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Evaluation of light collection from highly scattering media using wavelength-shifting fibers

Opaque scintillators are designed to have a short scattering length such that scintillation photons are probabilistically confined to a small region of space about their origin. The benefit of this feature is that information on the interaction event topology can be recorded with greater fidelity than in traditional highly transparent media with sensors at large distances from the light production region. Opaque scintillator detectors rely on wavelength-shifting fibers to extract the scintillation light; however, the efficiency of light collection has not yet been directly measured in experiment. We measured the efficiency of light collection as a function of the optical parameters of an opaque liquid and the distance from the origin of the light to the fiber. We use the experimental data to validate a Monte Carlo model of light transport and collection and discuss a simple diffusion model that reproduces the results of Monte Carlo simulation with high fidelity. Furthermore, this combination of validated models has the potential for use in predictions of performance in various designs of future opaque scintillator detectors such as LiquidO.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Improved Characterization of Soil Organic Matter by Integrating FT-ICR MS, Liquid Chromatography Tandem Mass Spectrometry, and Molecular Networking: A Case Study of Root Litter Decay under Drought Conditions

Understanding of how soil organic matter (SOM) chemistry is altered in a changing climate has advanced considerably; however, most SOM components remain unidentified, impeding the ability to characterize a major fraction of organic matter and predict what types of molecules, and from which sources, will persist in soil. Here we present a novel approach to better characterize SOM extracts by integrating information from three types of analyses, and we deploy this method to characterize decaying root-detritus soil microcosms subjected to either drought or normal conditions. To observe broad differences in composition, we employed direct infusion Fourier-transform ion cyclotron resonance mass spectrometry (DI-FT-ICR MS). We complemented this with liquid chromatography tandem mass spectrometry (LC-MS/MS) to identify components by library matching. Since libraries contain only a small fraction of SOM components, we also used fragment spectral cosine similarity scores to relate unknowns and library matches through molecular networks. This integrated approach allowed us to corroborate DI-FT-ICR MS molecular formulas using library matches, which included fungal metabolites and related polyphenolic compounds. We also inferred structures of unknowns from molecular networks and improved LC-MS/MS annotation rates from ~5 to 35% by considering DI-FT-ICR MS molecular formula assignments. Under drought conditions, we found greater relative amounts of lignin-like vs condensed aromatic polyphenol formulas and lower average nominal oxidation state of carbon, suggesting reduced decomposition of SOM and/or microbes under stress. Our integrated approach provides a framework for enhanced annotation of SOM components that is more comprehensive than performing individual data analyses in parallel.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2011

Quasi-Elastic Neutron Scattering Studies of the Slow Dynamics of Supercooled and Glassy Aspirin

Aspirin, also known as acetylsalicylic acid (ASA), is not only a wonderful drug, but also a good glass former. Therefore, it serves as an important molecular system to study the near-arrest and arrested phenomena. In this paper, a high-resolution quasi-elastic neutron scattering (QENS) technique is used to investigate the slow dynamics of supercooled liquid and glassy aspirin from 410 K down to 350 K. The measured QENS spectra can be analyzed with a stretched exponential model. We find that (i) the stretched exponent (Q) is independent of the wave vector transfer Q in the measured Q-range, and (ii) the structural relaxation time (Q) follows a power law dependence on Q. Consequently, the Q-independent structural relaxation time 0 can be extracted for each temperature to characterize the slow dynamics of aspirin. The temperature dependence of 0 can be fitted with the mode coupling power law, the Vogel-Fulcher-Tammann equation and a universal equation for fragile glass forming liquids recently proposed by M. Tokuyama in the measured temperature range. The calculated dynamic response function T(Q,t) using the experimentally determined self-intermediate scattering function of the hydrogen atoms of aspirin shows a direct evidence of the enhanced dynamic fluctuations as the aspirin is increasingly supercooled, in agreement with the fixed-time mean squared displacement x2 and non-Gaussian parameter 2 extracted from the elastic scattering.

08 HYDROGEN↗

DOE OSTI2015

Dereplicating and spatial mapping of secondary metabolites from fungal cultures in situ

Ambient ionization techniques coupled to mass spectrometry have recently become prevalent in natural product research due to their ability to examine secondary metabolites in situ. Identifying, mapping, and monitoring secondary metabolites directly on an organism provides invaluable spatial and temporal details that are lost through traditional extraction processes. Most ambient ionization techniques do not collect mutually supportive data, such as chromatographic retention times and/or UV/VIS spectra, and this can limit the ability to identify certain metabolites, such as differentiating isomers. To overcome this, the droplet liquid microjunction surface sampling probe (droplet LMJ SSP) was coupled with UPLC PDA HRMS MS/MS, thus providing separation, retention times, and UV/VIS data used in traditional dereplication protocols. By capturing these mutually supportive data, the identity of secondary metabolites could be confidently and rapidly assigned in situ. Using the droplet LMJ SSP, a protocol was constructed to analyze the secondary metabolite profile of fungal cultures directly without any sample preparation. The results demonstrate that fungal cultures can be dereplicated from the Petri dish, thus identifying secondary metabolites, including isomers, and confirming them against reference standards. As a result, heat maps, similar to mass spectrometry imaging, can be used to ascertain the location and relative concentration of secondary metabolites directly on the surface and/or surroundings of a fungal culture.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2011

Proteomic and targeted qPCR analyses of subsurface microbial communities for presence of methane monooxygenase

The Test Area North (TAN) site at the Idaho National Laboratory near Idaho Falls, ID, USA, sits over a trichloroethylene (TCE) contaminant plume in the Snake River Plain fractured basalt aquifer. Past observations have provided evidence that TCE at TAN is being transformed by biological natural attenuation that may be primarily due to co-metabolism in aerobic portions of the plume by methanotrophs. TCE co-metabolism by methanotrophs is the result of the broad substrate specificity of microbial methane monooxygenase which permits non-specific oxidation of TCE in addition to the primary substrate, methane. Arrays of experimental approaches have been utilized to understand the biogeochemical processes driving intrinsic TCE co-metabolism at TAN. In this study, aerobic methanotrophs were enumerated by qPCR using primers targeting conserved regions of the genes pmoA and mmoX encoding subunits of the particulate MMO (pMMO) and soluble MMO (sMMO) enzymes, respectively, as well as the gene mxa encoding the downstream enzyme methanol dehydrogenase. Identification of proteins in planktonic and biofilm samples from TAN was determined using reverse phase ultraperformance liquid chromatography (UPLC) coupled with a quadrupole-time-of-flight (QToF) mass spectrometer to separate and sequence peptides from trypsin digests of the protein extracts. Detection of MMO in unenriched water samples from TAN provides direct evidence of intrinsic methane oxidation and TCE co-metabolic potential of the indigenous microbial population. Mass spectrometry is also well suited for distinguishing which form of MMO is expressed in situ either soluble or particulate. Using this method, pMMO proteins were found to be abundant in samples collected from wells within and adjacent to the TCE plume at TAN.

03 NATURAL GAS↗

NASA NTRS1992

Beneficiation and extraction of nonterrestrial materials, part 2

A review of options for processing extraterrestrial materials was dominated by industrial materials scientist who tried to identify which processes utilizing space materials could be implemented in the near term. The most practical process seem to us to be the extraction of lunar oxygen and the extraction of metals and ceramics from the residues of the reduction process. The growth of space activity will be accompanied by increased demand for liquid oxygen for each round trip to the Moon. The oxygen and the intermediary product water will be needed for the life support at the base. The reduced metals and ceramics may be considered byproducts or may develop into primary products. Some of the same processes would be directly applicable to recovery of products from asteroids. We also discussed other processes for directly utilizing asteroid metals. Some of the topics covered include beneficiation and oxygen extraction methods, metallurgy, and extraterrestrial cement.

Agosto, William N.↗

NASA NTRS1999

Growth of Compound Semiconductors in a Low Gravity Environment: Microgravity Growth of PbSnTe

The growth of the alloy compound semiconductor lead tin telluride (PbSnTe) was chosen for a microgravity flight experiment in the Advanced Automated Directional Solidification Furnace (AADSF), on the United States Microgravity Payload-3 (USNP-3) in February, 1996 and on USNW- 4 in November, 1997. The objective of these experiments was to determine the effect of the reduction in convection, during the growth process, brought about by the microgravity environment. The properties of devices made from PbSnTe, an alloy of PbTe and SnTe, are dependent on the ratio of the elemental components in the starting crystal. Compositional uniformity in the crystal is only obtained if there is no significant mixing in the liquid during growth. The technological importance of PbSnTe lies in its band gap versus composition diagram which has a zero energy crossing at approximately 40% SnTe. This facilitates the construction of long wavelength (greater than 6 gm) infrared detectors and lasers. The properties and utilization of PbSnTe are the subject of other papers. 1,2 PbSnTe is also interesting from a purely scientific point of view. It is, potentially, both solutally and thermally unstable due to the temperature and density gradients present during growth. Density gradients, through thermal expansion, are imposed in directional solidification because temperature gradients are required to extract heat. Solutal gradients occur in directional solidification of alloys due to segregation at the interface. Usually the gradients vary with both experiment design and inherent materials properties. In a simplified one dimensional analysis with the growth axis parallel to the gravity vector, only one of the two instabilities work at a time. During growth, the temperature in the liquid increases ahead of the interface. Therefore the density, due to thermal expansion, is decreasing in that direction. However, the phase diagram shows that the lighter SnTe is preferentially rejected at the interface. This causes the liquid density to increase with distance away from the interface.

Fripp, A. L.↗

DOE OSTI2019

A semi-empirical power-law model for the dip-coating of a substrate into a particle-containing, non-Newtonian, complex fluid system

The apparent viscosity of a particle suspension of ZrSi 2 particles, polyhydromethylsiloxane (PHMS) preceramic polymer and n-Octane solvent, used to process polymer-derived ceramic composite coatings, is shown by viscometric experiments to be shear-thinning. The suspension is dip-coated onto substrates and the measured entrained coating thickness, h 0 , is observed to be a power-law function of U, the substrate extraction speed, as h 0 = 0.5051U 0.5 . The experimentally observed semi-empirical model is directly compared to the results of a variety of theoretically derived Landau-Levich scaling laws and other models that have similar liquids and that include other effects. None of these cases predicts the scaling observed in these experiments. A correction factor is introduced to quantify the difference between the semi-empirical model with existing theoretical models. Possible explanations for the observed scaling behavior are presented.

36 MATERIALS SCIENCE↗

DOE OSTI2018

DarkSide-20k: A 20 tonne two-phase LAr TPC for direct dark matter detection at LNGS

Abstract. Building on the successful experience in operating the DarkSide-50 detector, the DarkSide Collaboration is going to construct DarkSide-20k, a direct WIMP search detector using a two-phase Liquid Argon Time Projection Chamber (LAr TPC) with an active (fiducial) mass of 23 t (20 t). This paper describes a preliminary design for the experiment, in which the DarkSide-20k LAr TPC is deployed within a shield/veto with a spherical Liquid Scintillator Veto (LSV) inside a cylindrical Water Cherenkov Veto (WCV). This preliminary design provides a baseline for the experiment to achieve its physics goals, while further development work will lead to the final optimization of the detector parameters and an eventual technical design. Operation of DarkSide-50 demonstrated a major reduction in the dominant 39Ar background when using argon extracted from an underground source, before applying pulse shape analysis. Data from DarkSide-50, in combination with MC simulation and analytical modeling, shows that a rejection factor for discrimination between electron and nuclear recoils of > 3 × 109 is achievable. This, along with the use of the veto system and utilizing silicon photomultipliers in the LAr TPC, are the keys to unlocking the path to large LAr TPC detector masses, while maintaining an experiment in which less than < 0.1 events (other than ?-induced nuclear recoils) is expected to occur within the WIMP search region during the planned exposure. DarkSide-20k will have ultra-low backgrounds than can be measured in situ, giving sensitivity to WIMP-nucleon cross sections of 1.2×10 -47 cm2 (1.1×10 -46 cm2) for WIMPs of 1TeV/c2 (10TeV/c2) mass, to be achieved during a 5 yr run producing an exposure of 100 t yr free from any instrumental background.

Aalseth, Craig E.↗

NASA NTRS2013

A Search for Amino Acids and Nucleobases in the Martian Meteorite Roberts Massif 04262 Using Liquid Chromatography-Mass Spectrometry

The investigation into whether Mars contains signatures of past or present life is of great interest to science and society. Amino acids and nucleobases are compounds that are essential for all known life on Earth and are excellent target molecules in the search for potential Martian biomarkers or prebiotic chemistry. Martian meteorites represent the only samples from Mars that can be studied directly in the laboratory on Earth. Here, we analyzed the amino acid and nucleobase content of the shergottite Roberts Massif (RBT) 04262 using liquid chromatography-mass spectrometry. We did not detect any nucleobases above our detection limit in formic acid extracts; however, we did measure a suite of protein and nonprotein amino acids in hot-water extracts with high relative abundances of beta-alanine and gamma-amino-eta-butyric acid. The presence of only low (to absent) levels of several proteinogenic amino acids and a lack of nucleobases suggest that this meteorite fragment is fairly uncontaminated with respect to these common biological compounds. The distribution of straight-chained amine-terminal eta-omega-amino acids in RBT 04262 resembled those previously measured in thermally altered carbonaceous meteorites. A carbon isotope ratio of -24(0/00) +/- 6(0/00) for beta-alanine in RBT 04262 is in the range of reduced organic carbon previously measured in Martian meteorites (Steele et al. 2012). The presence of eta-omega-amino acids may be due to a high temperature Fischer-Tropschtype synthesis during igneous processing on Mars or impact ejection of the meteorites from Mars, but more experimental data are needed to support these hypotheses.

Laboratory analysis↗

DOE OSTI2017

Magnetic iron oxide nanoparticles for the collection and direct measurement of adsorbed alpha-emitting radionuclides from environmental waters by liquid scintillation analysis

Radioactive contamination in the environment, be it from accidental or intentional release, can create an urgent need to assess water and food supplies, the environment, and monitor human health. Alpha-emitting radionuclides represent the most ionizing, and therefore the most damaging, form of radiation when internalized. Additionally, because of its ease of energy attenuation in solids or liquids, alpha emissions cannot be reliably monitored using non-destructive means. In the event of such an emergency, rapid and efficient methods will be needed to screen scores of samples (food, water, and human excreta) within a short time window. Unfortunately, the assay of alpha-emitting radionuclides using traditional radioanalytical methods is typically labor intensive and time consuming. The creation of analytical counting sources typically requires a series of chemical treatment steps to achieve well performing counting sources. In an effort to devise radioanalytical methods that are fast, require little labor, and minimize the use of toxic or corrosive agents, researchers at PNNL have evaluated magnetite (Fe3O4) nanoparticles as extracting agents for alpha-emitting radionuclides from chemically unmodified aqueous systems. It is demonstrated that bare magnetic nanoparticles exhibit high affinity for representative α-emitting radionuclides (241Am and 210Po) from representative aqueous matrices: river and ground water. Furthermore, use of the magnetic properties of these materials to concentrate the sorbed analyte from the bulk aqueous solution has been demonstrated. The nanoparticle concentrate can be either directly dispensed into scintillation cocktail, or first dissolved and then added to scintillation cocktail as a solution for alpha emission assay by liquid scintillation analysis. Despite the extreme quench caused by the metal oxide suspensions, the authors have demonstrated that quench correction features available on modern liquid scintillation analyzers can be employed to assure that quench-induced analytical biases can be avoided.

actinide↗

DOE OSTI2026

Sustainable extraction of rare earth elements from coal fly ash leachates using a recyclable ionic liquid

The growing demand for rare earth elements (REEs) has prompted interest in their recovery from alternative sources such as coal fly ash (CFA). This study explores the ionic liquid (IL) betainium bis(trifluoromethylsulfonyl)imide, [Hbet][Tf 2 N], for selective extraction of REEs from leachates of a Class C CFA. While previous studies have demonstrated the effectiveness of using [Hbet][Tf 2 N] to extract REEs from different types of CFA in direct ash-IL systems, this study investigates four CFA leachates prepared using HCl, HNO 3 , H 2 SO 4 , and citrate. Extraction experiments were conducted across varying pH levels and with additives such as ascorbic acid and betaine. Among the systems tested, [Hbet][Tf 2 N] achieved REE recoveries of 51% and 47% from the HCl and citrate leachates, respectively, comparable to 49% REE recovery in ash-IL extraction. Co-extraction of bulk elements was significantly reduced in the leachate-IL systems. Optimal REE extraction occurred near pH 11, and addition of ascorbic acid effectively suppressed iron co-extraction without compromising REE recovery. Recycling experiments demonstrated that [Hbet][Tf₂N] retains its performance over five cycles with manageable losses. These results reveal the promise of [Hbet][Tf 2 N] for effectively recovering REEs from leachates of solid wastes, highlighting its applicability as a sustainable strategy for other aqueous REE feedstocks.

chemistry↗