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At least 1,297 records · Page 72
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Surveying Phase Modifier Functional Groups for Applications to Ln(III) Separations

The application of N,N,N',N'-tetraoctyl diglycolamide (TODGA) in solvent extraction systems for lanthanide (Ln) separations is well understood. In these systems, the formation of a third phase has motivated the use of phase modifiers to enable higher concentrations of H + and Ln common to industrial processes. Several different phase modifiers with applications to diglycolamide (DGA) systems have previously been reported, with a focus on tri-n-butyl phosphate (TBP), N,N'-dihexylactanamide (DHOA), N,N-dioctyl-2-hydroxyacetamide (DOHyA), N,N'-dimethyl-N,N'-dioctylhexylethoxy malonamide (DMDOHEMA), and octanol. While the primary utility of phase modifiers is the increased metal loading, they can have significant effects on the metal distribution ratios, which are well described by the energetics of the extraction process itself. However, the mechanisms by which phase modifiers impact distribution ratios are not generally understood. This work considers the ability of phase modifiers to affect Ln distribution ratios by using phase modifiers with two different functional groups (–Cl and –C≡N) and an octyl alkyl chain in a TODGA and n-dodecane system. Determining the effect of chlorooctane and octane nitrile is important for understanding how phase modifier functional groups and their hydrogen bonding interactions affect Ln extraction. Through combining distribution ratio measurements with organic phase spectroscopic investigations, the impact of chlorooctane and octane nitrile on Ln extraction and their inner-sphere complexes is reported. The addition of either chlorooctane or octane nitrile to TODGA in n-dodecane decreases Ln extraction while maintaining the same inner-sphere Ln complex. The lack of change in inner-sphere Ln-TODGA coordination upon incorporation of phase modifiers and the significant impact of these phase modifiers on distribution ratios suggest the importance of a supramolecular structure. Understanding the role of chlorooctane and octane nitrile on the organic phase structure at longer length scales has been identified as an avenue for future investigations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Antiferromagnetism-driven two-dimensional topological nodal-point superconductivity

Magnet/superconductor hybrids (MSHs) hold the promise to host emergent topological superconducting phases. Both one-dimensional (1D) and two-dimensional (2D) magnetic systems in proximity to -wave superconductors have shown evidence of gapped topological superconductivity with zero-energy end states and chiral edge modes. Recently, it was proposed that the bulk transition-metal dichalcogenide 4Hb-TaS 2 is a gapless topological nodal-point superconductor (TNPSC). However, there has been no experimental realization of a TNPSC in a MSH system yet. Here we present the discovery of TNPSC in antiferromagnetic (AFM) monolayers on top of an s-wave superconductor. Our calculations show that the topological phase is driven by the AFM order, resulting in the emergence of a gapless time-reversal invariant topological superconducting state. Using low-temperature scanning tunneling microscopy we observe a low-energy edge mode, which separates the topological phase from the trivial one, at the boundaries of antiferromagnetic islands. As predicted by the calculations, we find that the relative spectral weight of the edge mode depends on the edge’s atomic configuration. Our results establish the combination of antiferromagnetism and superconductivity as a novel route to design 2D topological quantum phases.

30 DIRECT ENERGY CONVERSION↗
NASA NTRS1982

Studies on aqueous two phase polymer systems useful for partitioning of biological materials

The two phase systems that result when aqueous solutions of dextran and poly(ethylene glycol) (PEG) are mixed above a critical concentration of a few percent provide a useful medium for the separation of biological cell subpopulations via partition between the top, PEG-rich phase and the liquid-liquid phase boundary. Interfacial tensions of such systems have been measured by the rotating drop technique and found to range between 0.1-100 micro-N/m. The tension was found to depend on the length of the tie line describing the system on a phase diagram, via a power law relationship which differed depending on the concentration of Na phosphate buffer present. The electrokinetic properties of drops of one phase suspended in the other were studied for a variety of systems. It was found that the droplet electrophoretic mobility increased monotonically with phosphate concentration and drop diameter but exhibited the opposite sign from that anticipated from phosphate partition measurements. It was possible to take advantage of these electrokinetic properties and dramatically enhance the speed of phase separation through application of relatively small electric fields.

Brooks, D. E.↗
NASA NTRS2014

Physics Based Model for Cryogenic Chilldown and Loading. Part IV: Code Structure

This is the fourth report in a series of technical reports that describe separated two-phase flow model application to the cryogenic loading operation. In this report we present the structure of the code. The code consists of five major modules: (1) geometry module; (2) solver; (3) material properties; (4) correlations; and finally (5) stability control module. The two key modules - solver and correlations - are further divided into a number of submodules. Most of the physics and knowledge databases related to the properties of cryogenic two-phase flow are included into the cryogenic correlations module. The functional form of those correlations is not well established and is a subject of extensive research. Multiple parametric forms for various correlations are currently available. Some of them are included into correlations module as will be described in details in a separate technical report. Here we describe the overall structure of the code and focus on the details of the solver and stability control modules.

cryogenic fluid management↗
DOE OSTI2023

Quantitative Separation of Unknown Organic–Metal Complexes by Liquid Chromatography–Inductively Coupled Plasma-Mass Spectrometry

Dissolved organic matter (DOM) is widely recognized to control the solubility and reactivity of trace metals in the environment. However, the mechanisms that govern metal-DOM complexation remain elusive, primarily due to the analytical challenge of fractionating and quantifying metal–organic species within the complex mixture of organic compounds that comprise DOM. Here, we describe a quantitative method for fractionation and element-specific detection of organic–metal complexes using liquid chromatography with online inductively coupled plasma mass spectrometry (LC–ICP-MS). The method implements a post-column compensation gradient to stabilize ICP–MS elemental response across the LC solvent gradient, thereby overcoming a major barrier to achieving quantitative accuracy with LC–ICP-MS. With external calibration and internal standard correction, the method yields concentrations of organic–metal complexes that were consistently within 6% of their true values, regardless of the complex’s elution time. We used the method to evaluate the effects of four stationary phases (C18, phenyl, amide, and pentafluoroylphenyl propyl) on the recovery and separation of environmentally relevant trace metals (Mn, Fe, Co, Ni, Cu, Zn, Cd, and Pb) in Suwannee River Fulvic Acid and Suwannee River Natural Organic Matter. The C18, amide, and phenyl phases generally yielded optimal metal recoveries (>75% for all metals except Pb), with the phenyl phase separating polar species to a greater extent than C18 or amide. We also fractionated organic-bound Fe, Cu, and Ni in oxidized and reduced soils, revealing divergent metal-DOM speciation across soil redox environments. Finally, by enabling quantitative fractionation of DOM-bound metals, our method offers a means for advancing a mechanistic understanding of metal–organic complexation throughout the environment.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1989

Cell separation in immunoaffinity partition in aqueous polymer two-phase systems

Two methods for immunoaffinity partitioning are described. One technique involves the covalent coupling of poly (ethylene glycol) (PEG) to immunoglobulin G antibody preparations. In the second method PEG-modified Protein A is used to complex with cells and unmodified antibody. The effects of PEG molecular weight, the degree of modification, and varying phase system composition on antibody activity and its affinity for the upper phase are studied. It is observed that both methods resulted in effective cell separation.

Karr, Laurel J.↗
NASA NTRS1983

Low-gravity experiments on Liquid Phase Miscibility Gap (LPMG) alloys: Materials Experiments Assembly (MEA)

Space shuttle experiments which study the massive separation which occurred during sounding rocket Al-In alloy tests are described. The gradient cool experiment studies surface tension driven droplet migration and particle pushing in an LPMG alloy. Isothermal experiments on the Te-Tl alloys test the hypothesis that LPMG systems with low surface energies produce relatively fine, and uniform emulsions and dispersions. It also examines the effect of droplet concentration on phase separation kinetics. Isothermal plunger experiments on Al-In alloys determine whether surface tension driven convection currents originating at a free surface contribute to massive separation. They ascertain whether In-rich droplets migrate under the action of a temperature gradient when they are not influenced by the crucible walls.

Gelles, S. H.↗
NASA NTRS1988

Applications of nuclear power to lunar and Mars missions

The initial elements of an ambitious program for human exploration beyond Earth have been developed and presented to NASA management for its consideration. The Outpost on the Moon and Humans to Mars are two key U.S. programs (Ride 1987). A major space goal of this magnitude can only be implemented by a series of program phases evolving from precursor robotic missions, to initial development of temporary surface stations and buildup of operational experience, through the eventual establishment of permanent and sustained surface bases. Each phase of the separate (or linked) lunar and Mars scenarios will require distinctly different levels and types of power sources to support both transportation and on-surface operations, i.e., the nuclear power reactor. Discussed are the respective types and specific amounts of power required for all major systems in a phased program of lunar and Mars exploration over the period 1990 to 2040. A comparative assessment of technology tradeoffs and special design problems is made to ascertain the most appropriate application for the different phases, as well as to identify synergistic developments across the programs.

Friedlander, Alan↗
NASA NTRS2020

DGEN Aeropropulsion Research Turbofan Source-Diagnostic Test: Experimental Setup and Acoustic-Data Structure

The experimental setup of, and available data from a recent core/combustor-noise source-diagnostic test utilizing a small turbofan engine are described. The 2019 test campaign continued the investigation of the core/combustor-noise component of aircraft-propulsor noise begun in an earlier baseline test, but with a more extensive acoustic-instrumentation layout. The purpose of both tests was to better understand the impact on civilian-transport airport-community noise from turbofan-combustor sources and thereby to lay the foundation for improved noise-prediction methods and noise-mitigation techniques. Simultaneous high-data-rate acoustic measurements were obtained using a circumferential sensor array at the core nozzle exit in conjunction with sideline and farfield microphone arrays. The test matrix contained engine operational points from engine idle to maximum power and was repeated for different circumferential and sideline array configurations, as well as for redundancy. The extensive data set (up to 93 channels of data and various configurations) allows the application of advanced source-separation and phased-array methods to elucidate not only the core-noise structure, but also the propagation characteristics of other propulsion noise sources. The present report provides a detailed description of the different test points, their associated instrumentation layouts, and the structure of the acquired data set. Results from various data analyses are reported separately.

Aeroacoustics↗
DOE OSTI2026

Vanishing dynamic strength measured in a transient high-pressure phase of tin

This work reports two independent experimental estimations of the dynamic strength of the body-centered tetragonal (bct) 𝛾 phase of tin, which occurs at pressures above about 9 GPa and transforms promptly back to the ambient 𝛽 phase upon pressure release. Measuring strength in such a transient high-pressure phase is challenging. One measurement used free-surface Richtmyer-Meshkov instabilities generated with gas gun impact. Another set of measurements used ramp-release loading in a pulsed-power facility. Strength estimations came from comparison to simulations using a comprehensive multiphase modeling framework that includes equation of state, shear moduli, and strength separately for each phase, and treats mixed-phase regions. Both experimental methods found the 𝛾-phase strength to be very low, within experimental uncertainty of zero. The existing literature on other materials, by contrast, almost universally reports higher strength in transient high-pressure phases compared with ambient phases. Recent Molecular-Dynamics simulations on tin in the literature showed almost zero deviatoric strength during a deformation-induced bct → bct transformation in which one of the 𝛾-phase 𝑎 axes “flips” to the 𝑐 axis. This reorientation currently provides the most plausible explanation for the low observed strength in 𝛾-phase tin.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Silver-mediated separations: A comprehensive review on advancements of argentation chromatography, facilitated transport membranes, and solid-phase extraction techniques and their applications

The use of silver(I) ions in chemical separations, also known as argentation separations, is a powerful approach for the selective separation and analysis of many natural and synthetic organic compounds. In this review, a comprehensive discussion of the most common argentation separation techniques, including argentation-liquid chromatography (Ag-LC), argentation-gas chromatography (Ag-GC), argentation-facilitated transport membranes (Ag-FTMs), and argentation-solid phase extraction (Ag-SPE) is provided. For each of these techniques, notable advancements, optimized separations, and innovative applications are discussed. The review begins with an explanation of the fundamental chemistry underlying argentation separations, mainly the reversible π-complexation between silver(I) ions and carbon-carbon double bonds. Within Ag-LC, the use of silver(I) ions in thin-layer chromatography, high-performance liquid chromatography, as well as preparative LC are explored. This discussion focuses on how silver(I) ions are employed in the stationary and mobile phase to separate unsaturated compounds. For Ag-GC and Ag-FTMs, different silver compounds and supporting media are discussed, often with relation to olefin-paraffin separations. Ag-SPE has been widely employed for the selective extraction of unsaturated compounds from complex matrices in sample preparation. This comprehensive review of Ag-LC, Ag-GC, Ag-FTMs, and Ag-SPE techniques emphasizes the immense potential of argentation separations in separations science and serves as a valuable resource for researchers seeking to learn, optimize, and utilize argentation separations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Experimental and modeling studies of IPDI-based polyurea elastomers – The role of hard segment fraction

Segmented polyureas (PUa) are industrially important class of polymers widely used in coatings, sealant, and adhesive applications. Here, in this paper, we report synthesis, characterization, and modeling of Isophorone Diisocyanate-Diethyl-Toluene-Diamine-Polyether amine (IPDI-DETDA-PO PUa) with varied hard segment contents of 20, 30, and 40 weight percent. For each of the three materials, we study its structure and phase behavior using FTIR, DSC, and TEM, and clearly show the presence of microphase separation between the hard and soft nanodomains. We then measure the linear viscoelastic response of the PUa-s using DMA (frequency sweeps at multiple temperatures). The DMA data are shown to obey the time-temperature superposition. Finally, we develop a new micromechanical model describing the DMA results; the model describes a phase-separated PUa as two “Fractional-order Maxwell gels” branches, connected in parallel, with the first FMG branch representing the “percolated hard phase" and the second one modeling the “filled soft phase". In agreement with the earlier thermodynamic theories, the volume-fraction of the percolated hard phase is related to the hard segment weight-fraction (HSWF), defined as the combined mass of IPDI and DETDA normalized to the total mass of the polymer. The data and model are found to be in a good qualitative and quantitative agreement.

36 MATERIALS SCIENCE↗
NASA NTRS2012

Wavefront Sensing for WFIRST with a Linear Optical Model

In this paper we develop methods to use a linear optical model to capture the field dependence of wavefront aberrations in a nonlinear optimization-based phase retrieval algorithm for image-based wavefront sensing. The linear optical model is generated from a ray trace model of the system and allows the system state to be described in terms of mechanical alignment parameters rather than wavefront coefficients. This approach allows joint optimization over images taken at different field points and does not require separate convergence of phase retrieval at individual field points. Because the algorithm exploits field diversity, multiple defocused images per field point are not required for robustness. Furthermore, because it is possible to simultaneously fit images of many stars over the field, it is not necessary to use a fixed defocus to achieve adequate signal-to-noise ratio despite having images with high dynamic range. This allows high performance wavefront sensing using in-focus science data. We applied this technique in a simulation model based on the Wide Field Infrared Survey Telescope (WFIRST) Intermediate Design Reference Mission (IDRM) imager using a linear optical model with 25 field points. We demonstrate sub-thousandth-wave wavefront sensing accuracy in the presence of noise and moderate undersampling for both monochromatic and polychromatic images using 25 high-SNR target stars. Using these high-quality wavefront sensing results, we are able to generate upsampled point-spread functions (PSFs) and use them to determine PSF ellipticity to high accuracy in order to reduce the systematic impact of aberrations on the accuracy of galactic ellipticity determination for weak-lensing science.

Jurling, Alden S.↗
DOE OSTI2026

Temperature-dependent changes in gas chromatographic separation metrics for trihexyl(tetradecyl)phosphonium-based ionic liquid stationary phases and comparison to conventional polysiloxane stationary phases

Here, to assess whether the trihexyl(tetradecyl)phosphonium chloride ([P 66614 + ][Cl - ]) ionic liquid (IL), employed as a gas chromatographic stationary phase, exhibits temperature-dependent phase transitions or structural heterogeneity, retention thermodynamics for probe molecules of varied chemical structure were investigated by gas chromatography (GC) over the temperature range of 25 to 64 °C using van’t Hoff analysis. All van’t Hoff plots for n-alkanes (C8–C12) and other probe analytes were linear, indicating the absence of detectable phase-transition behavior. The [P 66614 + ][Cl - ] IL was further compared with the [P 66614 + ] bis[(trifluoromethyl)sulfonyl]imide ([P 66614 + ][NTf 2 - ]) IL and commercial polysiloxane stationary phases in terms of temperature-dependent resolution behavior and chromatographic selectivity over the temperature range of 28–52 °C. The resolution factors of analytes in mixtures obtained using gas chromatography–mass spectrometry (GC–MS) and the summation of resolution values decreased smoothly with temperature on both IL stationary phases and on the dimethylphenylcyano-substituted polymeric stationary phase (OV-1701), whereas the poly(50% diphenyl/50% dimethyl siloxane) stationary phase (SPB-50) exhibited irregularities in its temperature-dependent summation of resolution profile, showing a distinct maximum in the temperature range of 34–40 °C. Selectivity values for the IL stationary phases were largely determined by the anion, with the [P 66614 + ][Cl - ] IL providing enhanced separation between polar and aromatic analytes, while the [P 66614 + ][NTf 2 - ] IL favored dispersive and π-π interactions that resulted in a reversal of elution order for some aliphatic–aromatic and alkyne-containing analyte pairs. Capillary columns prepared using different surface activation methods and coated with identical [P 66614 + ][Cl - ] IL stationary phase showed indistinguishable temperature-dependent trends in summation of resolution value and selectivity. An evaluation of analyte-specific selectivity provides insight into the characteristic separation behavior of the stationary phases and enables identification of analyte classes that are more efficiently separated on the [P 66614 + ]-based IL stationary phases compared to conventional stationary phase materials.

Chromatographic selectivity↗
DOE OSTI2025

Extraction and Separation of Rare-Earth Elements from Coal Fly Ash and Leachate using a Recyclable Ionic Liquid

Coal fly ash (CFA) can be a promising source for recovering rare-earth elements (REEs), as it contains a broad range of REEs with average concentrations frequently exceeding those in traditional rare earth mines. Recent research from our group has demonstrated that REEs can be preferentially extracted from CFA solids using a recyclable ionic liquid (IL), betainium bis-(trifluoromethylsulfonyl)imide ([Hbet][Tf2N]). When CFA was heated with the mixture of IL and an aqueous solution above 65°C, most leached REEs partitioned into the IL phase and were separated from the bulk elements. Subsequent acid stripping of the REE-loaded IL removed the REEs and regenerated the IL for reuse in multiple extraction cycles. This IL-based REE-CFA recovery method has been applied to ten CFA samples derived from different coal sources, including ash recovered from disposal ponds. Analysis of 34 elements confirmed the process consistently achieved high REE recovery efficiency, with strong selectivity over bulk and trace elements across diverse CFA types. In addition to the IL-solid extraction, the performance of [Hbet][Tf2N] in extracting REEs from fly-ash leachates have been evaluated by four commonly used leaching reagents, including HCl, HNO3, H2SO4, and citrate. During the IL-leachate extraction, [Hbet][Tf2N] was mixed and heated with a Class C fly ash leachate generated from each leaching reagent, followed by an acid stripping. It was observed that the partitioning and recovery of REEs increased as the leachate pH increased from 3 to 11. Among the investigated leachates, HCl and citrate proved to be the most compatible with IL extraction, exhibiting a slightly higher REE recovery and a lower non-REE co-extraction compared to the IL-solid extraction. Sc, Y, Nd, Sm, Gd, Dy, and Yb consistently showed a high recovery rate from both CFA solids and leachates. Notably, Pr, Tb, and Ho, which were not previously leached from the CFA solids, were partially recovered from the leachates. Overall, our studies revealed the strong potential of [Hbet][Tf2N] for effectively recovering REEs from leachates, highlighting its applicability as a sustainable strategy for other aqueous REE feedstocks. Furthermore, a techno-economic analysis will be performed to quantify the economic viability of the IL-based REE recovery method and guide future process improvement.

42 ENGINEERING↗
DOE OSTI2025

Approaches for Water Removal in Direct-Fired sCO 2 Power Cycles

There is interest in investigation of water removal processes in direct fired sCO 2 flows, as this may potentially lead to greater system efficiency as the removal of this contaminant will result in sCO 2 behaving close to idealized behaviors. Water removal should be split into a two-step process, condensation of the water, followed by separation of the liquid phase water from the sCO 2 . The two main avenues of condensation are manipulation of pressure and temperature for phase change. For this paper, temperature-based phase change is the primary focus through the implementation of heat exchangers. Of the heat exchangers investigated it was found that printed circuit heat exchangers (PCHEs) could be an alternative for this use case, though the specific design of flow channel geometry and flow direction depends on the specific system case and cannot be determined at this point. For water separation there were four processes identified, all of which already assume water is in liquid phase at that point in the system. Of these separation avenues the best candidate is the hydrocyclone as it has a proven history of separating liquid-liquid phase mixtures with small density differences in oilfield use, in addition they have been investigated and modeled specifically for water separation for sCO 2 flows and the footprint is relatively small.

20 FOSSIL-FUELED POWER PLANTS↗
NASA NTRS1980

Transverse injection of a particle-laden liquid jet in supersonic flow: A three-phase flow

The results of a two part study of the behavior of particle laden liquid jets injected into air are presented. Water was used as the liquid carrier and either 1-37 or 13-44 microns diam. spherical glass beads with a specific gravity of 2.8-3.0 as the particles. The observations were mainly photographic. The breakup of jets injected into still air was investigated as a function of particle loading, and the results were compared to the pure liquid jet case. The jets were found to be more stable with particles present. The length to breakup was increased, and the formation of satellite droplets was suppressed. The penetration and breakup of transverse jets in a Mach 3.0 air stream was studied. The general breakup mechanism of wave formation was found to be the same as for the all liquid case. Significant separation of the phases was observed, and the penetration of the liquid phase was reduced compared to all liquid cases at the same value of the jet to free stream momentum flux ratio.

Schetz, J. A.↗