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DOE OSTI2013

Evaluating ion exchange resin efficiency and oxidative capacity for the separation of uranium(IV) and uranium(VI)

Background: Previously described methods to separate dissolved U(IV) from dissolved U(VI) under acidic anoxic conditions prior to laboratory analysis were ineffective with materials currently available commercially. Three strong anion exchange resins were examined for their efficiency in separating, recovering, and preserving both redox states during separation. Results: Under oxic conditions, recovery of U(VI) from three exchange resins (Bio-Rad AG® 1x8 Poly-Prep® prefilled columns, Bio-Rad AGW 1x8 powder, and Dowex® 1x8 powder) ranged from 72% to 100% depending on the dosed mass, eluent volume, and resin selected. Dowex® 1x8 resin was the only resin found to provide 100% recovery of U (VI) with fewer than 5 bed volumes of eluent. Under anoxic conditions, all three resins oxidized U(IV) in aqueous solutions with relatively low U(IV) concentrations (<3x10-6 M). Resin-induced oxidation was observed visually using a leuco dye, safranin-o. Oxidants associated with the resin were irreversibly reduced by the addition of Ti(III). After anoxic resin pre-treatment, a series of U(IV)/U(VI) mixtures at micro-molar levels were prepared and separated using the Dowex® 1x8 resin with 100% recovery of both U(IV) and U(VI) with no resin-induced changes in oxidation state. Conclusions: Currently available anion exchange resins with apparently identical physical properties were found to have significantly different recoveries for hexavalent uranium at micro-molar concentrations. A novel qualitative technique was developed to visually assess oxidative capacities of anion exchange resins under acidic anoxic conditions. A protocol was developed for pre-treatment and use of currently available anion exchange resins to achieve quantitative separation of U(IV) and U(VI) in aqueous solutions with low U(IV) concentrations. This method can be applied to future work to quantitatively assess dissolved U(IV) and U(VI) concentrations in both laboratory and field samples.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

Synthesis and analysis of separation networks for the recovery of intracellular chemicals generated from microbial-based conversions

Background. Bioseparations can contribute to more than 70% in the total production cost of a bio-based chemical, and if the desired chemical is localized intracellularly, there can be additional challenges associated with its recovery. Based on the properties of the desired chemical and other components in the stream, there can be multiple feasible options for product recovery. These options are composed of several alternative technologies, performing similar tasks. The suitability of a technology for a particular chemical depends on (1) its performance parameters, such as separation efficiency; (2) cost or amount of added separating agent; (3) properties of the bioreactor effluent (e.g., biomass titer, product content); and (4) final product specifications. Our goal is to first synthesize alternative separation options and then analyze how technology selection affects the overall process economics. To achieve this, we propose an optimization-based framework that helps in identifying the critical technologies and parameters. Results. We study the separation networks for two representative classes of chemicals based on their properties. The separation network is divided into three stages: cell and product isolation (stage I), product concentration (II), and product purification and refining (III). Each stage exploits differences in specific product properties for achieving the desired product quality. The cost contribution analysis for the two cases (intracellular insoluble and intracellular soluble) reveals that stage I is the key cost contributor (>70% of the overall cost). Further analysis suggests that changes in input conditions and technology performance parameters lead to new designs primarily in stage I. Conclusions. The proposed framework provides significant insights for technology selection and assists in making informed decisions regarding technologies that should be used in combination for a given set of stream/product properties and final output specifications. Additionally, the parametric sensitivity provides an opportunity to make crucial design and selection decisions in a comprehensive and rational manner. This will prove valuable in the selection of chemicals to be produced using bioconversions (bioproducts) as well as in creating better bioseparation flow sheets for detailed economic assessment and process implementation on the commercial scale.

09 BIOMASS FUELS↗

DOE OSTI2016

Ultem ® /ZIF-8 mixed matrix membranes for gas separation: Transport and physical properties

Mixed matrix membranes are promising options for improving gas separation processes. Zeolitic imidazolate frameworks (ZIFs) have a porous structure similar to conventional zeolites, being capable in principle of separating gases based on their differences in kinetic diameter while offering the advantage of having a partial organic character. This partial organic nature improves the compatibility between the sieve and the polymer, and a combination of the mentioned characteristics makes these hybrid materials interesting for the preparation of mixed matrix gas separation membranes. In this context the present work reports the preparation of Ultem ® /ZIF-8 mixed matrix membranes and their permeabilities to pure CO 2 , N 2 and CH 4 gases. A significant increase in permeability with increase in CO 2 /N 2 selectivity was observed for the mixed matrix systems as compared to the properties of the neat Ultem ® . Sorption results allowed to speculate that the ZIF-8 framework is not completely stable dimensionally, what influences the separation process by allowing gases with higher kinetic diameter than its nominal aperture to be sorbed and to diffuse through the crystal. Lastly, sorption and diffusion selectivities indicate that the higher separation performance of the mixed matrix membranes is governed by the diffusion process associated with the influence of gas molecule´s geometry.

36 MATERIALS SCIENCE↗

DOE OSTI2015

Separation of tritiated water using graphene oxide membrane

In future nuclear fuel reprocessing plants and possibly for nuclear power plants, the cleanup of tritiated water will be needed for hundreds of thousands of gallons of water with low activities of tritium. This cleanup concept utilizes graphene oxide laminar membranes (GOx) for the separation of low-concentration (10 -3 -10 µCi/g) tritiated water to create water that can be released to the environment and a much smaller waste stream with higher tritium concentrations. Graphene oxide membranes consist of hierarchically stacked, overlapping molecular layers and represent a new class of materials. A permeation rate test was performed with a 2-µm-thick cast Asbury membrane using mixed gas permeability testing with zero air (highly purified atmosphere) and with air humidified with either H 2 O or D 2 O to a nominal 50% relative humidity. The membrane permeability for both H 2 O and D 2 O was high with N 2 and O 2 at the system measurement limit. The membrane water permeation rate was compared to a Nafion® membrane and the GOx permeation was approximately twice as high at room temperature. The H 2 O vapor permeation rate was 5.9 × 10 2 cc/m 2 /min (1.2 × 10 -6 g/min-cm 2 ), which is typical for graphene oxide membranes. To demonstrate the feasibility of such isotopic water separation through GOX laminar membranes, an experimental setup was constructed to use pressure-driven separation by heating the isotopic water mixture at one side of the membrane to create steam while cooling the other side. Several membranes were tested and were prepared using different starting materials and by different pretreatment methods. The average separation result was 0.8 for deuterium and 0.6 for tritium. Higher or lower temperatures may also improve separation efficiency but neither has been tested yet. A rough estimate of cost compared to current technology was also included as an indication of potential viability of the process. The relative process costs were based on the rough size of facility to accommodate the large surface area of the membranes and the energy needed to evaporate the water and pass through the membranes as compared to the currently used combined electrolysis and catalytic exchange process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

A Physicochemical Method for Separating Rare Earths: Addressing an Impending Shortfall

There are currently zero operating suppliers of critical rare earth elements La–Lu, Sc, Y (REs), in the western hemisphere. REs are critical materials due to their importance in clean energy and defense applications, including permanent magnets in wind turbines and phosphors in energy efficient lighting. It is not economically viable to produce pure REs in the U.S. given current separations technology. REs production is dominated by suppliers in the People’s Republic of China (PRC) because of their capacity in liquidliquid solvent extraction (SX) used to purify mixtures. Weak environmental regulations in the PRC also contribute to a competitive advantage. SX is a cost, time, solvent and waste intensive process but is highly optimized and scalable. The low efficiency of SX derives from the small thermodynamic differences in solvation enthalpy between the RE3+ cations. To foster stable domestic RE production there is a critical need for fundamentally new REs chemistry that contributes to disruptive technologies in RE separations. The overall goal of this project was to develop new thermodynamic bases, and apply them, for the solution separation of rare earth metals. We have developed the chemistry of rare earth metals: La–Lu, Sc and Y, with redox active ligands. Our hypothesis for the project was that electronhole coupling in complexes of certain lanthanide metals with redox active ligands can be used to manifest chemical distinctiveness and affect separations. We also developed separations based on unique solution equilibria from tailored ligands.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2023

Fundamental Structure/Property Studies of Gas Separation Membrane Polymers

Solution-processable polybenzimidazoles (PBIs) present opportunities for new gas separation membranes. We plan to develop systematic structure/property relations for this relatively new class of membrane materials. The fundamental questions we will address are: (1) How do chemical structure modifications of PBIs influence their gas solubility, diffusivity and permeability properties for a systematic series of gases? (2) Is the separation performance of PBIs affected by plasticization under operating conditions that are relevant to, for example, natural gas purification or olefin/paraffin separation and, if so, can this family of materials be tuned structurally to minimize deleterious effects of plasticization on separation properties? (3) What is the effect of water vapor on PBI separation performance? (4) What is the influence of physical aging on permeation properties of thin (i.e., <1 µm) PBI polymer films, and how does the rate of physical aging relate to polymer chemical structure? The primary focus of this research program is to develop a fundamental, molecular-based mechanistic understanding of the influence of chemical structure on the gas transport properties of PBIs and to establish structure/property relationships for this unique platform of materials.

08 HYDROGEN↗

DOE OSTI2026

Liquid centrifugation-based isotope separation of 7 Li, 37 Cl and D

Liquid centrifugation is an emerging method to separate isotopes. By spinning a liquid containing target isotopes (e.g., pure chemical or solution), the heavier isotope will be enriched at the outer part of a centrifuge, and the lighter ones will be enriched at the inner part of a centrifuge. The separation capability is positively correlated with rotation speed, outer radius and mass difference between isotopes to separate. This award targets to understand whether liquid centrifugation is effective in separating isotopes important for nuclear fission technologies. The results include the following three sections: 1) Effects of solute concentration on isotope separation; 2) Preliminary progress of building a low-speed countercurrent centrifuge, and 3) Analysis on possible candidates for 7 Li and 37 Cl. The award trained one research scientist, one Ph.D. student, one master student, and one undergraduate on liquid centrifugation and isotope measurements.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2015

Size-separation of silver nanoparticles using sucrose gradient centrifugation

Size and shape distributions of nanoparticles can drastically contribute to the overall properties of nanoparticles, thereby influencing their interaction with different chemotherapeutic molecules, biological organisms and or materials and cell types. Therefore, to exploit the proper use of nanoparticles for various biomedical and biosensor applications, it is important to obtain well-separated monodispersed nanoparticles. However, gaining precise control over the morphological characteristics of nanoparticles during their synthesis is often a challenging task. Consequently, post-synthesis separation of nanoparticles is necessary. In the present study, we demonstrate the successful one-pot post-synthesis separation of anisotropic silver nanoparticles to near modispersities using sucrose density gradient sedimentation. The separation of the nanoparticles was evidenced based on optical confirmation, and spectrophotometric and transmission electron microscopy measurements. Our results clearly demonstrate the facile separation of anisotropic silver nanoparticles using sucrose density gradient sedimentation and can enable the use of nanoparticles for various biomedical applications.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

NASA NTRS2008

Architecture Study on Telemetry Coverage for Immediate Post-Separation Phase

This document is the viewgraphs that accompanies a paper that presents the preliminary results of an architecture study that provides continuous telemetry coverage for NASA missions for immediate post-separation phase. After launch when the spacecraft separated from the upper stage, the spacecraft typically executes a number of mission-critical operations prior to the deployment of solar panels and the activation of the primary communication subsystem. JPL, GSFC, and APL have similar design principle statements that require continuous coverage of mission-critical telemetry during the immediate post-separation phase. To conform to these design principles, an architecture that consists of a separate spacecraft transmitter and a robust communication network capable of tracking the spacecraft signals is needed. The main results of this study are as follows: 1) At low altitude (< 10000 km) when most post-separation critical operations are executed, Earth-based network (e.g. Deep Space Network (DSN)) can only provide limited coverage, whereas space-based network (e.g. Space Network (SN)) can provide continuous coverage. 2) Commercial-off-the-shelf SN compatible transmitters are available for small satellite applications. In this paper we present the detailed coverage analysis of Earth-based and Space-based networks. We identify the key functional and performance requirements of the architecture, and describe the proposed selection criteria of the spacecraft transmitter. We conclude the paper with a proposed forward plan.

architecture↗

NASA NTRS2015

Output-Based Adaptive Meshing Applied to Space Launch System Booster Separation Analysis

This paper presents details of Computational Fluid Dynamic (CFD) simulations of the Space Launch System during solid-rocket booster separation using the Cart3D inviscid code with comparisons to Overflow viscous CFD results and a wind tunnel test performed at NASA Langley Research Center's Unitary PlanWind Tunnel. The Space Launch System (SLS) launch vehicle includes two solid-rocket boosters that burn out before the primary core stage and thus must be discarded during the ascent trajectory. The main challenges for creating an aerodynamic database for this separation event are the large number of basis variables (including orientation of the core, relative position and orientation of the boosters, and rocket thrust levels) and the complex flow caused by the booster separation motors. The solid-rocket boosters are modified from their form when used with the Space Shuttle Launch Vehicle, which has a rich flight history. However, the differences between the SLS core and the Space Shuttle External Tank result in the boosters separating with much narrower clearances, and so reducing aerodynamic uncertainty is necessary to clear the integrated system for flight. This paper discusses an approach that has been developed to analyze about 6000 wind tunnel simulations and 5000 flight vehicle simulations using Cart3D in adaptive-meshing mode. In addition, a discussion is presented of Overflow viscous CFD runs used for uncertainty quantification. Finally, the article presents lessons learned and improvements that will be implemented in future separation databases.

Booster↗

NASA NTRS2015

Strategic Time-Based Metering that Assures Separation for Integrated Operations in a Terminal Airspace

This paper reports an algorithm for strategic time-based metering of air traffic arriving and departing from a large ( tens of nautical miles) area (called here, the commitment region) around an airport or metroplex. The algorithm assures separation continuously in time and avoids a dictation of intent to an aircraft crew. This is accomplished by allowing an aircraft (specifically, its Flight Management System) to specify, and commit to, an intended route and ground speed profile along that route within the commitment region, and by supplying the time at which to enter the region to the aircraft crew. The airspace that comprises the commitment region need not be confined to the terminal airspace and can include some of the enroute space: the size and shape of the commitment region are parameters in the algorithm. An exact formula for including speed profile uncertainty in the algorithm is provided. The algorithm is applied to a number of data sets recorded during actual air traffic operations in the Southern California TRACON in July of 2014 and the Atlanta TRACON in November and December of 2013. The results of the numerical simulations indicate that the algorithm succeeds at keeping the aircraft separated, but introduces, in its current implementation, more separation than that observed in actual operations. This excess separation can be reduced by modeling more accurately the Visual Flight Rules separation practices, a direction for future research.

air traffic management↗

NASA NTRSDate not supplied

Space Launch System Booster Separation Supersonic Powered Testing with Surface and Off-body Measurements

A wind tunnel test was run in the NASA Langley Unitary Plan Wind Tunnel simulating the separation of the two solid rocket boosters (SRB) from the core stage of the NASA Space LaunchSystem (SLS). The test was run on a 0.9% scale model of the SLS Block 1B Cargo (27005) configuration and the SLS Block 1B Crew (28005) configuration at a Mach of 4.0. The SRBs weremounted separately from the core, and could be pitched, yawed, and translated in the X, Y, andZ directions relative to the core. High pressure air was used to simulate plumes from the booster separation motors located at the nose and aft skirt of the two boosters. Force and moment data were taken on both SRBs and on the core stage. Schlieren still photos and video were recorded throughout testing. A set of points were acquired using Cross-correlation Doppler Global Velocimetry (CCDGV) readings to get 3 component velocity measurements between the core and the left-hand SRB. The CCDGV laser was utilized to record flow visualization in the same location, between the core and the left-hand SRB. Pressure Sensitive Paint (PSP) data were taken on a separate set of runs. Computational Fluid Dynamics (CFD) runs were computed on a subset of the wind tunnel data points for comparison. A combinationof the force and moment, CCDGV, and PSP data (as well as schlieren images) at the CFD-specified test conditions will be used to validate the CFD simulations that will be used to build an SLS booster separation database at flight conditions.

SLS↗

NASA NTRSDate not supplied

Informing the Space Launch System Booster Separation Initial CFD Run Matrix with Observed Parametric Sensitivity

It currently requires significant computational cost to simulate the flow physics of the booster separation event on the Space Launch System. This comes from the large parametric space in which the event occurs, as pre-separation flight conditions and separated booster core-relative trajectories can vary. Functionally removing the risk of core-booster collision mandates careful assessment of the fluid dynamics in terms of several trajectory parameters. However, simulating the entire trajectory envelope is computationally intractable given the high parametric dimension. In order to reduce the uncertainty in the resulting low-parametric-resolution aerodynamic booster separation database, a data-driven approach was developed to select which breakpoints should be studied by simulations and experiments and which should be relegated to a regression-based interpolation procedure. This technique works by simulating cases where the flow physics are most sensitive to changes in the parameters and leaving the less parametrically sensitive regions for interpolation. The result is a booster separation run matrix whose computational cost is comparable to that of previous database generations but has lower interpolation errors.

SLS↗

NASA NTRSDate not supplied

Informing the Space Launch System Booster Separation Initial CFD Run Matrix with Observed Parametric Sensitivity

SLS↗

NASA NTRSDate not supplied

Separation Assurance in Urban Air Mobility Systems Using Shared Scheduling Protocols

Ensuring safe separation between aircraft is a critical challenge in air traffic management, particularly in urban air mobility (UAM) environments where high traffic density and low altitudes require precise control. In these environments, conflicts often arise at the intersections of flight corridors, posing significant risks. We propose a tactical separation approach leveraging shared scheduling protocols, originally designed for Ethernet networks and operating systems, to coordinate access to these intersections. Using a decentralized Markov decision process framework, the proposed approach enables aircraft to autonomously adjust their speed and timing as they navigate these critical areas, maintaining safe separation without a central controller. We evaluate the effectiveness of this approach in simulated UAM scenarios, demonstrating its ability to reduce separation violations to zero while acknowledging trade-offs in flight times as traffic density increases. Additionally, we explore the impact of non-compliant aircraft, showing that while shared scheduling protocols can no longer guarantee safe separation, they still provide significant improvements over systems without scheduling protocols.

Separation Assurance↗

NASA NTRSDate not supplied

Separation Assurance in Urban Air Mobility Systems Using Shared Scheduling Protocols

system safety↗

DOE OSTI2022

Techno-Economic Analysis and Life-Cycle Assessment of Emerging Technologies for Bioprocessing Separations

Limited availability, rising costs, and environmental concerns about fossil fuels have generated considerable interest in finding alternative, renewable sources including biomass, which can be converted into a number of biofuels and bioproducts. In comparison to petroleum-based products, high processing costs, mainly associated with bioprocessing separations, limit widespread implementation of biofuels and bioproducts. Bioprocess-related separations are also complicated, regardless of the conversion pathway, due to the dilute nature of products and the chemically complex mixtures that result from biomass deconstruction. In many cases, bioprocessing separation approaches lack a technology baseline, or definition of the state of technology (SOT). This work focuses on evaluating the technology readiness of novel separations technologies for the conversion of biomass into biofuels and bioproducts and will address three key topics: 1) SOT description, 2) economic viability analysis of both SOT and innovative separations, and 3) environmental impact assessment of both SOT and novel processes. The current SOT for lignin valorization, dilute carbon recovery, and impurity removal is used to identify potential opportunities for improvement and provide a baseline for comparison with the emerging technologies. Detailed techno-economic analysis (TEA) and life cycle assessment (LCA) are applied to understand the key drivers and challenges related to the economic feasibility and environmental impacts, respectively.

BASIC BIOLOGICAL SCIENCES,BIOMASS FUELS↗

DOE OSTI2019

Low‐Cost Self‐Assembled Oxide Separator for Rechargeable Batteries

Abstract Rechargeable battery cells having a liquid electrolyte require a separator permeable to the electrolyte between the two electrodes. Because the electrodes change their volume during charge and discharge, the porous separators are flexible polymers with an electronic energy gap E g large enough for the Fermi levels of the two electrodes to be within it. In this work, a porous film of self‐assembled SiO 2 nanoparticles is developed as the separator for a Li‐ion battery with a liquid electrolyte. This coating does not require the plasticity of a polymer membrane and has the required large E g . If adsorbed water is removed from the SiO 2 surface, the nanoparticles bond to one another and to an oxide cathode to form a plastic self‐assembling porous layer into which the liquid electrolyte can penetrate. The Li‐ion batteries with a LiCoO 2 cathode coated with SiO 2 as a separator show similar performance to cells with a traditional polypropylene separator and improved cyclability with a reduced volume of liquid electrolyte owing to the electrolyte wetting properties of the SiO 2 nanoparticles. The SiO 2 nanoparticles are easy to prepare, cheap, and environmentally friendly.

Grundish, Nicholas S.↗