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At least 1,675 records · Page 93

A single column separation method for barium isotope analysis of geologic and hydrologic materials with complex matrices

Abstract The increasing significance of barium (Ba) in environmental and geologic research in recent years has led to interest in the application of the Ba isotopic composition as a tracer for natural materials with complex matrices. Most Ba isotope measurement techniques require separation of Ba from the rest of sample prior to analysis. This paper presents a method using readily available materials and disposable columns that effectively separates Ba from a range of geologic and hydrologic materials, including carbonate minerals, silicate rocks, barite, river water, and fluids with high total dissolved solids and organic content such as oil and gas brines, rapidly and without need for an additional cleanup column. The technique involves off-the-shelf columns and cation exchange resin and a two-reagent elution that uses 2.5 N HCl followed by addition of 2.0 N HNO 3 . We present data to show that major matrix elements from almost any natural material are separated from Ba in a single column pass, and that the method also effectively reduces or eliminates isobaric interferences from lanthanum and cerium.

Matecha, R. M.↗

Enhanced capacity and stability for the separation of cesium in electrically switched ion exchange

Electrically switched ion exchange (ESIX) can be used to separate ionic contaminants from industrial wastewater, including that generated by the nuclear industry. The ESIX method involves sequential application of reduction and oxidation potentials to an ion exchange film to induce the respective loading and unloading of cesium. This technology is superior to conventional methods (e.g electrodialysis reversal or reverse osmosis) as it requires very little energy for ionic separation. In previous studies, ESIX films have demonstrated relatively low ion exchange capacities and limited film stabilities over repeated potential applications. In this study, the methodology for the deposition of electro-active films (nickel hexacyanoferrate) on nickel electrodes was modified to improve the ion exchange capacity for cesium removal using ESIX. Cyclic voltammetry was used to investigate the ion exchange capacity and stability. Scanning electron microscopy (SEM) was used to characterize the modified film surfaces. Additionally, the films were examined for the separation of cesium ions. This modified film preparation technique enhanced the ion exchange capacity and improves the film stability compared to previous methods for the deposition of ESIX films. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Utilization of traceable standards to validate plutonium isotopic purification and separation of plutonium progeny using AG MP-1M resin for nuclear forensic investigations

Radio-chronometric studies on plutonium (Pu) materials require independent measurement of the Pu (parent) content and isotopic distribution as well as concentration and isotopic distribution of the plutonium isotopic decay products. We performed a series of experiments to demonstrate the consistency of separations using the Lewatit MP 800 macroporous anion exchange resin and the AG MP-1M resin with traceable Pu isotopic certified reference material (CRM) standards 136, 137, 138, and 126-A. Two different mesh-sizes of the AG MP-1M resin were tested and the 50–100 mesh size resin was found to work more efficiently for the separation task. Both Lewatit and AG MP-1M resins were found to perform satisfactorily for quantitatively extracting the americium (Am) and uranium (U) progeny as well as gallium (Ga) present as a tracer in the Pu material. Both resins were effective in removing isobaric interferences from the Pu fraction used in isotopic measurements by thermal ionization mass spectrometry (TIMS). To address the co-elution of uranium and gallium, Alizarin red S (ARS) was used as a colorimetric dye to determine the behavior of UO 2 2+ and Ga 3+ on AG MP-1M resin with various acidic solutions as eluents using UV–vis spectra. Poor resolution of these peaks complicated quantitative analysis by UV–vis spectroscopy, but these results were informative in planning automated separation experiments by HPLC. LA-UR-24-28919.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Discovery of Innovative Polymers for Next-Generation Gas-Separation Membranes using Interpretable Machine Learning

Polymer membranes perform innumerable separations with far-reaching environmental implications. Despite decades of research on membrane technologies, design of new membrane materials remains a largely Edisonian process. To address this shortcoming, we demonstrate a generalizable, accurate machine-learning (ML) implementation for the discovery of innovative polymers with ideal separation performance. Specifically, multitask ML models are trained on available experimental data to link polymer chemistry to gas permeabilities of He, H2, O2, N2, CO2, and CH4. Here, we interpret the ML models and extract chemical heuristics for membrane design, through Shapley Additive exPlanations (SHAP) analysis. We then screen over nine million hypothetical polymers through our models and identify thousands of candidates that lie well above current performance upper bounds. Notably, we discover hundreds of never-before-seen ultrapermeable polymer membranes with O2 and CO2 permeability greater than 104 and 105 Barrer, respectively. These hypothetical polymers are capable of overcoming undesirable trade-off relationship between permeability and selectivity, thus significantly expanding the currently limited library of polymer membranes for highly efficient gas separations. High-fidelity molecular dynamics simulations confirm the ML-predicted gas permeabilities of the promising candidates, which suggests that many can be translated to reality.

Yang, Jason↗

Hydrogen separation membranes annual report for FY 2010.

The objective of this work is to develop dense ceramic membranes for separating hydrogen from other gaseous components in a nongalvanic mode, i.e., without using an external power supply or electrical circuitry. The goal of this project is to develop dense hydrogen transport membranes (HTMs) that nongalvanically (i.e., without electrodes or external power supply) separate hydrogen from gas mixtures at commercially significant fluxes under industrially relevant operating conditions. These membranes will be used to separate hydrogen from gas mixtures such as the product streams from coal gasification, methane partial oxidation, and water-gas shift reactions. Potential ancillary uses of HTMs include dehydrogenation and olefin production, as well as hydrogen recovery in petroleum refineries and ammonia synthesis plants, the largest current users of deliberately produced hydrogen. This report describes the results from the development and testing of HTM materials during FY 2010.

01 COAL, LIGNITE, AND PEAT↗

Dynamic Absorption Model for Off-Gas Separation

Modeling and simulations will aid in the future design of U.S. advanced reprocessing plants for the recovery and recycle of actinides in used nuclear fuel. The specific fuel cycle separation process discussed in this report is the off-gas treatment system. The off-gas separation consists of a series of scrubbers and adsorption beds to capture constituents of interest. Dynamic models are being developed to simulate each unit operation involved so each unit operation can be used as a stand-alone model and in series with multiple others. Currently, a rate based, dynamic absorption model is being developed in gPROMS software. Inputs include liquid and gas stream constituents, column properties, liquid and gas phase reactions, number of stages, and inlet conditions. It simulates multiple component absorption with countercurrent flow and accounts for absorption by mass transfer and chemical reaction. The assumption of each stage being a discrete well-mixed entity was made. Therefore, the model is solved stagewise. The simulation outputs component concentrations in both phases as a function of time from which the rate of absorption is determined. Temperature of both phases is output as a function of time also. The model will be used able to be used as a standalone model in addition to in series with other off-gas separation unit operations. The current model is being generated based on NOx absorption; however, a future goal is to develop a CO2 specific model. The model will have the capability to be modified for additional absorption systems. The off-gas models, both adsorption and absorption, will be made available via the server or web for evaluation by customers.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Metal-organic and zeolite imidazolate frameworks (MOFs and ZIFs) for highly selective separations

Metal-organic and zeolite imidazolate frameworks (MOFs and ZIFs) have been investigated for the realization as separation media with high selectivity. These structures are held together with strong bonds, making them architecturally, chemically, and thermally stable. Therefore, employing well designed building units, it is possible to discover promising materials for gas and vapor separation. This grant was focused on the study of MOFs and ZIFs with these specific objectives: (i) to develop a strategy for producing MOFs and ZIFs that combine high surface areas with active sites for their use in gas adsorption and separation of small organic compounds, (ii) to introduce active sites in the framework by a post-synthetic modification and metalation of MOFs and ZIFs, and (iii) to design and synthesize MOFs with extremely high surface areas and large pore volumes to accommodate large amounts of guest molecules. By the systematic study, this effort demonstrated how to introduce active functional groups in the frameworks, and this is also the origin of a new strategy, which is termed isoreticular functionalization and metalation. However, a large pore volume is still a prerequisite feature. One of the solutions to overcome this challenge is an isoreticular expansion of a MOF's structure. With triangular organic linker and square building units, we demonstrated that MOF-399 has a unit cell volume 17 times larger than that of the first reported material isoreticular to it, and it has the highest porosity (94%) and lowest density (0.126 g cm -3 ) of any MOF reported to date. MOFs are not just low density materials; the guest-free form of MOF-210 demonstrates an ultrahigh porosity, whose BET surface area was estimated to be 6240 m 2 g -1 by N 2 adsorption measurements.

36 MATERIALS SCIENCE↗

Experiments with the LECO Pegasus® Gas Chromatograph/ Time-of-Flight Mass Spectrometer Phase 2: 2D Fast GC Separations

Conventional analysis by gas chromatography/ quadrupole mass spectrometry (GC/MS) can be time-consuming (30 – 60 minutes) and prone to interferences. The use of fast gas chromatography coupled with time-of-flight mass spectrometry (GC/TOF-MS) offers the advantages of faster (~10 min) analysis times, improved GC resolution afforded by the use of narrower (0.1– 0.18 mm id) columns, and improved mass resolution and scan speed provided by the TOF-MS. In addition, GC/TOF-MS offers the promise of better instrument detection limits than quadrupole GC/MS, while still providing full mass spectral data. If the GC/TOF-MS can be operated to perform two-dimensional (2D) separations, the ability to resolve peaks of interest from interfering compounds is improved. In 2D chromatography, a second GC column with a different chemical phase than that of the first GC column is used to provide additional separation of analytes as they elute from the first column. Because the chemistry of the second GC column is different from the first, compounds that co-elute from the first column may be easily resolved after a separation on the second GC column (i.e., the peak capacity of the system is increased and the specificity of analyte detection is improved).

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Advanced Palladium Membrane Scale-up for Hydrogen Separation

The main objective of this project was to construct, test, and demonstrate a Pd-Cu metallic tubular membrane micro-channel separator capable of producing 2 lb day -1 H 2 at 95% recovery when operating downstream of an actual coal gasifier. A key milestone for the project was to complete a pilot-scale gasifier test by 1 September 2011 and demonstrate the separation of 2 lb day -1 H 2 to verify progress toward the DOE's goals prior to down-selection for larger-scale (100 lb day -1 ) hydrogen separator development.

08 HYDROGEN↗

Novel, Ceramic Membrane System For Hydrogen Separation

Separation of hydrogen from coal gas represents one of the most promising ways to produce alternative sources of fuel. Ceramatec, teamed with CoorsTek and Sandia National Laboratories has developed materials technology for a pressure driven, high temperature proton-electron mixed conducting membrane system to remove hydrogen from the syngas. This system separates high purity hydrogen and isolates high pressure CO 2 as the retentate, which is amenable to low cost capture and transport to storage sites. The team demonstrated a highly efficient, pressure-driven hydrogen separation membrane to generate high purity hydrogen from syngas using a novel ceramic-ceramic composite membrane. Recognizing the benefits and limitations of present membrane systems, the all-ceramic system has been developed to address the key technical challenges related to materials performance under actual operating conditions, while retaining the advantages of thermal and process compatibility offered by the ceramic membranes. The feasibility of the concept has already been demonstrated at Ceramatec. This project developed advanced materials composition for potential integration with water gas shift rectors to maximize the hydrogen production.

08 HYDROGEN↗

2012-13 Blue Room Low Enriched Uranium Sample Irradiation, Associated Gas Handling System, and Subsequent Separation Chemistry

An irradiation experiment was designed for the production of 100 mCi of medical isotope Mo-99 from a Low Enriched Uranium (LEU) solution. 300 mL of 150 gU/L LEU sulfate solution (pH1) was prepared and irradiated at the LANSCE Blue Room facility. The apparatus designed for the irradiation included a gas handling system, in which safe operation could be controlled by monitoring change in gas pressure. The gas handling system also contained a hydrogen oxygen recombiner, to recombine the gases generated through radiolysis of water, and an iodine trap, primarily for I-131. Pressure transients were observed during irradiation, which could be controlled by increasing the flow rate of the circulating pump. After irradiation the LEU solution was transferred to a hot cell facility for subsequent Mo-99 recovery using a titania column separation process, with samples also subsequently shipped to a radiochemical laboratory for further analysis. Gamma spectroscopy analysis revealed that ca. 70 mCi of Mo-99 was present at end of beam, in good agreement with the predicted value when actual beam history was included into the calculation. There was 80-85 % recovery of Mo-99 through a titania column separation, excluding losses through radioactive decay. The % Mo-99 recovery was lower than observed previously for the 1 mCi Mo-99 production (Target 4) experiments undertaken at LANL using the same separation apparatus, with on this occasion evidence of lower oxidation state molybdenum remaining irreversibly bound to the titania column. Subsequent postmortem analysis of the Blue room apparatus revealed that there had been no leaks in the gas handling system, the hydrogen and oxygen recombination appeared to work efficiently, and recovery of irradiated uranium trapped in the system allowed for >99% uranium mass balance.

07 ISOTOPE AND RADIATION SOURCES↗

Center for Advanced Separation Technology

The U.S. is the largest producer of mining products in the world. In 2011, U.S. mining operations contributed a total of $\$$232 billion to the nation’s GDP plus $\$$138 billion in labor income. Of this the coal mining industry contributed a total of $\$$97.5 billion to GDP plus $\$$53 billion in labor income. Despite these contributions, the industry has not been well supported with research and development funds as compared to mining industries in other countries. To overcome this problem, the Center for Advanced Separation Technologies (CAST) was established to develop technologies that can be used by the U.S. mining industry to create new products, reduce production costs, and meet environmental regulations. Originally set up by Virginia Tech and West Virginia University, CAST is now a five-university consortium – Virginia Tech, West Virginia University, University of Kentucky, University of Utah and Montana Tech, - that is supported through U.S. DOE Cooperative Agreement No. DE-FE0000699, Center for Advanced Separation Technology. Much of the research to be conducted with Cooperative Agreement funds will be longer term, high-risk, basic research and will be carried out in two broad areas: Advanced Pre-Combustion Clean Coal Technologies and Gas-Gas Separations. Distribution of funds is handled via competitive solicitation of research proposals through Site Coordinators at the five member universities. These were reviewed and the selected proposals were forwarded these to the DOE/NETL Project Officer for final review and approval.

01 COAL, LIGNITE, AND PEAT↗

Bio-Oil Separation and Stabilization by Supercritical Fluid Fractionation. 2014 Final Report

The objective of this project is to use supercritical fluids to separate and fractionate algal-based bio-oils into stable products that can be subsequently upgraded to produce drop-in renewable fuels. To accomplish this objective, algae was grown and thermochemically converted to bio-oils using hydrothermal liquefaction (HTL), pyrolysis, and catalytic pyrolysis. The bio-oils were separated into an extract and a raffinate using near-critical propane or carbon dioxide. The fractions were then subjected to thermal aging studies to determine if the extraction process had stabilized the products. It was found that the propane extract fraction was twice as stable as the parent catalytic pyrolysis bio-oils as measured by the change in viscosity after two weeks of accelerated aging at 80°C. Further, in-situ NMR aging studies found that the propane extract was chemically more stable than the parent bio-oil. Thus the milestone of stabilizing the product was met. A preliminary design of the extraction plant was prepared. The design was based on a depot scale plant processing 20,000,000 gallons per year of bio-oil. It was estimated that the capital costs for such a plant would be $8,700,000 with an operating cost of $3,500,000 per year. On a per gallon of product cost and a 10% annual rate of return, capital costs would represent $0.06 per gallon and operating costs would amount to $0.20 per gallon. Further, it was found that the energy required to run the process represented 6.2% of the energy available in the bio-oil, meeting the milestone of less than 20%. Life cycle analysis and greenhouse gas (GHG) emission analysis found that the energy for running the critical fluid separation process and the GHG emissions were minor compared to all the inputs to the overall well to pump system. For the well to pump system boundary, energetics in biofuel conversion are typically dominated by energy demands in the growth, dewater, and thermochemical process. Bio-oil stabilization by near critical propane extraction had minimal impact in the overall energetics of the process with NER contributions of 0.03. Based on the LCA, the overall conversion pathways were found to be energy intensive with a NER of about 2.3 and 1.2 for catalytic pyrolysis and HTL, respectively. GHG emissions for the catalytic pyrolysis process were greater than that of petroleum diesel at 210 g CO2 eq compared to 18.9 g CO2 eq. Microalgae bio-oil based diesel with thermochemical conversion through HTL meets renewable fuel standards with favorable emission reductions of -10.8 g CO2 eq. The importance of the outcomes is that the critical fluid extraction and stabilization process improved product stability and did so with minimal energy inputs and processing costs. The LCA and GHG emission calculations point toward the HTL pathway as the more favorable thermochemical route towards upgrading algae to bio-fuels. Since the quality of the HTL oil was significantly lower than that of the catalytic pyrolysis bio-oil, the next steps point toward improving the quality of the HTL oils from algae biomass and focusing the critical fluid stabilization on that bio-oil product.

09 BIOMASS FUELS↗

Lithium Thiophosphate Compounds as Stable High Rate Li-Ion Separators

Battery separators based upon lithium thiophosphate (LiPS4) have previously been demonstrated at UC Boulder, but the thickness of the separators was too high to be of practical use in a lithium ion battery. The separators are solid phase, which makes them intrinsically less prone to thermal runaway and thereby improves safety. Results of attempting to develop sputtered thin film layers of this material by starting with targets of pure Li, Li2S, and P2S5 are reported. Sputtering rates and film quality and composition are discussed, along with efforts to use Raman spectroscopy to determine quantitative film composition. The latter is a rate limiting step in the investigation of these films, as they are typically thin and require long times to get to sufficient thickness to be analyzed using traditional methods, whereas Raman is particularly well suited to this analysis, if it can be made quantitative. The final results of the film deposition methods are reported, and a path towards new films is discussed. Finally, it should be noted that this program originally began with one graduate student working on the program, but this student ultimately chose to not continue with a PhD. A second student took over in the middle of the effort, and a new program has been proposed with a significantly altered chemistry to take the program in a new direction.

25 ENERGY STORAGE↗

Final Technical Report for the Energy Frontier Research Center Understanding Charge Separation and Transfer at Interfaces in Energy Materials (EFRC:CST)

Our EFRC was founded with the vision of creating a broadly collaborative and synergistic program that would lead to major breakthroughs in the molecular-level understanding of the critical interfacial charge separation and charge transfer (CST) processes that underpin the function of candidate materials for organic photovoltaic (OPV) and electrical-energy-storage (EES) applications. Research in these energy contexts shares an imposing challenge: How can we understand charge separation and transfer mechanisms in the presence of immense materials complexity that spans multiple length scales? To address this challenge, our 50-member Center undertook a total of 28 coordinated research projects aimed at unraveling the CST mechanisms that occur at interfaces in these nanostructured materials. This rigorous multi-year study of CST interfaces has greatly illuminated our understanding of early-timescale processes (e.g., exciton generation and dissociation dynamics at OPV heterojunctions; control of Li+-ion charging kinetics by surface chemistry) occurring in the immediate vicinity of interfaces. Program outcomes included: training of 72 graduate student and postdoctoral energy researchers at 5 institutions and spanning 7 academic disciplines in science and engineering; publication of 94 peer-reviewed journal articles; and dissemination of research outcomes via 340 conference, poster and other presentations. Major scientific outcomes included: implementation of a hierarchical strategy for understanding the electronic communication mechanisms and ultimate fate of charge carriers in bulk heterojunction OPV materials; systematic investigation of ion-coupled electron transfer processes in model Li-ion battery electrode/electrolyte systems; and the development and implementation of 14 unique technologies and instrumentation capabilities to aid in probing sub-ensemble charge separation and transfer mechanisms.

14 SOLAR ENERGY↗

Separation of Plutonium from Irradiated Fuels and Targets

Spent nuclear fuel from power production reactors contains moderate amounts of transuranium (TRU) actinides and fission products in addition to the still slightly enriched uranium. Originally, nuclear technology was developed to chemically separate and recover fissionable plutonium from irradiated nuclear fuel for military purposes. Military plutonium separations had essentially ceased by the mid-1990s. Reprocessing, however, can serve multiple purposes, and the relative importance has changed over time. In the 1960’s the vision of the introduction of plutonium-fueled fast-neutron breeder reactors drove the civilian separation of plutonium. More recently, reprocessing has been regarded as a means to facilitate the disposal of high-level nuclear waste, and thus requires development of radically different technical approaches. In the last decade or so, the principal reason for reprocessing has shifted to spent power reactor fuel being reprocessed (1) so that unused uranium and plutonium being recycled reduce the volume, gaining some 25% to 30% more energy from the original uranium in the process and thus contributing to energy security and (2) to reduce the volume and radioactivity of the waste by recovering all long-lived actinides and fission products followed by recycling them in fast reactors where they are transmuted to short-lived fission products; this reduces the volume to about 20%, reduces the long-term radioactivity level in the high-level waste, and complicates the possibility of the plutonium being diverted from civil use – thereby increasing the proliferation resistance of the fuel cycle. In general, reprocessing schemes can be divided into two large categories: aqueous/hydrometallurgical systems, and pyrochemical/pyrometallurgical systems. Worldwide processing schemes are dominated by the aqueous (hydrometallurgical) systems. This document provides a historical review of both categories of reprocessing.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Multi-Column Experimental Test Bed for Xe/Kr Separation

Previous research studies have shown that INL-developed engineered form sorbents are capable of capturing both Kr and Xe from various composite gas streams. The previous experimental test bed provided single column testing for capacity evaluations over a broad temperature range. To advance research capabilities, the employment of an additional column to study selective capture of target species to provide a defined final gas composition for waste storage was warranted. The second column addition also allows for compositional analyses of the final gas product to provide for final storage determinations. The INL krypton capture system was modified by adding an additional adsorption column in order to create a multi-column test bed. The purpose of this modification was to investigate the separation of xenon from krypton supplied as a mixed gas feed. The extra column was placed in a Stirling Ultra-low Temperature Cooler, capable of controlling temperatures between 190 and 253K. Additional piping and valves were incorporated into the system to allow for a variety of flow path configurations. The new column was filled with the AgZ-PAN sorbent which was utilized as the capture medium for xenon while allowing the krypton to pass through. The xenon-free gas stream was then routed to the cryostat filled with the HZ-PAN sorbent to capture the krypton at 191K. Selectivities of xenon over krypton were determined using the new column to verify the system performance and to establish the operating conditions required for multi-column testing. Results of these evaluations verified that the system was operating as designed and also demonstrated that AgZ-PAN exhibits excellent selectivity for xenon over krypton in air at or near room temperature. Two separation tests were performed utilizing a feed gas consisting of 1000 ppmv xenon and 150 ppmv krypton with the balance being made up of air. The AgZ-PAN temperature was held at 295 or 253K while the HZ-PAN was held at 191K for both tests. The effluent from the AgZ-PAN column was monitored via GC-TCD during the tests with no xenon being observed exiting the column during either test. Samples from each column were taken via evacuated sample bombs and were analyzed by GC-MS analysis. The results demonstrated the ability to separate xenon from krypton from a mixed gas feed utilizing the new multi-column system.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mixed Metal Phosphonate- Phosphate Resins for Separation of Lanthanides from Actinides

As indicated in the previous annual report the goals of this project are to develop procedures for efficient separation of lanthanides from actinides and curium from americium. These processes are required for the nuclear fuel cycle to minimize the waste and recover the valuable actinides. The basis for our study is that we have prepared a group of compounds that are porous and favor the uptake of ions with charges 3+ and 4+ over ions of lesser charge. The general formula for these materials is M(O 3 PC 6 H 4 PO 3 ) 1-x/2 (APO 4 )x·nH 2 O: where M=Zr 4+ , Sn 4+ , A=H, Na, or K and X=O, 0.5, 0.8, 1.0, 1.33 and 1.61-3. One of our tasks is to determine which members of this group of compounds are effective in carrying out the required separations. A difficulty in obtaining this required information is that the compounds are amorphous. That is they are not crystalline, therefore we need to resort to synchrotron data to obtain structural data which will be presented in detail. This information will be provided as a separate section.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗