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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Platinum and CeO 2-x Occlusion Electrodeposition at Unsupported Vulcan XC-72R for Methanol and Ethanol Oxidation Reactions in Alkaline Media

Abstract Platinum was electrodeposited in a slurry solution of CeO2 and Vulcan XC-72R to produce Pt/CeO2-x/Vulcan XC-72R catalysts by using the Rotating Disk Slurry Electrodeposition (RoDSE) Technique. The activity of the catalysts was measured towards methanol and ethanol oxidation reactions in alkaline conditions by cyclic voltammetry and chronoamperometry. The electrochemical results were compared to those obtained on commercial catalysts. Pt/CeO2-x/Vulcan XC-72R (with ~ 26 wt.% Pt) catalyst was the most active for both alcohol oxidation reactions when compared to commercial 40 wt.% and 20% /Vulcan XC-72R (ETEK) catalysts. The mass activity increases 2.0x and 2.4x for methanol and ethanol oxidation reactions when compare with 40 and 20 Pt wt. % commercial catalysts, respectively. The Pt/CeO2-x/Vulcan XC-72R catalysts contained Pt nanoparticles growth within the cerium oxide through an occlusion electrodeposition method. These effects were systematically investigated using X-ray Diffraction (XRD), High Resolution Transmission Electron Microscopy (HR-TEM), and X-ray Photoelectron Spectroscopy (XPS).

Suleiman Mahmoud, Amal↗
DOE OSTI2024

Hydrothermal conditioning of oleaginous yeast cells to enable recovery of lipids as potential drop-in fuel precursors

Abstract Background Lipids produced using oleaginous yeast cells are an emerging feedstock to manufacture commercially valuable oleochemicals ranging from pharmaceuticals to lipid-derived biofuels. Production of biofuels using oleaginous yeast is a multistep procedure that requires yeast cultivation and harvesting, lipid recovery, and conversion of the lipids to biofuels. The quantitative recovery of the total intracellular lipid from the yeast cells is a critical step during the development of a bioprocess. Their rigid cell walls often make them resistant to lysis. The existing methods include mechanical, chemical, biological and thermochemical lysis of yeast cell walls followed by solvent extraction. In this study, an aqueous thermal pretreatment was explored as a method for lysing the cell wall of the oleaginous yeast Rhodotorula toruloides for lipid recovery. Results Hydrothermal pretreatment for 60 min at 121 °C with a dry cell weight of 7% (w/v) in the yeast slurry led to a recovery of 84.6 ± 3.2% (w/w) of the total lipids when extracted with organic solvents. The conventional sonication and acid-assisted thermal cell lysis led to a lipid recovery yield of 99.8 ± 0.03% (w/w) and 109.5 ± 1.9% (w/w), respectively. The fatty acid profiles of the hydrothermally pretreated cells and freeze-dried control were similar, suggesting that the thermal lysis of the cells did not degrade the lipids. Conclusion This work demonstrates that hydrothermal pretreatment of yeast cell slurry at 121 °C for 60 min is a robust and sustainable method for cell conditioning to extract intracellular microbial lipids for biofuel production and provides a baseline for further scale-up and process integration. Graphical abstract

09 BIOMASS FUELS↗
DOE OSTI2026

Data for Optimization of Pre-Commercial Enzymes Dosage for a Potential Lignocellulosic Biorefinery

Lignocellulolytic enzymes remain one of the primary cost constraints in second-generation (2G) ethanol biorefineries. Achieving efficient hydrolysis of structural carbohydrates with minimal enzyme dosage, maintaining slurry fermentability for industrially relevant ethanol titers, and maximizing ethanol yield per ton of biomass are among the major challenges in 2G processes. In this study, we optimized the dosages of pre-commercial cellulase (NS22257) and hemicellulase (NS22244) on pilot-scale, hydrothermally pretreated lignocellulosic substrates. Enzyme dosages were evaluated at three levels: 20 mg of cellulase with 7.25 mg of hemicellulase (ED-1), 40 mg with 14.5 mg (ED-2), and 60 mg with 21.75 mg (ED-3). As expected, the highest sugar yields were obtained with ED-3; however, for sweet sorghum, oilcane, and miscanthus, sugar yields from ED-2 and ED-3 were not significantly different (p < 0.05). For example, sweet sorghum produced 123.78 ± 1.54 g L−1 and 125.76 ± 0.46 g L−1 of total sugars (glucose and xylose) with ED-2 and ED-3, respectively. Although energycane exhibited a statistically significant difference between ED-2 and ED-3, the incremental gain with ED-3 was modest, increasing sugar release by only 9.02 g L−1 relative to ED-2. Importantly, ED-1 resulted in sugar yields of 88.88 ± 3.64 to 106.86 ± 1.21 g L−1, sufficient to achieve ethanol titers ≥40 g L−1, the threshold required for industrial relevance. A semi-integrated bioprocess validated this outcome, producing 42.09 ± 2.38 g L−1 ethanol and an estimated yield of 213.38 L of ethanol per dry ton of pretreated biomass, requiring only 20.83 L of cellulase and 6.25 L of hemicellulase per ton. Remarkably, these enzyme dosages were approximately tenfold lower than those reported in prior studies.

Energycane↗
DOE OSTI2024

Data for Hydrothermal Conditioning of Oleaginous Yeast Cells to Enable Recovery of Lipids as Potential Drop-in Fuel Precursors

Lipids produced using oleaginous yeast cells are an emerging feedstock to manufacture commercially valuable oleochemicals ranging from pharmaceuticals to lipid-derived biofuels. Production of biofuels using oleaginous yeast is a multistep procedure that requires yeast cultivation and harvesting, lipid recovery, and conversion of the lipids to biofuels. The quantitative recovery of the total intracellular lipid from the yeast cells is a critical step during the development of a bioprocess. Their rigid cell walls often make them resistant to lysis. The existing methods include mechanical, chemical, biological and thermochemical lysis of yeast cell walls followed by solvent extraction. In this study, an aqueous thermal pretreatment was explored as a method for lysing the cell wall of the oleaginous yeast Rhodotorula toruloides for lipid recovery. Hydrothermal pretreatment for 60 min at 121 °C with a dry cell weight of 7% (w/v) in the yeast slurry led to a recovery of 84.6 ± 3.2% (w/w) of the total lipids when extracted with organic solvents. The conventional sonication and acid-assisted thermal cell lysis led to a lipid recovery yield of 99.8 ± 0.03% (w/w) and 109.5 ± 1.9% (w/w), respectively. The fatty acid profiles of the hydrothermally pretreated cells and freeze-dried control were similar, suggesting that the thermal lysis of the cells did not degrade the lipids. This work demonstrates that hydrothermal pretreatment of yeast cell slurry at 121 °C for 60 min is a robust and sustainable method for cell conditioning to extract intracellular microbial lipids for biofuel production and provides a baseline for further scale-up and process integration.

Conversion↗
DOE OSTI2024

Sludge Batch 11 Assembly: Tank 26 (Rev.1)

Savannah River Mission Completion Nuclear Safety and Engineering Integration (SRMC-E) has requested that Savannah River National Laboratory (SRNL) perform Tank 26 characterization analyses in support of Sludge Batch 11 (SB11) assembly. This report provides important characterization of the slurry in Tank 26 prior to transfer from Tank 26 to Tank 51 that confirms the transfer is "Low Rem" and ensures the sludge concurs with the estimated transfer mass for the SB11 recipe. Two Tank 26 samples were delivered to SRNL and composited into a single sample in September 2023. The composite sample was analyzed for the following: density, weight percent solids, chemical composition, radionuclides, supernate corrosion control tests, and x-ray diffraction for burkeite, gibbsite, and boehmite. The slurry was also evaluated for sulfate washing behavior in order to provide knowledge on insoluble sulfate dissolution during Tank 51 sludge washing similar to a previous washing study performed in 2019. The Tank 26 sample results are consistent with and representative of PUREX sludge and the prior usage of Tank 26 as a feed tank for the 1F and 2F Evaporators.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Characterization of Precipitate Reactor Feed Tank (PRFT) Batches 15, 22, and 26 from the Defense Waste Processing Facility (DWPF)

The Savannah River Site (SRS) Defense Waste Processing Facility (DWPF) processes a Monosodium Titanate/Sludge Solids (MST/SS) waste stream received from the Salt Waste Processing Facility (SWPF) via the Precipitate Reactor Feed Tank (PRFT). During processing, DWPF is required to provide evidence of compliance with the Waste Acceptance Product Specifications (WAPS) to ensure acceptance of their vitrified high-level waste (HLW) into the Civilian Radioactive Waste Management System. Production Records must document the constituents of the MST/SS material in the PRFT from each salt batch (StB) processed at SWPF. Savannah River Mission Completion (SRMC) has requested Savannah River National Laboratory (SRNL) to analyze PRFT samples representing each SWPF salt batch for thirty-two radionuclides. Additionally, elemental analysis of PRFT slurry and MST/SS solids was performed to aid SRMC in further refinement of the inputs and assumptions used in future frit development and Material Tracking Program calculations. The analyses of PRFT Batches 15, 22, and 26, which corresponds to material from the processing of StB4, StB5, and StB7, respectively, are reported herein. The unwashed dried solids of the PRFT batches were found to be 86-87% MST. Additionally, the total sulfur values are well below the assumed 982 mg of sulfate/kg of PRFT slurry used in Material Tracking Program calculations.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Wabash Hydrogen Negative Emissions Technology Demonstration

The objectives of the Wabash Hydrogen Negative Emissions Technology Demonstration Project (Wabash Project) are to develop and design all aspects of the scope, cost, characteristics and investment case of a world class flexible gasification, net negative carbon, hydrogen co-products power plant. The outcome of this undertaking is a complete set of deliverables that has been produced by a preeminent team of engineers, constructors, operators, and developers, building upon previous technology, utilizing cutting edge technology, and thoroughly defining all aspects of this fully integrated 21st Century Powerplant. The Wabash Project encapsulates several cross-cutting initiatives within the US Department of Energy, such as 100% hydrogen powered combustion turbine, geological carbon sequestration, coal with biomass gasification and hydrogen energy storage. The flexible gasifier at the Wabash Valley Resources plant is a slurry-fed, entrained flow, high-temperature, oxygen-blown gasifier that has been proven commercially to operate successfully on various coals and petroleum coke (petcoke). The ability to be fuel flexible and feed various biomass (woody biomass and agriculture residue) and petroleum waste (plastics) was evaluated during BP 1 (BP1). This involved the preparation and testing of feedstocks into slurries to determine what fuels can be fed to the gasifier. By utilizing a flexible oxygen-blown gasifier, the ability to address operational issues common to lower temperature biomass gasification, such as the handling of tars, can be mitigated. The overall goal is to achieve a design capable of carbon-negative emissions while leveraging the substantial investments made and operating experience already gained at the Wabash site.

01 COAL, LIGNITE, AND PEAT↗
DOE OSTI2025

Plutonium Solubility and Supernate Concentration for Neutralized Fast Critical Assembly Discards to Savannah River Site Tank Waste

The Savannah River Site (SRS) plans to dissolve non-irradiated stainless steel (SS)-clad bundles of Fast Critical Assembly (FCA) materials in eighteen batches.1 FCA dissolution is currently underway in the 6.3D dissolver by simultaneous chemical and electrolytic dissolution, which is required to generate the harsh conditions necessary for dissolution of metal-oxide (MOX) and non-aluminum spent nuclear fuels (NASNFs).2 Nitric acid and potassium fluoride are used to promote chemical dissolution.2 Gadolinium will be added during processing as a thermal neutron poison for criticality control. There are no plans for recovering plutonium from this waste stream. After FCA dissolution, the acidic (HNO3/KF) “discards” containing the dissolved metals will be neutralized by addition of 50 wt% sodium hydroxide to a final free hydroxide concentration of 1.2 M.1 Neutralization will precipitate a slurry of insoluble solids, predominantly metal oxides/hydroxides of plutonium, uranium, and SS components. Small fractions of the SS components, Pu, U, and Gd will remain dissolved in the supernate. The neutralized slurry will be composited to existing radioactive waste storage tanks within the SRS Concentration, Storage, and Transfer Facilities (CSTF) containing other similar sludge batch (SB) materials.1 The fate of soluble plutonium and freshly-precipitated, colloidal plutonium from this process are of concern since the total Pu can challenge the waste acceptance criteria (WAC) at the downstream SRS Liquid Waste (LW) facility. Supernate decants including the neutralized FCA discards (nFCAd) within the CSTF will be composited with salt batch (StB) materials and transferred to the SRS Salt Waste Processing Facility (SWPF), where total plutonium is also of concern.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2026

Characterization of Precipitate Reactor Feed Tank (PRFT) Batches 44 and 49 from the Defense Waste Processing Facility (DWPF)

The Savannah River Site (SRS) Defense Waste Processing Facility (DWPF) processes a Monosodium Titanate/Sludge Solids (MST/SS) waste stream received from the Salt Waste Processing Facility (SWPF) via the Precipitate Reactor Feed Tank (PRFT). During processing, DWPF is required to provide evidence of compliance with the Waste Acceptance Product Specifications (WAPS). Savannah River Mission Completion (SRMC) has requested Savannah River National Laboratory (SRNL) to analyze PRFT samples representing each SWPF salt batch for thirty-two radionuclides. Additionally, elemental analysis of PRFT slurry and MST/SS solids was performed to aid SRMC in further refinement of the inputs and assumptions used in future frit development and Material Tracking Program calculations. The analyses of PRFT Batches 44 and 49, which correspond to material from the processing of Salt Batches (StB) 12 and 11, respectively, are reported herein. The unwashed dried solids of the PRFT Batches 44 and 49 are predominately MST, ~63-59% MST. The two batches have a much higher amount of Fe, Mn, and Ni compared to all previous batches. For Batch 44 this appears to be due to the use of a sludge simulant filter aid during processing of StB 12 and for Batch 49, it is possibly due to the larger amount of insoluble solids for StB 11 in comparison to all previous salt batches. Like previous PRFT batches, a significant amount of the unwashed dried solids are alkaline earth metals. The total sulfate, in mg/kg of slurry, for PRFT Batches 44 and 49 is 119 and 139, respectively, which is well below the current sulfate concentration used in Material Tracking Program calculations and is in agreement with DWPF laboratory sulfate measurements.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS1967

Development of Coatings for Tantalum Alloy Nozzle Vanes

A group of silicide coatings developed for the T222 tantalum-base alloy have afforded over 600 hours of protection at 1600 and 2400 F during cyclic exposure in air. These coatings were applied in two steps. A modifier alloy was applied by slurry techniques and was sintered in vacuum prior to siliciding by pack cementation in argon. Application of the modifier alloy by pack cementation was found to be much less effective. The addition of titanium and vanadium to molybdenum and tungsten yielded beneficial modifier alloys, whereas the addition of chromium showed no improvement. After siliciding, the 15Ti- 35W-15V-35Mo modifier alloy exhibited the best performance; one sample survived 1064 hours of oxidation at 2400 F. This same coating was the only coating to reproducibly provide 600 hours of protection at both 1600 and 2400 F; in the second and third of three experiments, involving oxidation of three to five specimens at each temperature in each experiment, no failures were observed in 600 hours of testing. The slurry coatings were also shown to protect the Cb752 and D43 columbium-base alloys.

PROTECTIVE COATING↗
NASA NTRS1972

Design and development of a prototype wet oxidation system for the reclamation of water and the disposition of waste residues onboard space vehicles

Laboratory investigations to define optimum process conditions for oxidation of fecal/urine slurries were conducted in a one-liter batch reactor. The results of these tests formed the basis for the design, fabrication, and testing of an initial prototype system, including a 100-hour design verification test. Areas of further development were identified during this test. Development of a high pressure slurry pump, materials corrosion studies, oxygen supply trade studies, comparison of salt removal water recovery devices, ammonia removal investigation, development of a solids grinder, reactor design studies and bearing life tests, and development of shutoff valves and a back pressure regulator were undertaken. The development work has progressed to the point where a prototype system suitable for manned chamber testing can be fabricated and tested with a high degree of confidence of success.

Jagow, R. B.↗
NASA NTRS1973

Preparation of prepreg graphite tape with insoluble polymer

Powdered polymer is finely ground. Second polymer, soluble, is mixed with appropriate solvent. Milled polymer and graphite filaments are added to soluble polymer-solvent solution to create slurry. Slurry is dried, and when ready for processing, the soluble, binder-polymer is removed by heat during precure or cure cycle.

Yates, C. I.↗
NASA NTRS1972

Wear and related characteristics of an aircraft tire during braking

Wear and related characteristics of friction and temperature developed during braking of size 22 x 5.5, type aircraft tires are studied. The testing technique involved gearing the tire to a driving wheel of a ground vehicle to provide operations at constant slip ratios on asphalt, concrete, and slurry-seal surfaces. Data were obtained over the range of slip ratios generally attributed to an aircraft braking system during dry runway operations. The results show that the cumulative tire wear varies linearly with distance traveled and the wear rate increases with increasing slip ratio and is influenced by the runway-surface character. Differences in the wear rates associated with the various surfaces suggest that runways can be rated on the basis of tire wear. The results also show that the friction coefficients developed during fixed-slip-ratio operations are in good agreement with those obtained by other investigators during cyclic braking, in that the dry friction is insensitive to the tire tread temperature is shown to increase with increasing slip ratio and, at the higher ratios, to be greater during braking on asphalt and slurry seal than on concrete.

Mccarty, J. L.↗
NASA NTRS1973

Outer skin protection of columbium Thermal Protection System (TPS) panels

A coated columbium alloy material system 0.04 centimeter thick was developed which provides for increased reliability to the load bearing character of the system in the event of physical damage to and loss of the exterior protective coating. The increased reliability to the load bearing columbium alloy (FS-85) was achieved by interposing an oxidation resistant columbium alloy (B-1) between the FS-85 alloy and a fused slurry silicide coating. The B-1 alloy was applied as a cladding to the FS-85 and the composite was fused slurry silicide coated. Results of material evaluation testing included cyclic oxidation testing of specimens with intentional coating defects, tensile testing of several material combinations exposed to reentry profile conditions, and emittance testing after cycling of up to 100 simulated reentries. The clad material, which was shown to provide greater reliability than unclad materials, holds significant promise for use in the thermal protection system of hypersonic reentry vehicles.

Culp, J. D.↗
NASA NTRS1974

Fused silicon-rich coatings for superalloys

Various compositions of nickel-silicon and aluminum-silicon slurries were sprayed on IN 100 specimens and fusion-sintered to form fully dense coatings. Cyclic furnace oxidation tests in 1 atm air at 1100 C showed all the coatings to be protective for at least 600 hours, and one slurry, Al-60Si, was protective for 1000 hours. This coating also protected NASA TAZ 8A and NASA-TRW VIA for 1000 hours in the same furnace test. Alloys B 1900, TD-NiCr, and Mar-M200 were protected for lesser times, while NX 188 and NASA WAZ 20 were scarcely protected at all. Limited stress-rupture testing on 0.64-cm-diam IN 100 specimens detected no degradation of mechanical properties due to silicon diffusion.

Smialek, J. L.↗
NASA NTRS1975

Low gravity synthesis of polymers with controlled molecular configuration

Heterogeneous chemical systems have been studied for the synthesis of isotactic polypropylene in order to establish baseline parameters for the reaction process and to develop sensitive and accurate methods of analysis. These parameters and analytical methods may be used to make a comparison between the polypropylene obtained at one g with that of zero g (gravity). Baseline reaction parameters have been established for the slurry (liquid monomer in heptane/solid catalyst) polymerization of propylene to yield high purity, 98% isotactic polypropylene. Kinetic data for the slurry reaction showed that a sufficient quantity of polymer for complete characterization can be produced in a reaction time of 5 min; this time is compatible with that available on a sounding rocket for a zero-g simulation experiment. The preformed (activated) catalyst was found to be more reproducible in its activity than the in situ formed catalyst.

Heimbuch, A. H.↗
NASA NTRS1975

Fusible heat sink for EVA thermal control

The preliminary design and analysis of a heat sink system utilizing a phase change slurry material to be used eventually for astronaut cooling during manned space missions is described. During normal use, excess heat in the liquid cooling garment coolant is transferred to a reusable/regenerable fusible heat sink. Recharge is accomplished by disconnecting the heat sink from the liquid cooling garment and placing it in an on board freezer for simultaneous slurry refreeze and power supply electrical rechange.

Roebelen, G. J., Jr.↗