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All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Paraburkholderia solitsugae sp. nov. and Paraburkholderia elongata sp. nov., phenolic acid-degrading bacteria isolated from forest soil and emended description of Paraburkholderia madseniana

Two bacterial strains, 1N T and 5N T , were isolated from hemlock forest soil using a soluble organic matter enrichment. Cells of 1N T (0.65×1.85 µm) and 5N T (0.6×1.85 µm) are Gram-stain-negative, aerobic, motile, non-sporulating and exist as single rods, diplobacilli or in chains of varying length. During growth in dilute media (≤0.1× tryptic soy broth; TSB), cells are primarily motile with flagella. At higher concentrations (≥0.3× TSB), cells of both strains increasingly form non-motile chains, and cells of 5N T elongate (0.57×~7 µm) and form especially long filaments. Optimum growth of 1N T and 5N T occurred at 25–30 °C, pH 6.5–7.0 and <0.5% salinity. Results of comparative chemotaxonomic, genomic and phylogenetic analyses revealed that 1N T and 5N T were distinct from one another and their closest related type strains: Paraburkholderia madseniana RP11 T , Paraburkholderia aspalathi LMG 27731 T and Paraburkholderia caffeinilytica CF1 T . The genomes of 1N T and 5N T had an average nucleotide identity (91.6 and 91.3%) and in silico DNA–DNA hybridization values (45.8%±2.6 and 45.5%±2.5) and differed in functional gene content from their closest related type strains. The composition of fatty acids and patterns of substrate use, including the catabolism of phenolic acids, also differentiated strains 1N T and 5N T from each other and their closest relatives. The only ubiquinone present in strains 1N T and 5N T was Q-8. The major cellular fatty acids were C 16 : 0 , 3OH-C 16 : 0 , C 17 : 0 cyclo, C 19 : 0 cyclo ω8 c and summed features 2 (3OH-C 14 : 0 / C 16 : 1 iso I), 3 (C 16 : 1 ω6 c /ω7 c ) and 8 (C 18 : 1 ω7 c /ω6 c ). A third bacterium, strain RL16-012-BIC-B, was isolated from soil associated with shallow roots and was determined to be a strain of P. madseniana (ANI, 98.8%; 16S rRNA gene similarity, 100%). Characterizations of strain RL16-012-BIC-B (DSM 110723=LMG 31706) led to proposed emendments to the species description of P. madseniana . Our polyphasic approach demonstrated that strains 1N T and 5N T represent novel species from the genus Paraburkholderia for which the names Paraburkholderia solitsugae sp. nov. (type strain 1N T =DSM 110721 T =LMG 31704 T ) and Paraburkholderia elongata sp. nov. (type strain 5N T =DSM 110722 T =LMG 31705 T ) are proposed.

Microbiology↗
NASA NTRS1998

Acquisition and Early Losses of Rare Gases from the Deep Earth

Direct observations show that the deep Earth contains rare gases of solar composition distinct from those in the atmosphere. We examine the implications of mantle rare gas characteristics on acquisition of rare gases from the solar nebula and subsequent losses due to a large impact. Deep mantle rare gas concentrations and isotopic compositions can be obtained from a model of transport and distribution of mantle rare gases. This model assumes the lower mantle closed early, while the upper mantle is open to subduction from the atmosphere and mass transfer from the lower mantle. Constraints are derived that can be incorporated into models for terrestrial volatile acquisition: (1) Calculated lower-mantle Xe-isotopic ratios indicate that the fraction of radiogenic Xe produced by I-129 and Pu-244 during the first about 10(exp 8) yr was lost, a conclusion also drawn for atmospheric Xe. Thus, either the Earth was made from materials that had lost >99% of rare gases about (0.7-2) x 10(exp 8) yr after the solar system formed, or gases were then lost from the fully formed Earth. (2) Concentrations of 3He and 20Ne in the lower mantle were established after these losses. (3) Neon-isotopic data indicates that mantle Ne has solar composition. The model allows for solar Ar/Ne and Xe/Ne in the lower mantle if a dominant fraction of upper mantle Ar and Xe are subduction-derived. If Earth formed in the presence of the solar nebula, it could have been melted by accretional energy and the blanketing effect of a massive, nebula-derived atmosphere. Gases from this atmosphere would have been sequestered within the molten Earth by dissolution at the surface and downward mixing. It was found that too much Ne would be dissolved in the Earth unless the atmosphere began to escape when the Earth was only partially assembled. Here we consider conditions required to initially dissolve sufficient rare gases to account for the present lower mantle concentrations after subsequent losses at 10(exp 8) yr. It is assumed that equilibration of the atmosphere with a thoroughly molten mantle was rapid, so that initial abundances of gases retained in any mantle layer reflected surface conditions when the layer solidified. For subsequent gas loss of 99.5% and typical solubility coefficients, a total pressure of 100 atm was required for an atmosphere of solar composition. Calculations of the pressure at the base of a primordial atmosphere indicate that this value might be exceeded by an order of magnitude or more for an atmosphere supported by accretional energy. Surface temperatures of about 4000 K would have been produced, probably high enough to melt the deep mantle. Initial distributions of retained rare gases would then be determined by the history of surface pressure and temperature during mantle cooling and solidification, i.e., the coupled cooling of Earth and atmosphere. The Earth's thermal state was determined by its surface temperature and the efficiency of convection in the molten mantle, estimated to be sufficient to maintain an adiabatic gradient. Because the melting curve is steeper than the adiabat, solidification of the mantle proceeded outward from the interior. Incorporation of atmospheric gases in the mantle therefore occurred over a range in surface temperature of a few thousand degrees Kelvin. The thermal state of the atmosphere was controlled by total luminosity of the Earth (energy) released by accreting planetesimals and the cooling Earth), nebular temperature and pressure, and atmospheric opacity. The energy released by accretion declined with time as did nebular pressure. Analytical solutions for an idealized (constant opacity radiative atmosphere show that declining energy sources under constant nebular conditions result in slowly diminishing surface temperature but dramatically increasing surface pressure. For such an atmosphere with declining nebular pressure but constant total luminosity, surface pressure decreases gradually with decreasing temperaure. A decline in accretion luminosity might be compensated by energy released as the mantle cools for about 10(exp 5) year, after which luminosity must decline. The total complement of dissolved rare gases will depend on the particular evolutionary path determined by the declining accretional luminosity, the Earth thermal history, removal of the nebula, and opacity variations of the atmosphere. Models for these coupled evolutionary histories for Earth's acquisition of nebular-derived noble gases are in progress. The later losses required at about 10(exp 8) yr (depleting the interior concentrations of the sequestered solar gases by a factor of > 100) were presumably related to the major impact in which the Moon formed.

Porcelli, D.↗
NASA NTRS2013

Carbon Nanotube Microarrays Grown on Nanoflake Substrates

This innovation consists of a new composition of matter where single-walled carbon nanotubes (SWNTs) are grown in aligned arrays from nanostructured flakes that are coated in Fe catalyst. This method of growth of aligned SWNTs, which can yield well over 400 percent SWNT mass per unit substrate mass, exceeds current yields for entangled SWNT growth. In addition, processing can be performed with minimal wet etching treatments, leaving aligned SWNTs with superior properties over those that exist in entangled mats. The alignment of the nanotubes is similar to that achieved in vertically aligned nanotubes, which are called "carpets. " Because these flakes are grown in a state where they are airborne in a reactor, these flakes, after growing SWNTs, are termed "flying carpets. " These flakes are created in a roll-to-roll evaporator system, where three subsequent evaporations are performed on a 100-ft (approx. =30-m) roll of Mylar. The first layer is composed of a water-soluble "release layer, " which can be a material such as NaCl. After depositing NaCl, the second layer involves 40 nm of supporting layer material . either Al2O3 or MgO. The thickness of the layer can be tuned to synthesize flakes that are larger or smaller than those obtained with a 40-nm deposition. Finally, the third layer consists of a thin Fe catalyst layer with a thickness of 0.5 nm. The thickness of this layer ultimately determines the diameter of SWNT growth, and a layer that is too thick will result in the growth of multiwalled carbon nanotubes instead of single-wall nanotubes. However, between a thickness of 0.5 nm to 1 nm, single-walled carbon nanotubes are known to be the primary constituent. After this three-layer deposition process, the Mylar is rolled through a bath of water, which allows catalyst-coated flakes to detach from the Mylar. The flakes are then collected and dried. The method described here for making such flakes is analogous to that which is used to make birefringent ink that is coated on U.S. currency. After deposition, the growth is carried out in a hot-filament chemical vapor deposition apparatus. A tungsten hot filament placed in the flow of H2 at a temperature greater than 1,600 C creates atomic hydrogen, which serves to reduce the Fe catalyst into a metallic state. The catalyst can now precipitate SWNTs in the presence of growth gases. The gases used for the experiments reported are C2H2, H2O, and H2, at rates of 2, 2, and 400 standard cubic centimeters per minute (sccm), respectively. In order to retain the flakes, a cage is constructed by spot welding stainless steel or copper mesh to form an enclosed area, in which the flakes are placed prior to growth. This allows growth gases and atomic hydrogen to reach the flakes, but does not allow the flakes, which rapidly nucleate SWNTs, to escape from the cage.

Schmidt, Howard K.↗
DOE OSTI2020

Disulfonamide Ligands as f-Element Extractants from Alkaline High-Level Waste

Almost 100 million gallons of high level waste (HLW) has been generated from defense reprocessing programs to support nuclear weapons production. HLW is currently stored at the Hanford and Savannah River Sites (SRS) [1]. It contains radioactive components, such as {sup 137}Cs, {sup 99}Tc and {sup 90}Sr, as well as large amounts of non-radioactive species, including solvated cations and insoluble metal hydroxides. HLW has high concentration of soluble hydroxides ([OH{sup -}] = 2 M at SRS [2]), complexing inorganic anions ([NO{sub 3}{sup -}] ∼ 0.65 - 3.7 M at SRS [2]) and a high ionic strength. Even though the majority of actinide component in alkaline HLW is precipitated, studies of An(III) and Ln(III) complexation in highly alkaline solutions in the presence of high nitrate concentrations have showed that soluble nitrate complexes can be formed [3]. The current treatment of HLW at SRS currently consists of two processes: The Actinide Removal Process (ARP) and the Next-Generation Caustic-Side Solvent Extraction process (NG-CSSX). Strontium and actinides are removed by sorption on monosodium titanate through the Actinide Removal Process (ARP) commonly referred to as the alpha-strike step [4]. Then, cesium is selectively extracted from the alkaline media via the Caustic-Side Solvent Extraction (CSSX) process [5]. The CSSX solvent consists of a calix[4]arene-crown-6 extractant dissolved in an inert hydrocarbon matrix containing i) a solvent modifier (alkylphenoxy alcohol) which increases extractant solubility and prevents third phase formation, and ii) a suppressor (trioctylamine or guanidine) - that mitigates surfactant effects. The CSSX process removes {sup 137}Cs selectively and rapidly, yet the post- CSSX aqueous stream may still contain high amounts of An, thus requiring a second ARP treatment (referred to as 'alpha-finishing') for some tanks. Despite the success of the ARP process in removing Sr and An, it often represents the kinetic bottleneck of integrated processing, as it is slower than solvent extraction. Understanding the complexation of actinides by organic ligands that are compatible with the CSSX process could eventually lead to a combined caustic-side Cs/Sr/actinide extraction process with better economics due to a reduced amount of monosodium titanate and/or a shorter required contact time with titanate during ARP. This would ensure a low-activity waste (LAW) stream with no actinides without additional ARP processing post-CSSX. Disulfonamides were studied for extraction of Sm(III) from alkaline aqueous media of pH 10-14 into dichloromethane. Up to 82% of Sm(III) was extracted from solutions of pH 12.5 -13.5 and up to 84% from solutions of pH 10.5 - 11.5. These results show some resemblance with Am extraction results by calixarene ligands previously reported [10]. Kinetic studies demonstrated that even 5 min is enough to complete stripping, whereas extraction is time-limiting process and requires up to 20 h for efficient removal of Sm(III) from alkaline aqueous media. Determination of composition of complexes in solution after extraction by the equilibrium shift method showed a 1:1 Sm(III):dsa-2 complexation ratio for the extracted species.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Chromium and Vanadium Incorporation in Sulfate-Containing Sodium Aluminoborosilicate Glass

In the composition space for Hanford low-activity nuclear waste glass, the waste loading of some formulations is limited by poor incorporation of sulfate. In particular, certain elements identified in previous studies tend to raise or lower sulfate solubility in borosilicate glass. The aim of the current study is to understand how vanadium and chromium each affect a sulfate-containing sodium aluminoborosilicate glass structure. Glass transition temperature, mass density, visible absorption, and Raman scattering were measured to investigate changes in the glass structure. Both Cr6+ (CrO42-) and Cr3+ were found in the chromium-containing glasses while vanadium primarily existed in the 5+ oxidation state in the vanadium-containing glasses. Electron probe microanalysis determined elemental compositions to assess retention of components. Increasing Cr2O3 caused saturation of Cr concentration within the glass and formation of crystalline eskolaite (Cr2O3). On the other hand, all the targeted V was incorporated into the glass. A fraction of batched S was not incorporated in any glass, presumably due to volatilization during melting. Apparently, the details of incorporation of Cr, and to an extent V, are different depending on whether sulfur is added as in this study or in oversaturated conditions as described in the literature, where Cr partitions to a sulfate-containing salt phase.

Borosilicate glass, Waste Glass, vanadium chemistr↗
NASA NTRS2014

Producing Zirconium Diboride Components with Complex, Near-Net Shape Geometries by Aqueous Room-Temperature Injection Molding

Room-temperature injection molding is proposed as a novel, low-cost and more energy efficient manufacturing process capable of forming complex-shaped zirconium diboride (ZrB2) parts. This innovative processing method utilized aqueous suspensions with high powder loading and a minimal amount (5 vol.) of water-soluble polyvinylpyrrolidone (PVP), which was used as a viscosity modifier. Rheological characterization was performed to evaluate the room-temperature flow properties of ZrB2-PVP suspensions. ZrB2 specimens were fabricated with high green body strength and were machinable prior to binder removal despite their low polymer content. After binder burnout and pressureless sintering, the bulk density and microstructure of specimens were characterized using Archimedes technique and scanning electron microscopy. X-Ray Diffraction was used to determine the phase compositions present in sintered specimens. Ultimate strength of sintered specimens will be determined using ASTM C1323-10 compressive C-ring test.

Near-Net Shape Forming↗
DOE OSTI2020

Mercury Speciation via Diffusive Gradients Thin-Films Technology

Objectives: Develop and test various diffusive gradient in thin films (DGT) samplers for mercury - SRNL is developing reactive DGTS (rDGTs). Test chemistry to differentiate methylmercury from total and/or inorganic mercury in environmental samples. Fabricate and test rDGT samplers for deployment. Deploy the rDGTs in variable settings. Mercury is a persistent-bioaccumulative-toxic environmental pollutant. Mercury exists in different species such as elemental, inorganic, and methyl. Mercury speciation determine mercury behavior and toxicity. For example, methylmercury strongly accumulates in biota such as fish resulting in potential human health impacts. DGTs are innovative samplers to measure water concentration by diffusion and capture. Types of Hg DGTs used: Total Hg, Inorganic Hg, and Methyl Hg. Deployment Sites: Upper Three Runs, Lower Three Runs, Steele Creek, East Fork Poplar Creek (SRNL Sites), Horizons Creek, NOA Creek, Bruners Creek (ORNL Sites). DGT concentration estimates closely matched alternative measurements for soluble mercury at each Oak Ridge site - DGTs did not respond to particulate mercury. DGTs provide a representative measure for biota uptake since they are left out longer which allows for an average exposure concentration. DMA-80 provided an efficient and quick analysis. Variability in site location made a difference in Hg species. DGT preparations and sampling wasn't as quick and simple as microcolumn technology. Copper reagent degraded agarose gel - more work and cleaner data are needed to assess speciation in rDGTs. Future Work: Use cross-linked polyacrylamide for the collection layer for a stronger plastic. Make a copper diffusion layer without agarose. Test copper separation in lab using realistic stream conditions such as high organic carbon.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2012

Non-Toxic, Low-Freezing, Drop-In Replacement Heat Transfer Fluids

A non-toxic, non-flammable, low-freezing heat transfer fluid is being developed for drop-in replacement within current and future heat transfer loops currently using water or alcohol-based coolants. Numerous water-soluble compounds were down-selected and screened for toxicological, physical, chemical, compatibility, thermodynamic, and heat transfer properties. Two fluids were developed, one with a freezing point near 0 C, and one with a suppressed freezing point. Both fluids contain an additive package to improve material compatibility and microbial resistance. The optimized sub-zero solution had a freezing point of 30 C, and a freezing volume expansion of 10-percent of water. The toxicity of the solutions was experimentally determined as LD(50) greater than 5g/kg. The solutions were found to produce minimal corrosion with materials identified by NASA as potentially existing in secondary cooling loops. Thermal/hydrodynamic performance exceeded that of glycol-based fluids with comparable freezing points for temperatures Tf greater than 20 C. The additive package was demonstrated as a buffering agent to compensate for CO2 absorption, and to prevent microbial growth. The optimized solutions were determined to have physically/chemically stable shelf lives for freeze/thaw cycles and longterm test loop tests.

Cutbirth, J. Michael↗
NASA NTRS1994

Protein crystal growth in microgravity: Temperature induced large scale crystallization of insulin

One of the major stumbling blocks that prevents rapid structure determination using x-ray crystallography is macro-molecular crystal growth. There are many examples where crystallization takes longer than structure determination. In some cases, it is impossible to grow useful crystals on earth. Recent experiments conducted in conjuction with NASA on various Space Shuttle missions have demonstrated that protein crystals often grow larger and display better internal molecular order than their earth-grown counterparts. This paper reports results from three Shuttle flights using the Protein Crystallization Facility (PCF). The PCF hardware produced large, high-quality insulin crystals by using a temperature change as the sole means to affect protein solubility and thus, crystallization. The facility consists of cylinders/containers with volumes of 500, 200, 100, and 50 ml. Data from the three Shuttle flights demonstrated that larger, higher resolution crystals (as evidenced by x-ray diffraction data) were obtained from the microgravity experiments when compared to earth-grown crystals.

Long, Marianna M.↗
NASA NTRS2002

Tissue engineering skeletal muscle for orthopaedic applications

With current technology, tissue-engineered skeletal muscle analogues (bioartificial muscles) generate too little active force to be clinically useful in orthopaedic applications. They have been engineered genetically with numerous transgenes (growth hormone, insulinlike growth factor-1, erythropoietin, vascular endothelial growth factor), and have been shown to deliver these therapeutic proteins either locally or systemically for months in vivo. Bone morphogenetic proteins belonging to the transforming growth factor-beta superfamily are osteoinductive molecules that drive the differentiation pathway of mesenchymal cells toward the chondroblastic or osteoblastic lineage, and stimulate bone formation in vivo. To determine whether skeletal muscle cells endogenously expressing bone morphogenetic proteins might serve as a vehicle for systemic bone morphogenetic protein delivery in vivo, proliferating skeletal myoblasts (C2C12) were transduced with a replication defective retrovirus containing the gene for recombinant human bone morphogenetic protein-6 (C2BMP-6). The C2BMP-6 cells constitutively expressed recombinant human bone morphogenetic protein-6 and synthesized bioactive recombinant human bone morphogenetic protein-6, based on increased alkaline phosphatase activity in coincubated mesenchymal cells. C2BMP-6 cells did not secrete soluble, bioactive recombinant human bone morphogenetic protein-6, but retained the bioactivity in the cell layer. Therefore, genetically-engineered skeletal muscle cells might serve as a platform for long-term delivery of osteoinductive bone morphogenetic proteins locally.

Review↗
DOE OSTI2024

Separation of Lipoproteins for Quantitative Analysis of 14 C-Labeled Lipid-Soluble Compounds by Accelerator Mass Spectrometry

To date, 14 C tracer studies using accelerator mass spectrometry (AMS) have not yet resolved lipid-soluble analytes into individual lipoprotein density subclasses. The objective of this work was to develop a reliable method for lipoprotein separation and quantitative recovery for biokinetic modeling purposes. The novel method developed provides the means for use of small volumes (10–200 µL) of frozen plasma as a starting material for continuous isopycnic lipoprotein separation within a carbon- and pH-stable analyte matrix, which, following post-separation fraction clean up, created samples suitable for highly accurate 14 C/ 12 C isotope ratio determinations by AMS. Manual aspiration achieved 99.2 ± 0.41% recovery of [5- 14 CH 3 ]-(2R, 4'R, 8'R)-α-tocopherol contained within 25 µL plasma recovered in triacylglycerol rich lipoproteins (TRL = Chylomicrons + VLDL), LDL, HDL, and infranatant (INF) from each of 10 different sampling times for one male and one female subject, n = 20 total samples. Small sample volumes of previously frozen plasma and high analyte recoveries make this an attractive method for AMS studies using newer, smaller footprint AMS equipment to develop genuine tracer analyses of lipophilic nutrients or compounds in all human age ranges.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2004

Determining the Thermal Properties of Space Lubricants

Many mechanisms used in spacecrafts, such as satellites or the space shuttle, employ ball bearings or gears that need to be lubricated. Normally this is not a problem, but in outer space the regular lubricants that are used on Earth will not function properly. Regular lubricants will quickly vaporize in the near vacuum of space. A unique liquid called a perfluoropolyalkylether (PFPE) has an extremely low vapor pressure, around l0(exp -10) torr at 20 C, and has been used in numerous satellites and is currently used in the space shuttle. Many people refer to the PFPEs as "liquid Teflon". PFPE lubricants however, have a number of problems with them. Lubricants need many soluble additives, especially boundary and anti-wear additives, in them to function properly. All the regular known boundary additives are insoluble in PFPEs and so PFPEs lubricate poorly under highly loaded conditions leading to many malfunctioning ball bearings and gears. JAXA, the Japanese Space Agency, is designing and building a centrifuge rotor to be installed in the International Space Station. The centrifuge rotor is part of a biology lab module. They have selected a PFPE lubricant to lubricate the rotor s ball bearings and NASA bearing experts feel this is not a wise choice. An assessment of the centrifuge rotor design is being conducted by NASA and part of the assessment entails knowing the physical and thermal properties of the PFPE lubricant. One important property, the thermal diffusivity, is not known. An experimental apparatus was set up in order to measure the thermal diffusivity of the PFPE. The apparatus consists of a constant temperature heat source, cylindrical Pyrex glassware, a thermal couple and digital thermometer. The apparatus was tested and calibrated using water since the thermal diffusivity of water is known.

Maldonado, Christina M.↗
NASA NTRS2016

Localized and Areally Extensive Alterations in Marathon Valley, Endeavour Crater Rim, Mars

Mars Exploration Rover Opportunity is exploring the rim of 22 km diameter, Noachian-aged Endeavour crater. Marathon Valley cuts through the central region of the western rim providing a window into the local lower rim stratigraphic record. Spectra from the Compact Reconnaissance Imaging Spectrometer for Mars show evidence for the occurrence of Fe-Mg smectite in this valley, indicating areally extensive and distinct lithologic units and/or styles of aqueous alteration. The Alpha Particle X-ray Spectrometer has determined the compositions of 59 outcrop targets on untreated, brushed and abraded surfaces. Rocks in the Marathon Valley region are soft breccias composed of mm- to cm-sized darker clasts set in a lighter-toned, finegrained matrix. They are basaltic in non-volatile-element composition and compositionally similar to breccias investigated elsewhere on the rim. Alteration styles recorded in the rocks include: (1) Enrichments in Si, Al, Ti and Cr in more reddish-colored rock, consistent with leaching of more soluble cations and/or precipitation of Si +/- Al, Ti, Cr from fluids. Coprecipitation of Ge-rich phases with Si occurred in the western area only; high water:rock is indicated. Pancam multispectral observations indicate higher nanophase ferric oxide contents, but the rocks have lower Fe contents. The highly localized nature of the red zones indicate they cannot be the source of the widespread smectite signature observed from orbit. (2) Outcrops separated by approximately 65 m show common compositional changes between brushed and abraded (approximately 1 mm deep) targets: increases in S and Mg; decreases in Al, Cl and Ca. These changes are likely due to relatively recent, surface-related alteration of valley rocks and formation of surface coatings under low water:rock. (3) One target, from the center of a region of strong CRISM smectite signature, shows modest differences in composition (higher Si, K; lower Mn) compared to most Marathon Valley rocks, while another target approximately 40 cm away on the same outcrop does not; a change towards smectite bulk compositions is not observed. The smectite signature likely resulted from alteration under low water:rock such that primary minerals were partially altered to phyllosilicates, but wholesale leaching of cations by fluids did not occur.

Mittlefehldt, David W.↗
NASA NTRS1980

Gas phase hydrogen permeation in alpha titanium and carbon steels

Commercially pure titanium and heats of Armco ingot iron and steels containing from 0.008-1.23 w/oC were annealed or normalized and machined into hollow cylinders. Coefficients of diffusion for alpha-Ti and alpha-Fe were determined by the lag-time technique. Steady state permeation experiments yield first power pressure dependence for alpha-Ti and Sievert's law square root dependence for Armco iron and carbon steels. As in the case of diffusion, permeation data confirm that alpha-titanium is subject to at least partial phase boundary reaction control while the steels are purely diffusion controlled. The permeation rate in steels also decreases as the carbon content increases. As a consequence of Sievert's law, the computed hydrogen solubility decreases as the carbon content increases. This decreases in explained in terms of hydrogen trapping at carbide interfaces. Oxidizing and nitriding the surfaces of alpha-titanium membranes result in a decrease in the permeation rate for such treatment on the gas inlet surfaces but resulted in a slight increase in the rate for such treatment on the gas outlet surfaces. This is explained in terms of a discontinuous TiH2 layer.

Johnson, D. L.↗
DOE OSTI2022

Improved Moisture Management Technology for Eco-N-Control Fertilizer

Three fertilizer technologies to manage nitrogen (N) release rates in soil dominate the market today: 1) bulk controlled-release technologies, which use the intrinsic solubility properties of a N-organic co-polymer to control N release; 2) barrier-based controlled-release technologies, which use porous polymer or sulfur coatings as a physical barrier to control N release from encapsulated N nutrients; and 3) slow-release technologies, which use enzyme inhibitors to chemically slow down the transformation of N nutrients into ammonia (NH 3 ) or to temporarily reduce populations of bacteria in the soil that are responsible for converting ammonium (NH 4 + ) to highly soluble nitrates. These technologies are expensive and provide only limited control of N-release rates. Also, from another environmental perspective, synthetic polymer coatings do not decompose easily and will accumulate over time with continuous application of fertilizer. For most of the past two decades we have been developing the Eco-N-Control solid-nitride fertilizer technology, a type of bulk controlled-release technology. With Eco-N-Control, solid-nitride compounds weather like a mineral, slowly releasing N at a rate determined by their composition. Testing by an industrial collaborator, however, showed that earlier versions of Eco-N-Control released at 25% of the desired rate when deployed in unsaturated soils. The overall goal of the current project, therefore, was to strengthen our IP position and the potential for licensing of Eco-N-Control solid-nitride fertilizer technology by developing new ways to manage the level of moisture in contact with the fertilizer when applied to soil thereby ensuring the desired N-release rate. We achieved this goal by developing a biodegradable polymer cross-linking approach that substantially improved performance of our patented solid-nitride fertilizer. We found that cross-linking an environmentally friendly and biodegradable polymer with a mixture of solid nitrides, other N-nutrient compounds and other additives offers several advantages: 1) mechanical robustness of fertilizer beads, 2) chemical stability during storage, 3) maintenance of sufficient water content in the vicinity of the nitride, and 4) control of N-release rates. We also updated our N-release testing protocol to more realistically simulate the conditions found in soil. Finally, we filed an invention disclosure record to protect these new aspects of Eco-N-Control technology, which offers a potential way to lower both agricultural and industrial pollution by providing an efficient N-delivery mechanism to plants.

42 ENGINEERING↗
DOE OSTI2022

Alternate Methods for Cleaning Zirconium Plate

The United States High Performance Research Reactor Conversion Program identified the need to transition from highly enriched uranium fuel to lowly enriched uranium fuel for high power research and civil reactors. One of the fuel configurations selected for these reactors was a uranium (U) foil alloyed with 10% molybdenum (Mo). The U-10Mo fuel foil was then covered with a zirconium (Zr) interlayer and pressed into an aluminum cladding. Idaho National Laboratory prescribed a need to remove surface oxidation on the Zr prior to bonding it with U-10Mo fuel foil. To determine the best method of oxidation removal, a variety of polishing methods, including hand polishing with a diamond paste or Scotch-Brite™ pads, mechanically wet-polishing with abrasive belts, and chemical etching with hydrofluoric/nitric acid mixtures, were investigated on pre-polished Zircaloy 702 sheets purchased directly from the manufacturer. No change in surface roughness was detected using any of these methods relative to the as-received material. In fact, scanning electron microscopy detected grit from hand polishing with Amplex Grade 30 waste soluble diamond paste and Scotch-Brite™ pads. Visible staining was found, and fluorine detected via X-ray photoelectron spectroscopy on the flash etching samples. These contaminants were not seen on the as-received material. In addition to the need to remove the oxide layer on the Zr prior to co-rolling, there are concerns that the Neolube debonding agent on the co-rolling can may contaminate the Zr surface after co-rolling. The experimental results found that zirconium in contact with Neolube coated steel plates was easily cleaning with ethanol wiping after heat treated and no carbide inclusions remained on the surface. Overall, all cleaning methods tested did not significantly change the surface roughness of the plates or reduce the oxide layer present on the zirconium. Carbon was found on all the samples, before and after cleaning, except for the flash etch samples which detected fluorine instead. The insignificant changes seen in the cleaned plates relative to the as received plates question the need for cleaning prior to rolling. Further investigation in the requirements for cleaning at this step is recommended. Current methods for cleaning the surface after hot rolling with alcohol appear sufficient. After hot rolling, if Neolube does peel off the can and onto the zirconium coated foil surface, a dry abrasive or diamond paste polish is not recommended due to the chance of abrasive being embedded into the surface. However, the ability of an etchant to lift the lubricant off the zirconium surface indicates that a spot etch method could work to clean specific spots where Neolube is present, if the need arises.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
NASA NTRS2002

Fabrication and Electromagnetic Characterization of Novel Self-Metallized Thin Films

Unique, self-metallized films were investigated for deployable reflector antenna applications at L-band. Polyamic acid resins or soluble polyimides were doped with metal complexes, cast into films, and thermally cured. Each resulting film had a metallic layer on one side, adhering unfailingly to the polymer. Metallization was successful for silver or palladium in 3,3',4,4'-benzophenonetetracarboxylic acid dianhydride (BTDA) and 4,4'- oxydianiline and for gold in BTDA and 2,2-bis[4-(4- aminophenoxy)phenyl]hexafluoropropane (4-BDAF) or the space durable polyimide, 2,2-bis(3,4-dicarboxyphenyl)- hexafluoropropane dianhydride and 4-BDAF (LaRCCP1). Reflectivity, transmissivity, and emissivity were determined, using an HP 8510 Vector Network Analyzer, to within 0.001 precision and accuracy. A custom-made test fixture/positioner, a thru-reflect-line calibration, and calculated reflection coefficients were used. The Ag film proved most suitable for further study, with 0.9957 reflectivity and 0.0042 emissivity. The Pd films were 0.89 reflective and 0.11 emissive; both Au films tested entirely transmissive. Transmission and scanning electron micrographs, S-parameters, and power coefficients are shown.

Mackenzie, Anne I.↗