A Genomic Island of Vibrio cholerae Encodes a Three-Component Cytotoxin with Monomer and Protomer Fo
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Herrera, Alfa↗
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Melting relations and elemental distribution of portion of the system Fe-S-Si-O to 32 KB with planetary application
The melting relations and distribution of K and Cs in portions of the system was determined at high pressures. Ferrosilite is stable as a primary phase at high pressures because of the incongruent melting of ferrosilite to quartz plus liquid and the boundary between the one and two liquid fields on the joint Fe(1-x) O-FeS-SiO2 shifts away from silica with increasing pressures. Potassium K was found to have limited solubility in metal sulfide liquids at pressures up to 45 kb. The speculation that K may dissolve significantly in metal-metal sulfide liquids after undergoing first order isomorphic transition was tested by determining the distribution of Cs between sulfide and silicate liquids as an analogy to K. At 45 kb, 1400 C and 27 kb, 1300 C only limited amounts of Cs were detected in quench sulfide liquids even at pressures beyond the isomorphic transition of Cs.
Huang, W. L.↗
Alternate working fluids for solar air conditioning applications
An experimental investigation of sixteen different refrigerant-absorbent fluid pairs has been carried out in order to determine their suitability as the working fluid in a solar-powered absorption cycle air conditioner. The criteria used in the initial selection of a refrigerant-absorbent pair included: high affinity (large negative deviation from Raoult's Law), high solubility, low specific heat, low viscosity, stability, corrosive properties, safety, and cost. For practical solar considerations of a fluid pair, refrigerants were selected with low boiling points whereas absorbent fluids were selected with a boiling point considerably above that of the refrigerant. Additional restrictions are determined by the operating temperatures of the absorber and the generator; these temperatures were specified as 100 F (39 C) and 170 F (77 C). Data are presented for a few selected pressures at the specified absorber and generator temperatures.
Evans, R. D.↗
Biodegradation of Fresh vs. Oven-Dried Inedible Crop Residue in a Continuously Stirred Tank Reactor
The degradation of soluble organics and mineral recovery from fresh and oven-dried biomass were compared in an Intermediate-Scale Aerobic Bioreactor (8 L working volume) to determine if drying crop residue improves performance in a continuously stirred tank reactor (CSTR). The study was conducted in an Intermediate-Scale Aerobic Bioreactor (ISAB) CSTR with dimensions of 390 mm height x 204 mm diameter. The pH in the bioreactor was controlled at 6.0, temperature at 30 C, and aeration at 7.0 L/min. Gases monitored were CO2 evolution and dissolved oxygen. Homogeneously mixed wheat cultures, used either fresh or oven-dried biomass and were leached, then placed in the ISAB for a 4-day degradation period. Studies found that mineral recovery was greater for leached oven-dried crop residue. However, after activity by the mixed microbial communities in the ISAB CSTR, there were little notable differences in the measured mineral recovery and degradation of soluble organic compounds. Degradation of soluble organic compounds was also shown to improve for leached oven-dried crop residue, but after mixing in the CSTR the degradation of the fresh biomass seemed to be slightly greater. Time for the biomass to turn in the CSTR appeared to be one factor for the experimental differences between the fresh and oven-dried biomass. Other factors, although not as defined, were the differing physical structures in the cell walls and varying microbial components of the fresh and oven-dried treatments due to changes in chemical composition after drying of the biomass.
Crawford, Kamau↗
A fusion of the Bacteroides fragilis ferrous iron import proteins reveals a role for FeoA in stabilizing GTP-bound FeoB
Iron is an essential element for nearly all organisms, and under anoxic and/or reducing conditions, Fe 2+ is the dominant form of iron available to bacteria. The ferrous iron transport (Feo) system is the primary prokaryotic Fe 2+ import machinery, and two constituent proteins (FeoA and FeoB) are conserved across most bacterial species. However, how FeoA and FeoB function relative to one another remains enigmatic. In this work, we explored the distribution of feoAB operons encoding a fusion of FeoA tethered to the N-terminal, G-protein domain of FeoB via a connecting linker region. We hypothesized that this fusion poises FeoA to interact with FeoB to affect function. To test this hypothesis, we characterized the soluble NFeoAB fusion protein from Bacteroides fragilis, a commensal organism implicated in drug-resistant infections. Using X-ray crystallography, we determined the 1.50-Å resolution structure of BfFeoA, which adopts an SH3-like fold implicated in protein–protein interactions. Using a combination of structural modeling, small-angle X-ray scattering, and hydrogen–deuterium exchange mass spectrometry, we show that FeoA and NFeoB interact in a nucleotide-dependent manner, and we mapped the protein–protein interaction interface. Finally, using guanosine triphosphate (GTP) hydrolysis assays, we demonstrate that BfNFeoAB exhibits one of the slowest known rates of Feo-mediated GTP hydrolysis that is not potassium-stimulated. Importantly, truncation of FeoA from this fusion demonstrates that FeoA–NFeoB interactions function to stabilize the GTP-bound form of FeoB. Taken together, our work reveals a role for FeoA function in the fused FeoAB system and suggests a function for FeoA among prokaryotes.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Uniform secondary current distribution at disk electrodes under Tafel kinetics enabled by concentric current-shielding rings
Non-uniform secondary current distribution at rotating disk electrodes (RDE) is a common problem when using resistive electrolyte media or large applied currents. In a recent publication, we have shown that auxiliary electrodes such as the ring of a rotating ring disk electrode (RRDE) can help suppress current non-uniformities at the disk enabling reliable electroanalytical measurements. However, this previous work considered linear kinetics where current distribution non-uniformities were moderate. In the present contribution, we consider current distribution non-uniformities encountered under Tafel kinetics. We show, for the case of 2,5-dihydroxy-1,4-benzoquinone (DHBQ) reduction, that optimally chosen ring conditions serve to provide effective shielding at the disk edge rendering the overall disk current distribution to be uniform. Numerical modeling and scaling analysis (using the Wagner number) are presented to aid a user in determining the optimal ring current density for achieving uniform disk current distribution under Tafel kinetics. This approach is especially useful when studying soluble-soluble redox transitions for which, unlike deposit distribution in electrodeposition, the current distribution non-uniformity is not visually apparent.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Stability of aqueous neodymium complexes in carbonate-bearing solutions from 100–600 °C
Rare earth element exploration requires a quantitative understanding of factors governing their mobilization and economic concentration. However, the behavior of rare earth elements in carbonate- bearing hydrothermal fluids associated with carbonatite-hosted deposits is poorly understood, and conflicting mechanisms of rare earth transport by anionic ligands and alkali behavior have been described. Here, we report quantitative data to characterize the role of carbonate-bearing solutions in the hydrothermal mobilization of neodymium. Solubility studies of neodymium phosphate were performed at temperatures ranging from 100 to 600 °C in carbonate-bearing solutions. The thermodynamic data determined for the predominant complex were used to model the separation of neodymium from thorium in a simple flow-through system based on fluid and mineral compositions characteristic of carbonatite deposits. Our data suggest that neodymium transport is controlled by the stability of the carbonate species NdCO 3 OH o , and at temperatures of 500–600 °C, the concentrations of neodymium in solutions can reach ~1000 ppm.
58 GEOSCIENCES↗
Structure-property study of keto-ether polyimides
As part of an on-going effort to develop an understanding of how changes in the chemical structure affect polymer properties, an empirical study was performed on polyimides containing only ether and/or carbonyl connecting groups in the polymer backbone. During the past two decades the structure-property relationships in linear aromatic polyimides have been extensively investigated. More recently, work has been performed to study the effect of isomeric attachment of keto-ether polyimides on properties such as glass transition temperature and solubility. However, little work has been reported on the relation of polyimide structure to mechanical properties. The purpose of this study was to determine the effect of structural changes in the backbone of keto-ether polyimides on their mechanical properties, specifically, unoriented thin film tensile properties. This study was conducted in two stages. The purpose of the initial stage was to examine the physical and mechanical properties of a representative group (four) of polyimide systems to determine the optimum solvent and cure cycle requirements. These optimum conditions were then utilized in the second stage to prepare films of keto-ether polyimides which were evaluated for mechanical and physical properties. All of the polyimides were prepared using isomers of oxydianiline (ODA) and diaminobenzophenone (DABP) in combination with 3,3',4,4'-benzophenonetetracarboxylic dianhydride (BTDA) and 4,4'-oxydiphthalic anhydride (ODPA).
Dezern, James F.↗
The Feasibility of Bulk Crystallization as an Industrial Purification and Production Technique for Proteins
Bulk crystallization in stirred vessels is used industrially for the recovery and purification of many inorganic and organic materials. Although much has been written on the crystallization of proteins for X-ray diffraction analysis, very little has been reported on the application of bulk crystallization in stirred vessels. In this study, a 1-liter, seeded, stirred, batch crystallizer was used with ovalbumin as a model protein to test the feasibility of this crystallization method as a recovery and purification process for proteins. Results were obtained for ovalbumin solubility, nucleation thresholds, crystal breakage and crystal growth kinetics in bulk solution under a range of operating conditions of pH and ammonium sulphate concentration (Judge et al., 1996). Experiments were also performed to determine the degree of purification that can be achieved by the crystallization of ovalbumin from a mixture of proteins. The effect of the presence of these proteins upon the ovalbumin crystal growth kinetics was also investigated (Judge et al., 1995). All of these aspects are essential for the design of bulk crystallization processes which have not previously been reported for proteins. Results from a second study that investigated the effect of structurally different proteins on the solubility, crystal growth rates and crystal purity of chicken egg white lysozyme are also presented (Judge et al., 1997). In this case face growth rates were measured using lysozyme purified by liquid chromatography and the effect of the addition of specific protein impurities were observed on the (110) and (101) crystal faces. In these two studies the results are presented to show the feasibility and purifying ability of crystallization as a production process for proteins.
Judge, Russell A.↗
The solubility of NdPO 4 and DyPO 4 and stability of Nd and Dy chloride and hydroxyl complexes as a function of pH and salinity to 450 °C
The mobility of rare earth elements (REE) in geological systems is often controlled by the stability of monazite and xenotime, which are important hosts for the light and heavy REE. These REE phosphates constitute important resources and provide information on ore formation conditions and timing due to their uses as geothermometers and geochronometers. While the thermodynamic properties for these minerals are well-established up to high temperature and pressure, the properties for the aqueous REE complexes are not well constrained with limited information up to 300 °C. In this study, the solubility of synthetic NdPO 4 and DyPO 4 endmembers were measured in hydrothermal sub- to supercritical NaCl-bearing aqueous solutions from 350 at saturated water vapor pressure to 450 °C at 700 bar. The speciation of Nd and Dy was determined in acidic to alkaline solutions (pH 25 °C values from 2 to 10), and indicates that the hydroxyl species REE(OH) 2 + and REE(OH) 3 0 predominate at low salinity (0.01 mol/kg NaCl) with some contribution of REE chloride species REECl 2+ and REECl 2 + in acidic fluids. The REE phosphate solubility measured in these experiments is up to two orders of magnitude higher than predicted using existing thermodynamic properties from literature for aqueous species extrapolated from lower temperature data to supercritical conditions. To address this discrepancy, the thermodynamic properties of the REE aqueous species were optimized using GEMSFITS to derive the formation constants for the REE chloride (β Cl ) and hydroxyl (β OH ) complexes in the studied temperature range. This study highlights the importance of the hydroxyl species REE(OH) 2 + and REE(OH) 3 0 over a wide range of pH and temperature. As a result, the revised thermodynamic properties for Dy and Nd chloride and hydroxyl species more accurately predict the solubility of NdPO 4 and DyPO 4 and provide insight into the speciation and mobility of the light and heavy REE in hydrothermal supercritical fluids in the crust.
58 GEOSCIENCES↗
Hydrogen interactions with metals
Review of the literature on the nature and extent of hydrogen interactions with metals and the role of hydrogen in metal failure. The classification of hydrogen-containing systems is discussed, including such categories as covalent hydrides, volatile hydrides, polymeric hydrides, and transition metal hydride complexes. The use of electronegativity as a correlating parameter in determining hydride type is evaluated. A detailed study is made of the thermodynamics of metal-hydrogen systems, touching upon such aspects as hydrogen solubility, the positions occupied by hydrogen atoms within the solvent metal lattice, the derivation of thermodynamic functions of solid solutions from solubility data, and the construction of statistical models for hydrogen-metal solutions. A number of theories of hydrogen-metal bonding are reviewed, including the rigid-band model, the screened-proton model, and an approach employing the augmented plane wave method to solve the one-electron energy band problem. Finally, the mechanism of hydrogen embrittlement is investigated on the basis of literature data concerning stress effects and the kinetics of hydrogen transport to critical sites.
Mclellan, R. B.↗
Theory of Ostwald ripening in a two-component system
When a two-component system is cooled below the minimum temperature for its stability, it separates into two or more immiscible phases. The initial nucleation produces grains (if solid) or droplets (if liquid) of one of the phases dispersed in the other. The dynamics by which these nuclei proceed toward equilibrium is called Ostwald ripening. The dynamics of growth of the droplets depends upon the following factors: (1) The solubility of the droplet depends upon its radius and the interfacial energy between it and the surrounding (continuous) phase. There is a critical radius determined by the supersaturation in the continuous phase. Droplets with radii smaller than critical dissolve, while droplets with radii larger grow. (2) The droplets concentrate one component and reject the other. The rate at which this occurs is assumed to be determined by the interdiffusion of the two components in the continuous phase. (3) The Ostwald ripening is constrained by conservation of mass; e.g., the amount of materials in the droplet phase plus the remaining supersaturation in the continuous phase must equal the supersaturation available at the start. (4) There is a distribution of droplet sizes associated with a mean droplet radius, which grows continuously with time. This distribution function satisfies a continuity equation, which is solved asymptotically by a similarity transformation method.
Baird, J. K.↗
Electrochemical Reactivity of Hydrogen Storage Materials: Exploring Borohydride and Hydrazinium Salt Mixtures
Electrochemical characterization of hydrogen storage materials was conducted in a non-aqueous environment to investigate the direct electrochemical release and consumption of hydrogen and the potential for regeneration. We first address the challenge of minimal solubility of the synthetic precursors, sodium borohydride (NaBH 4 ) and hydrazinium bromide (N 2 H 5 Br), in both organic and inorganic solvents. We next determine and calibrate a reference electrode formulation compatible with our non-aqueous media and analytes that demonstrates a stable reference potential. We employ cyclic voltammetry (CV) to characterize the precursors and mixtures thereof. Each CV peak is assigned to a corresponding electrochemical reaction. Using the rate-dependent CV method and Randles–Ševčík equation, we calculate the diffusion coefficient of each chemical (NaBH 4 and N 2 H 5 Br). Analysis of the CVs, coupled with 11B NMR analysis, reveals a room temperature chemical transformation of NaBH 4 and N 2 H 5 Br mixtures into hydrazine borane (N 2 H 4 BH 3 ). These results are particularly significant, considering the limited information available on the electrochemical characterization of metal borohydride and hydrazinium salt in non-aqueous media. This work establishes a foundation for adapting a non-aqueous electrochemical system to further study the borohydride family of chemistries and to design and develop electrochemical devices for direct electrical and chemical energy interconversion with hydrogen storage materials.
08 HYDROGEN↗
Analysis of Dust Samples Collected from an Inland ISFSI Site (''Site B'').
In October of 2020, dust samples were collected from the surface of spent nuclear fuel (SNF) dry storage canisters during an inspection at an inland Independent Spent Fuel Storage Installation, the second inland site at which surface deposits have been sampled. The purpose of the sampling was to assess the composition and abundance of the soluble salts present on the canister surface, information which provides a metric for potential corrosion risks. The samples were delivered to Sandia National laboratories for analysis. At Sandia, the soluble salts were leached from the dust and quantified by ion chromatography. In addition, subsamples of the dust were taken for scanning electron microscopy to determine the texture and mineralogy of the dust and salts. The results of those analyses are presented in this report.
11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
Analysis of Dust Samples Collected from a Near-Marine East Coast ISFSI Site ("Site C")
In June of 2022, dust samples were collected from the surface of an in-service spent nuclear fuel dry storage canister during an inspection at an Independent Spent Fuel Storage Installation. The site is anonymous but is a near-marine or brackish water east coast location referred to here as "Site C". The purpose of the sampling was to assess the composition and abundance of the soluble salts present on the canister surface, information that provides a metric for potential corrosion risks. Following collection, the samples were delivered to Sandia National Laboratories for analysis. At Sandia, the soluble salts were leached from the dust and quantified by ion chromatography. In addition, subsamples of the dust were taken for scanning electron microscopy to determine the particle sizes, morphology, and mineralogy of the dust and salts. The results of those analyses are presented in this report.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Zirconium fluoride glass - Surface crystals formed by reaction with water
The hydrated surfaces of a zirconium barium fluoride glass, which has potential for application in optical fibers and other optical elements, were observed by scanning electron microscopy. Crystalline zirconium fluoride was identified by analysis of X-ray diffraction patterns of the surface crystals and found to be the main constituent of the surface material. It was also found that hydrated zirconium fluorides form only in highly acidic fluoride solutions. It is possible that the zirconium fluoride crystals form directly on the glass surface as a result of its depletion of other ions. The solubility of zirconium fluoride is suggested to be probably much lower than that of barium fluoride (0.16 g/100 cu cm at 18 C). Dissolution was determined to be the predominant process in the initial stages of the reaction of the glass with water. Penetration of water into the glass has little effect.
Doremus, R. H.↗
Pulse Stripping Analysis: A Technique for Determination of Some Metals in Aerosols and Other Limited Size Samples
A technique for determining lead with a detection limit down to a nanogram on limited size samples is described. The technique is an electrochemical one and involves pre-concentration of the metal species in a mercury drop. Although the emphasis in this paper is on the determination of lead, many metal ion species which are reducible to the metal at an electrode are equally determinable. A technique called pulse polarography is proposed to determine the metals in the drop and this technique is discussed and is compared with other techniques. Other approaches for determination of lead are also compared. Some data are also reported for the lead content of Ventura County particulates. The characterization of lead species by solubility parameters is discussed.
Parry, Edward P.↗
Near-term lander experiments for growing plants on Mars: requirements for information on chemical and physical properties of Mars regolith
In order to support humans for long-duration missions to Mars, bioregenerative Advanced Life Support (ALS) systems have been proposed that would use higher plants as the primary candidates for photosynthesis. Hydroponic technologies have been suggested as the primary method of plant production in ALS systems, but the use of Mars regolith as a plant growth medium may have several advantages over hydroponic systems. The advantages for using Mars regolith include the likely bioavailability of plant-essential ions, mechanical support for plants, and easy access of the material once on the surface. We propose that plant biology experiments must be included in near-term Mars lander missions in order to begin defining the optimum approach for growing plants on Mars. Second, we discuss a range of soil chemistry and soil physics tests that must be conducted prior to, or in concert with, a plant biology experiment in order to properly interpret the results of plant growth studies in Mars regolith. The recommended chemical tests include measurements on soil pH, electrical conductivity and soluble salts, redox potential, bioavailability of essential plant nutrients, and bioavailability of phytotoxic elements. In addition, a future plant growth experiment should include procedures for determining the buffering and leaching requirements of Mars regolith prior to planting. Soil physical tests useful for plant biology studies in Mars regolith include bulk density, particle size distribution, porosity, water retention, and hydraulic conductivity.
NASA Center JSC↗