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NASA NTRS1973

New formaldehyde base disinfectants.

Preparations of formaldehyde in various organic liquids - ethylene glycol, glycerol, and propylene glycol - serve as effective disinfectants towards microbial vegetative cells and spores. This disinfection is a temperature-dependent process and is manifest when these formaldehyde base disinfectants are dissolved in water. The irritating vapors associated with formaldehyde disinfection are not present in either of these new formaldehyde base disinfectants or in aqueous solutions of them.

Trujillo, R.↗

NASA NTRS1987

Chemical interactions between the present-day Martian atmosphere and surface minerals

Thermochemical and photochemical reactions between surface minerals and present-day atmospheric constituents are predicted to produce microscopic effects on the surfaces of mineral grains. Relevant reactions hypothesized in the literature include conversions of silicates and volcanic glasses to clay minerals, conversion of ferrous to ferric compounds, and formation of carbonates, nitrates, and sulfates. These types of surface-atmosphere interactions are important for addressing issues such as chemical weathering of minerals, biological potential of the surface environment, and atmospheric stability in both present and past Martian epochs. It is emphasized that the product of these reactions will be observable and interpretable on the microscopic surface layers of Martian surface rocks using modern techniques with obvious implications for sample return from Mars. Macroscopic products of chemical weathering reactions in past Martian epochs are also expected in Martian surface material. These products are expected not only as a result of reactions similar to those proceeding today but also due to aqueous reactions in past epochs in which liquid water was putatively present. It may prove very difficult or impossible however to determine definitively from the relic macroscopic product alone either the exact weathering process which led to its formation or the identity of its weathered parent mineral. The enormous advantages of studying Martian chemical weathering by investigating the microscopic products of present-day chemical reactions on sample surfaces are very apparent.

Prinn, Ronald↗

NASA NTRS1988

Chemical interactions between the present-day Martian atmosphere and surface minerals: Implications for sample return

Thermochemical and photochemical reactions between surface minerals and present-day atmospheric constituents are predicted to produce microscopic effects on the surface of mineral grains. Relevant reactions hypothesized in the literature include conversions of silicates and volcanic glasses to clay minerals, conversion of ferrous to ferric compounds, and formation of carbonates, nitrates, and sulfates. These types of surface-atmosphere weathering of minerals, biological potential of the surface environment, and atmospheric stability in both present and past Martian epochs. It is emphasized that the product of these reactions will be observable and interpretable on the microscopic surface layers of Martian surface rocks using modern techniques with obvious implications for sample return from Mars. Macroscopic products of chemical weathering reactions in past Martian epochs are also expected in Martian surface materials. These products are expected not only as a result of reactions similar to those proceeding today but also due to aqueous reactions in past epochs in which liquid water was putatively present. It may prove very difficult or impossible, however, to determine definitively from the relic macroscopic product alone either the exact weathering process which led to its formation of the identity of its weathering parent mineral. The enormous advantages of studying the Martian chemical weathering by investigating the microscopic products of present-day chemical reactions on sample surfaces are very apparent.

Prinn, Ronald↗

NASA NTRS2000

Magnetic Susceptibility Effects and Lorentz Damping in Diamagnetic Fluids

A great number of crystals (semi-conductor and protein) grown in space are plagued by convective motions which contribute to structural flaws. The character of these instabilities is not well understood but is associated with density variations in the presence of residual gravity and g-jitter. Both static and dynamic (rotating or travelling wave) magnetic fields can be used to reduce the effects of convection in materials processing. In semi-conductor melts, due to their relatively high electrical conductivity, the induced Lorentz force can be effectively used to curtail convective effects. In melts/solutions with reduced electrical conductivity, such as aqueous solutions used in solution crystal growth, protein crystal growth and/or model fluid experiments for simulating melt growth, however, the variation of the magnetic susceptibility with temperature and/or concentration can be utilized to better damp fluid convection than the Lorentz force method. This paper presents a comprehensive, comparative numerical study of the relative damping effects using static magnetic fields and gradients in a simple geometry subjected to a thermal gradient. The governing equations are formulated in general terms and then simplified for the numerical calculations. Operational regimes, based on the best damping technique for different melts/solutions are identified based on fluid properties. Comparisons are provided between the numerical results and available results from experiments in surveyed literature.

Ramachandran, Narayanan↗

DOE OSTI2024

The Role of Radiation-Induced Non-Equilibrium Plutonium Oxidation States in Solution

Plutonium plays a key role in global actinide research and nuclear fuel cycle technologies, and yet, our fundamental understanding of its inherent radiation-induced chemical behavior is limited. These radiation-induced processes cannot simply be switched off, as they are as fundamentally inherent to plutonium as the impact of relativistic effects on its f-electrons. In less chemically complex actinide systems, such as aqueous solutions of neptunium and americium, both steady-state and transient radiolysis products play a significant role in the redox cycling of their oxidation states, which ultimately impacts their chemistry and transport. However, plutonium's multiple, coexisting, and chemically active oxidation states, which comprise of bare ions and dioxo cations, provide additional redox pathways that complicate the aforementioned radiation-induced competition kinetics. Mechanistically understanding the response of these multiple oxidation states, both equilibrium and non-equilibrium, to intense ionizing radiation fields is essential for predicting the behavior of plutonium under a host of conditions that support technological innovation in global nuclear energy and non-proliferation efforts. Here, advances in radiation-induced plutonium solution chemistry will be presented, including new results from time-resolved electron pulse and steady-state gamma and alpha irradiations.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

NASA NTRS2017

PHYS: Division of Physical Chemistry 258 - Properties and Origins of Cometary and Asteroidal Organic Matter Delivered to the Early Earth

Comets and asteroids may have contributed much of the Earth's water and organic matter. The Earth accretes approximately 4x10(exp 7) Kg of dust and meteorites from these sources every year. The least altered meteorites contain complex assemblages of organic compounds and abundant hydrated minerals. These carbonaceous chondrite meteorites probably derive from asteroids that underwent hydrothermal processing within the first few million years after their accretion. Meteorite organics show isotopic and chemical signatures of low-T ion-molecule and grain-surface chemistry and photolysis of icy grains that occurred in cold molecular clouds and the outer protoplanetary disk. These signatures have been overprinted by aqueously mediated chemistry in asteroid parent bodies, forming amino acids and other prebiotic molecules. Comets are much richer in organic matter but it is less well characterized. Comet dust collected in the stratosphere shows larger H and N isotopic anomalies than most meteorites, suggesting better preservation of primordial organics. Rosetta studies of comet 67P coma dust find complex organic matter that may be related to the macromolecular material that dominates the organic inventory of primitive meteorites. The exogenous organic material accreting on Earth throughout its history is made up of thousands of molecular species formed in diverse processes ranging from circumstellar outflows to chemistry at near absolute zero in dark cloud cores and the formative environment within minor planets. NASA and JAXA are currently flying sample return missions to primitive, potentially organic-rich asteroids. The OSIRIS-REx and Hayabusa2 missions will map their target asteroids, Bennu and Ryugu, in detail and return regolith samples to Earth. Laboratory analyses of these pristine asteroid samples will provide unprecedented views of asteroidal organic matter relatively free of terrestrial contamination within well determined geological context. Studies of extraterrestrial materials and returned samples are essential to understand the origins of Solar System organic material and the roles of comets and asteroids to providing the starting materials for the emergence of life.

Messenger, Scott↗

DOE OSTI2024

Design of a high-temperature cell for cobalt-60 irradiations of aqueous solutions with in situ UV–visible spectroscopy

To understand the speciation of solutes in aqueous solutions in high temperature radiation environments, we report the design and fabrication of a custom-built, high temperature (≤300 °C) titanium irradiation cell with in situ optical spectroscopy capabilities, as afforded by coupled fiber optic cables. The wetted surfaces of the 8-inch tall cylindrical cell with 3.5 in. diameter are entirely made of titanium, sapphire, and gold, which are chemically and radiolytically inert. The initial benchmarking results are reported, including the baseline spectrum of deionized water as a function of temperature, the stability of a spectrum over 4 h at 100 °C, and an irradiated Fricke dosimetry solution under ambient irradiator temperature conditions (27.0 ± 0.5 °C). Further, the average gamma radiation dose rate in the cell in its current configuration is 26.1 ± 1.3 Gy min -1 . This cell has application in studying several processes throughout the nuclear fuel cycle, including the reactor coolant behavior.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

DOE OSTI2025

Scattering insights into shear-induced scission of rod-like micelles

Understanding the scission of rod-like micelles under mechanical forces is crucial for optimizing their stability and behavior in industrial applications. This study investigates how micelle length, flexibility, and external forces interact, offering insights into the design of micellar systems in processes influenced by mechanical stress. Although significant, direct experimental observations of flow-induced micellar scission using scattering techniques remain scarce. Small angle neutron scattering (SANS) is used to explore the shear response of aqueous cetyltrimethylammonium bromide (CTAB) solutions with sodium nitrate. Rheological tests show shear thinning with no shear banding, ensuring a uniform flow field for reliable interpretation of scattering data. As shear rate increases, the scattering spectra show angular distortion, which is analyzed using spherical harmonic decomposition to characterize flow-induced scission and micelle orientation under shear. Two analysis steps are used: a model-independent spectral eigendecomposition reveals a decrease in micellar length, while regression analysis quantifies the evolution of the length distribution and mean length with shear rate. Additionally, micelle alignment increases with shear, quantified by the orientational distribution function. In conclusion, these findings provide experimental evidence for flow-induced alignment and scission, offering a new framework for understanding shear-induced phenomena in micellar systems.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2023

Lead leaching and electrowinning in acetic acid for solar module recycling

It is imperative to recover lead (Pb) contained in end-of-life solar modules. In this paper, a two-step leaching and electrowinning process using acetic acid is investigated for Pb recovery. Acetic acid with hydrogen peroxide can dissolve Pb quickly and, under some conditions, in a matter of minutes. Pb electrowinning has been successfully demonstrated from aqueous solutions of 0.009 M lead(II) acetate with 0–10% v/v acetic acid. Pb-containing deposits are found on both the copper cathode and graphite anode. X-ray diffraction, energy-dispersive X-ray spectroscopy, and Fourier transform infrared spectroscopy confirm the presence of metallic Pb and Pb(II) oxide (PbO) co-deposits on the cathode. Further, there is also the formation of lead subacetate on the cathode under certain conditions. On the anode, the deposit consists of lead(IV) oxide and superoxide (PbO 2 and Pb 1–x O 2 ). A Pb recovery rate of 99% is achieved in 0.009 M lead(II) acetate solutions with 10% v/v acetic acid by applying a reduction potential of either –0.8 V or –1.0 V versus the silver/silver chloride reference electrode for 24h. Pb leaching with acetic acid is also demonstrated from milled silicon solar modules.

14 SOLAR ENERGY↗

DOE OSTI2021

Dynamics of Liquid–Liquid Phase Separation in Submicrometer Aerosol

Nanoscale materials, when compared to their bulk components, possess unique properties. In particular, shifts in phase transitions can occur for submicron particles. For instance, small particles do not undergo the process of liquid-liquid phase separation (LLPS). LLPS has applications in emulsions such as Janus particles, controllable morphology to create drug-rich phases during drug delivery, and is often observed in atmospheric aqueous aerosol particles. In atmospheric particles, LLPS is tracked as a function of particle water activity, which is equivalent to the relative humidity (RH) at equilibrium. We probed three organic/inorganic aerosol systems in the range of RH over which phase separation occurs (SRH). Our findings indicate that SRH for submicron aerosol particles is lower than for micron-sized droplets. These findings show that it may be necessary to update the representation of phase transitions in aerosol particles in climate models. The vast majority of organic/inorganic aerosol particles have submicron diameters, and a decrease in SRH for submicron particles indicates that the current estimation of phase separated aerosols may be overestimated. Furthermore, understanding the properties of LLPS at the nanoscale can provide key parameters to describe these systems and may lead to better control of phase separation in submicron particles.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2020

An extended trajectory-mechanics approach for calculating two-phase flow paths

A technique originating in quantum dynamics is used to derive a trajectory-based, semi-analytical solution for two-phase flow. The partial differential equation governing the evolution of the aqueous phase is equivalent to a family of ordinary differential equations defined along a path through the porous medium. The trajectories may be found by solving the differential equations directly or by post-processing the output of a numerical solution to the full set of governing equations. The trajectories, which differ from conventional streamlines, are found to bend downward in response to gravitational forces. The curvature is more pronounced as the dip of the porous layer containing the flow increases. Subtle changes in the relative permeability curve can lead to significant variations in the trajectories. The ordinary differential equation for the trajectory provides an expression for the travel time along the path. The expression produces a semi-analytical approximation to the model parameter sensitivities, the partial derivatives of the travel times with respect to changes in the permeability model. The semi-analytical trajectory-based sensitivities generally agree with those computed using a numerical reservoir simulator and a perturbation approach. The sensitivities are useful in tomographic imaging algorithms designed to estimate the spatial variation in permeability within a porous medium using multiphase observations.

58 GEOSCIENCES↗

DOE OSTI2026

SULI Report - Development of a Molten Salt Circulation Loop for in-situ Spectroscopy

This project supports the development of real time optical monitoring capabilities for molten salt reactor (MSR) environments by designing, testing, and refining a molten salt circulation loop suitable for combined laser induced breakdown spectroscopy (LIBS) and ultraviolet visible (UV Vis) absorption measurements. Online spectroscopic monitoring is increasingly important for nuclear safeguards, corrosion tracking, and material accountancy, yet MSR process fluids present substantial challenges due to their chemical complexity and hazards such as high temperatures and radiation. To address these needs, this work focuses on Phase I, the development of a room temperature aqueous circulation loop that serves as a surrogate platform for evaluating flow behavior, optical access, and component performance prior to high temperature salt operation. Initial testing identified several practical issues—including leaks, obstructions, and two-phase flow through the absorption cell—that were systematically resolved through hardware replacement, flow path redesign, and venturi pressure optimization. Relocating the flow cell upstream of the primary venturi enabled periods of stable single-phase flow, demonstrating the feasibility of integrating optical diagnostics into a circulation system. The results of Phase I provide essential design insight for Phase II, which will incorporate furnace compatible materials and LiCl KCl eutectic salt. Completion of the molten salt system will deliver a reusable testbed for evaluating multimodal spectroscopic techniques, advancing nondestructive, real time monitoring tools for future MSR and nuclear fuel cycle applications.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

NASA NTRS1978

Hydrogen from the solar photolysis of water

Developments related to the study of photosynthesis are examined and aspects of photosensitization by solids are considered. It is pointed out that solids photosensitization for solar photochemical fuel formation is now an extremely active research area as a consequence of the promising results obtained with semiconductor photoelectrodes. The investigation of water decomposition schemes involving heterogeneous reactions is likely to be a productive area. As is the case for photosynthesis, the known examples of water decomposition by solids photosensitization involve charge separation processes immediately following light absorption. Homogeneous photoredox reactions are also discussed, taking into account thermochemical and photochemical cycles leading to the formation of a photooxidized ion, hydrogen quantum yields in the photo-oxidation aqueous ions, and thermochemical and photochemical cycles leading to the formation of a photoreduced ion.

Ryason, P. R.↗

NASA NTRS1999

Lipid synthesis under hydrothermal conditions by Fischer-Tropsch-type reactions

Ever since their discovery in the late 1970's, mid-ocean-ridge hydrothermal systems have received a great deal of attention as a possible site for the origin of life on Earth (and environments analogous to mid-ocean-ridge hydrothermal systems are postulated to have been sites where life could have originated or Mars and elsewhere as well). Because no modern-day terrestrial hydrothermal systems are free from the influence of organic compounds derived from biologic processes, laboratory experiments provide the best opportunity for confirmation of the potential for organic synthesis in hydrothermal systems. Here we report on the formation of lipid compounds during Fischer-Tropsch-type synthesis from aqueous solutions of formic acid or oxalic acid. Optimum synthesis occurs in stainless steel vessels by heating at 175 degrees C for 2-3 days and produces lipid compounds ranging from C2 to > C35 which consist of n-alkanols, n-alkanoic acids, n-alkenes, n-alkanes and alkanones. The precursor carbon sources used are either formic acid or oxalic acid, which disproportionate to H2, CO2 and probably CO. Both carbon sources yield the same lipid classes with essentially the same ranges of compounds. The synthesis reactions were confirmed by using 13C labeled precursor acids.

Non-NASA Center↗

NASA NTRS2014

Coordinated Mineralogical and Isotopic Analysis of a Cosmic Symplectite Identified in a Stardust Terminal Particle

Comet Wild-2 samples returned by the Stardust spacecraft contain a chemically diverse mixture of material, underscoring the complex nature of comets. Studies of entire Stardust aerogel tracks afford the opportunity to examine the fine-grained particle fragments distributed along the length of the track as well as the terminal particles. Previous TEM characterization of a terminal particle (TP) in track #147 revealed a symplectically intergrown iron sulfide and oxide assemblage. Mineralogically similar assemblages, known as cosmic symplectites (COS, formerly termed "new-PCP"), have only been identified in the primitive carbonaceous chondrite Acfer 094. Meteoritic COS have isotopically heavy O compositions (delta (sup 17), O-18 = 180per mille) that point to interactions with early solar system primordial water. In this study we report mineralogical and O isotopic measurements of the Wild-2 COS assemblage. Experimental: Track #147 is a "bulbous"-type track (4600 microns long) containing 7 terminal particles. The TPs were removed from the track, embedded in epoxy, and ultramicrotomed. A JEOL 2500SE 200 keV field-emission scanning-transmission electron microscope was used to obtain quantitative elemental maps and detailed mineralogical characterization. Following TEM analysis, two thin sections of TP4 (12 microns) were analyzed for O isotopes by raster ion imaging with the JSC NanoSIMS 50L. All three O isotopes were measured simultaneously using electron multipliers. San Carlos olivine grains were used as isotopic standards. Results and Discussion: The COS in the Wild-2 track #147 TP4 sample consists of symplectically intergrown pentlandite and nanocrystalline maghemite which coexists with high-Ca pyroxene with Na and Cr (kosmochlor component). This kosmochlor component could have a nebular origin and be precursors to type II chondrules in ordinary chondrites. Yet pentlandite is not a stable phase in the nebula. The COS in Acfer 094 also consists of pentlandite, but contains magnetite [4] rather than the more oxidized maghemite observed in the Wild-2 COS. The Acfer 094 COS display heavy O isotopic compositions that are the result of sulfidization and oxidation of Fe, Ni-metal grains and sulfides by O-17- and O-18-rich water in the solar nebula or possibly on the parent body. The O isotopic composition of the Wild-2 COS, however, is indistinguishable from terrestrial, indicating it was not altered by the same primordial aqueous reservoir as the Acfer 094 COS. The alteration could have occurred on the parent body by isotopically equilibrated ice. The mineralogy and petrography of Wild-2 samples suggests an incomplete or nascent hydration process. In future work we will analyze S isotopes in the track #147 TP4 COS and search for additional COS in Stardust samples.

Nguyen, A. N.↗

DOE OSTI2025

Electrodepositing Textured Sn Film as a Highly Reversible Anode for Aqueous Batteries

Electrodepositing metal materials in large capacity, at low potential, and with high reversibility serves as the foundation for any aqueous rechargeable battery chemistry to realize the promises of high energy, low cost, and high safety. However, such a foundation is not solid because of the natural tendency of metals to form irregular, nonplanar, and often dendritic morphologies during electrochemical crystallization, which is further amplified in an acidic environment due to the faster kinetics of the coupled proton and mass-transport processes between hydrated metal ions and free metal atoms. As a typical representative, tin metal (Sn 0 ) has potential to achieve high energy in acidic batteries, but its nonuniform large-particle morphology, obtained from traditional electrodeposition, leads to dead Sn 0 formation and deteriorating reversibility, accompanied by the sustained hydrogen evolution reaction (HER) and active Sn 0 loss. Here, in this study, we report quaternary onium salts as effective interfacial cocations that, via selective adsorption, steadily texturize Sn 0 deposition along the (211) plane, which is intrinsically inert to the HER, thus regulating the film deposition process by favoring the formation of planar Sn 0 film. Such Sn 0 film brings exceptional reversibility in acidic electrolytes, which translates into sustained cycling stability at applicable areal capacities in both anode-half cells (similar to 1500 deposition/dissolution cycles at 5 mAh cm -2 ) and full cells (350 charge/discharge cycles at 5 mAh cm -2 ). Textured electrodeposition with intrinsic HER-suppression capability provides a universal solution for diverse metal anode materials in rechargeable energy-dense aqueous batteries.

Sn metal↗

DOE OSTI2023

Reconfigurable Magnetic Liquid Building Blocks for Constructing Artificial Spinal Column Tissues

All-liquid molding can be used to transform a liquid into free-form solid constructs, while maintaining internal fluidity. Traditional biological scaffolds, such as cured pre-gels, are normally processed in solid state, sacrificing flowability and permeability. However, it is essential to maintain the fluidity of the scaffold to truly mimic the complexity and heterogeneity of natural human tissues. Here, this work molds an aqueous biomaterial ink into liquid building blocks with rigid shapes while preserving internal fluidity. The molded ink blocks for bone-like vertebrae and cartilaginous-intervertebral-disc shapes, are magnetically manipulated to assemble into hierarchical structures as a scaffold for subsequent spinal column tissue growth. It is also possible to join separate ink blocks by interfacial coalescence, different from bridging solid blocks by interfacial fixation. Generally, aqueous biomaterial inks are molded into shapes with high fidelity by the interfacial jamming of alginate surfactants. The molded liquid blocks can be reconfigured using induced magnetic dipoles, that dictated the magnetic assembly behavior of liquid blocks. The implanted spinal column tissue exhibits a biocompatibility based on in vitro seeding and in vivo cultivating results, showing potential physiological function such as bending of the spinal column.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Extended thermodynamic model for high salinity produced waters

To support the development of desalination processes for high salinity produced waters, we developed a comprehensive thermodynamic model that reliably predicts the thermodynamic properties and phase behavior of produced water. Here this study extends a previously developed thermodynamic model for the aqueous hexary oceanic salt system by incorporating the Sr 2+ and Ba 2+ ions. Based on the electrolyte nonrandom two-liquid theory, the model requires two adjustable binary interaction parameters for each water-electrolyte and electrolyte-electrolyte pair that has a common ion. The binary interaction parameters for the electrolyte-electrolyte pairs involving Sr 2+ and Ba 2+ ions were identified using thermodynamic and salt solubility data. The model was validated for temperatures from 273.15 K to 473.15 K and electrolyte concentrations from infinite dilution to salt saturation. Extension of the model to include HCO 3 − , CO 3 2− , and CO 2 is currently in progress.

42 ENGINEERING↗