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At least 199 records · Page 11
All sourcesNASA NTRSDOE OSTI
DOE OSTI2020

Method To Determine MgO and MgOHCl in Chloride Molten Salts

A commercial blend of mainly carnallite (KCl∙MgCl 2 ∙6H 2 O) is considered as a next-generation heat transfer fluid in solar thermal plants. Corrosive properties of MgCl2 hydrates must be addressed at the operating temperatures of 500-720 degrees C. For successful chemical monitoring of the carnallite heat transfer fluid, an experimental method was developed to separate and titrate for MgO and MgOHCl from solid carnallite. This new method was assessed for error and accuracy. The method's relative error for MgOHCl was -7.0% for a mass fraction of 9.0 wt % MgOHCl in the carnallite salt. The method's relative error for MgO was less than +1.0% for a mass fraction of 12.0 wt % MgO in the carnallite salt. Titration results were used to track changes in the MgOHCl concentration in carnallite salt through the carnallite's dehydration and purification.

14 SOLAR ENERGY↗
DOE OSTI2020

Molten Chloride Thermophysical Properties, Chemical Optimization, and Purification

Next-generation concentrating solar power (CSP) technology requires high-temperature heat-transfer fluids and thermal energy storage that can operate in the temperature range of 500°–720°C. This high temperature demands a new chemistry for the heat-transfer fluids that must have high-temperature thermal and chemical stabilities, high energy density, and low corrosion rate on metallic materials used in the heat exchangers, piping, and thermal energy storage tanks. A ternary MgCl 2 -KCl-NaCl chloride-salt system has been proposed to achieve such goals, given its high-temperature thermal stability. The chloride-salt-based systems have been used by the metallurgy industry as the electrolyte to electrolytically extract metallic magnesium. They have also attracted attentions from the nuclear industry for developing the molten salt fast reactors that can operate at close to atmospheric pressure and at higher temperature than traditional light-water reactors. However, the corrosion properties of the ternary salt are not well known. The corrosion mechanism is believed to be correlated to the presence of MgOHCl impurity at the operation temperature. MgOHCl is fundamentally caused by the hygroscopic nature of the MgCl 2 component. Therefore, the first key objective of this project is to understand the nature of the corrosiveness of the ternary chloride-salt system and its prevention by designing new lab-scale purification processes. Because of its importance, a working group called the Chloride Salt Collective across multiple U.S. Department of Energy national laboratories is established to gain experimental agreement on the corrosion behaviors. In addition, water generation during salt dehydration could lead to highly corrosive HCl/water mixture via a hydrolysis process between water and anhydrous MgCl 2 or MgCl 2 hydrates. MgOHCl will eventually be converted to MgO particulates regardless of the chemical path chosen (i.e., by thermal decomposition, chemical purification with an active metal, or electrochemical purification utilizing the reduction power of electron flows). Large MgO particles with high hardness can wear out bearing and bushing and even clog the delicate channels in the primary heat exchanger. Because of this, a second objective is to understand the chemistry behind salt purification and transfer the scientific understanding to a set of engineering know-how for large-scale salt melter design. Because there is limited information on the thermophysical properties and the sensitivity of these properties around the targeted salt composition, a third objective is to measure thermophysical properties relevant to system and component design and support Topic 1 Liquid Pathway development. For example, composition shift due to salt reaction with water can be a potential issue because it can lead to changes of thermophysical properties, such as (1) melting point (or freeze point), which can jeopardize safe operation of the supercritical CO 2 power cycle proposed for next-generation CSP, and (2) heat capacity and density, which can decrease the overall power-generation capability of the plants. The value of the thermal conductivity of the selected salt composition is also a critical criterion for the solar receiver design.

14 SOLAR ENERGY↗
NASA NTRS1999

Renal Stone Risk During Space Flight

Space flight produces a number of metabolic and physiological changes in the crewmembers exposed to microgravity. Following launch, body fluid volumes, electrolyte levels, and bone and muscle undergo changes as the human body adapts to the weightless environment. Changes in the urinary chemical composition may lead to the potentially serious consequences of renal stone formation. Previous data collected immediately after space flight indicate changes in the urine chemistry favoring an increased risk of calcium oxalate and uric acid stone formation (n = 323). During short term Shuttle space flights, the changes observed include increased urinary calcium and decreased urine volume, pH and citrate resulting in a greater risk for calcium oxalate and brushite stone formation (n = 6). Results from long duration Shuttle/Mir missions (n = 9) followed a similar trend and demonstrated decreased fluid intake and urine volume and increased urinary calcium resulting in a urinary environment saturated with the calcium stone-forming salts. The increased risk occurs rapidly upon exposure to microgravity, continues throughout the space flight and following landing. Dietary factors, especially fluid intake, or pharmacologic intervention can significantly influence the urinary chemical composition. Increasing fluid intake to produce a daily urine output of 2 liters/day may allow the excess salts in the urine to remain in solution, crystals formation will not occur and a renal stone will not develop. Results from long duration crewmembers (n = 2) who had urine volumes greater than 2.5 L/day minimized their risk of renal stone formation. Also, comparisons of stone-forming risk in short duration crewmembers clearly identified greater risk in those who produced less than 2 liters of urine/day. However, hydration and increased urine output does not correct the underlying calcium excretion due to bone loss and only treats the symptoms and not the cause of the increased urinary salts. Dietary modification and promising pharmacologic treatments may also be used to reduce the potential risk for renal stone formation. Potassium citrate is being used clinically to increase the urinary inhibitor levels to minimize the development of crystals and the growth of renal stones. Bisphosphonates are a class of drugs recently shown to help in patients with osteoporosis by inhibiting the loss of bones in elderly patients. This drug could potentially prevent the bone loss observed in astronauts and thereby minimize the increase in urinary calcium and reduce the risk for renal stone development. Results of NASA's renal stone risk assessment program clearly indicate that exposure to microgravity changes the urinary chemical environment such that there is an increased risk for supersaturation of stone-forming salts, including calcium oxalaie and brushite. These studies have indicated specific avenues for development of countermeasures for the increased renal stone risk observed during and following space flight. Increased hydration and implementation of pharmacologic countermeasures should largely mitigate the in-flight risk of renal stones.

Whitson, Peggy A.↗
DOE OSTI2023

Cation–polymer interactions and local heterogeneity determine the relative order of alkali cation diffusion coefficients in PEGDA hydrogels

Current research efforts are focused on endowing polymer membranes with ion–ion selectivity by incorporating ion–polymer interactions into materials to bias the selective partitioning and or diffusivity of one species over another. However, little is known about the impact of such interactions on the mechanisms of ion transport. In this study, we probe the influence of cation–polymer interactions on cation, anion, and salt diffusivity in a model membrane material, poly(ethylene glycol) diacrylate (PEGDA) by modeling concentrated polyethylene oxide solutions via molecular dynamics simulations. These results are compared to published experimental data for LiCl, NaCl, and KCl diffusion in PEGDA. Experimentally, the order of salt and cation diffusion coefficients for LiCl, NaCl, and KCl deviate from the order in aqueous solutions. Here, simulations identify these deviations to arise from cation–polymer coordination in the membrane. Both the fraction of bound cations and the average binding lifetime increases with decreasing cation hydration free energy (moving down the alkali series), leading to different diffusivity trends in the membrane compared to solution. However, to recover the experimentally observed order of diffusivities cations and salt in our simulations, we needed to incorporate membrane heterogeneity explicitly via a polymer charge scaling procedure. Together, our results indicate that cation–polymer interactions, as well as spatial heterogeneity within the membrane, play a critical role in dictating the observed order of alkali cation and salt diffusion coefficients in membranes.

36 MATERIALS SCIENCE↗
NASA NTRS2011

Polymer Electrolyte-Based Ambient Temperature Oxygen Microsensors for Environmental Monitoring

An ambient temperature oxygen microsensor, based on a Nafion polymer electrolyte, has been developed and was microfabricated using thin-film technologies. A challenge in the operation of Nafion-based sensor systems is that the conductivity of Nafion film depends on the humidity in the film. Nafion film loses conductivity when the moisture content in the film is too low, which can affect sensor operation. The advancement here is the identification of a method to retain the operation of the Nafion films in lower humidity environments. Certain salts can hold water molecules in the Nafion film structure at room temperature. By mixing salts with the Nafion solution, water molecules can be homogeneously distributed in the Nafion film increasing the film s hydration to prevent Nafion film from being dried out in low-humidity environment. The presence of organics provides extra sites in the Nafion film to promote proton (H+) mobility and thus improving Nafion film conductivity and sensor performance. The fabrication of ambient temperature oxygen microsensors includes depositing basic electrodes using noble metals, and metal oxides layer on one of the electrode as a reference electrode. The use of noble metals for electrodes is due to their strong catalytic properties for oxygen reduction. A conducting polymer Nafion, doped with water-retaining components and extra sites facilitating proton movement, was used as the electrolyte material, making the design adequate for low humidity environment applications. The Nafion solution was coated on the electrodes and air-dried. The sensor operates at room temperature in potentiometric mode, which measures voltage differences between working and reference electrodes in different gases. Repeat able responses to 21-percent oxygen in nitrogen were achieved using nitrogen as a baseline gas. Detection of oxygen from 7 to 21 percent has also been demonstrated. The room-temperature oxygen micro sensor developed has extremely low power consumption (no heating for operation, no voltage applied to the sensor, only a voltmeter is needed to measure the output), is small in size, is simple to batch-fabricate, and is high in sensor yield. It is applicable in a wide humidity range, with improved operation in low humidity after the additives were added to the Nafion film. Through further improvement and development, the sensor can be used for aerospace applications such as fuel leak detection, fire detection, and environmental monitoring.

Hunter, Gary W.↗
NASA NTRS2017

Impact-Facilitated Hydrothermal Alteration in the Rim of Endeavour Crater, Mars

Endeavour crater, a Noachian-aged, 22 km diameter impact structure on Meridiani Planum, Mars, has been investigated by the Mars Exploration Rover Opportunuity for over 2000 sols (Mars days). The rocks of the western rim region (oldest to youngest) are: (i) the pre-impact Matijevic fm.; (ii) rim-forming Shoemaker fm. polymict impact breccias; (iii) Grasberg fm., fine-grained sediments draping the lower slopes; and (iv) Burns fm., sulfate-rich sandstones that onlap the Grasberg fm. The rim is segmented and transected by radial fracture zones. Evidence for fluid-mediated alteration includes m-scale detections of phyllosilicates from orbit, and cm-scale variations in rock/soil composition/mineralogy documented by the Opportunity instrument suite. The m-scale phyllosilicate detections include Fe(3+)-Mg and aluminous smectites that occur in patches in the Matijevic and Shoemaker fms. Rock compositions do not reveal substantial differences for smectite-bearing compared to smectite-free rocks. Interpretation: large-scale hydrothermal alteration powered by impact-deposited heat acting on limited water supplies engendered mineralogic transfomations under low water/rock, near-isochemical conditions. The cm-scale alterations, localized in fracture zones, occurred at higher water/rock as evidenced by enhanced Si and Al contents through leaching of more soluble elements, and deposition of Mg, Ni and Mn sulphates and halogen salts in soils. Visible/near infrared reflectance of narrow curvilinear red zones indicate higher nanophase ferric oxide contents and possibly hydration compared to surrounding outcrops. Broad fracture zones on the rim have reflectance features consistent with development of ferric oxide minerals. Interpretation: water fluxing through the fractures in a hydrothermal system resulting from the impact engendered alteration and leaching under high water/rock conditions. Late, localized alteration is documented by Ca-sulfate-rich veins that are not confined to fracture zones; some cross-cut the Grasberg fm. Interpretation: late fluid mobilization of soluble elements, likely in a later alteration event.

Mittlefehldt, D. W.↗
DOE OSTI2022

Hydro-mechanical behavior of heated bentonite buffer for geologic disposal of high-level radioactive waste: A bench-scale X-ray computed tomography investigation

The behavior of heated bentonite buffer is critical for the security and long-term performance of a geological repository for high-level radioactive waste (HLW). While laboratory column experiments have been conducted to investigate compacted bentonite and coupled THMC (thermal-hydro-mechanical and chemical) processes for a moderate temperature range of up to 100 °C, data for a higher temperature range are limited. Understanding bentonite behavior and coupled THMC processes under higher temperatures (e.g., up to 200 °C) could allow for a more economic repository design and would expand the data and knowledge base for more reliable modeling. In this study, a bench-scale experiment was conducted in a compacted bentonite column experiencing both heating up to 200 °C in the center and hydration from a sand-clay boundary surrounding the column. During the experiment run for 1.5 years, frequent X-ray computed tomography (CT) scanning of bentonite provided insights into the spatiotemporal evolution of (1) hydration/dehydration, (2) clay swelling/shrinkage, (3) displacement, and (4) mineral precipitation. After the experiment, a comprehensive post-dismantling characterization of bentonite samples was conducted. Results showed that the bentonite hydration was axi-symmetrical despite the initial heterogeneity due to packing, confirming the ability of bentonite to seal fast flow/transport paths. Further, compared to a non-heated control experiment, the heated column showed greater CT density variations along the radial distance, indicating that homogenization of bentonite might be more difficult if a temperature gradient is maintained in the repository. Precipitation of an anhydrite layer occurred in the inner hot zone, pointing to potential concerns about salt precipitation causing canister corrosion. Ultimately, the experiments provided a high-resolution window into the strongly dynamic and coupled behavior of bentonite exposed to heating, hydration and swelling, which will be valuable for improving modeling of coupled processes, especially for the early state of a HLW repository.

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

Hydration size-dependent transport of ions across nanoporous graphene membranes

Nanoporous atomically-thin membranes are promising candidates for metal ion separations due to their chemical stability and high permeance and selectivity, but experimental evidence of the mechanisms responsible for ion-ion selectivity is sparse. Here, in this work, we measured the simultaneous diffusion of a dilute mixture of ten different Group I, Group II, and rare earth cations in a salt background across nanoporous graphene (NPG) membranes with sub-nanometer pores. The membranes exhibited ion-ion selectivity, including between similarly-charged ions. Cation transport was governed primarily by the hydrated ion size that was consistent with continuum models of ion diffusion, with additional influence of the ionic charge. Selectivity enhancement was achieved by modifying ion sizes using an ion-selective complexing agent. Our study provides evidence of the importance of size-sieving and electrostatic mechanisms governing ion transport across NPG, and allows for quantitative prediction of transport rates to guide future development of ion-selective atomically-thin membranes.

36 MATERIALS SCIENCE↗
NASA NTRS1983

Method of forming oxide coatings

This invention is concerned with an improved plating process for covering a substrate with a black metal oxide film. The invention is particularly directed to making a heating panel for a solar collector. A compound is electrodeposited from an aqueous solution containing cobalt metal salts onto a metal substrate. This compound is converted during plating into a black, highly absorbing oxide coating which contains hydrated oxides. This is achieved by the inclusion of an oxidizing agent in the plating bath. The inclusion of an oxidizing agent in the plating bath is contrary to standard electroplating practice. The hydrated oxides are converted to oxides by treatment in a hot bath, such as boiling water. An oxidizing agent may be added to the hot liquid treating bath.

Mcdonald, G. E.↗
NASA NTRS1992

Systematic variations in the spectral properties of bright regions on Mars

The color and albedo of the martian surface define two basic surface units, dark gray material interpreted as relatively unaltered 'rock' and bright reddish material interpreted as weathered 'soil'. Understanding the processes contributing to soil formation first requires assessment of the soil's composition and compositional diversity. We report first results of an investigation of the character and variability of Fe- and water-bearing phases in bright reddish materials using ISM data. We also explore implications of these results for chemical evolution of martian soil. Information on the composition and distribution of bright reddish material comes from three major sources: Viking images, measurements by the XRF and GCMS instruments on the Viking Landers, and spectroscopic data. The XRF experiment found nearly identical, Fe-rich major-element compositions comparable to weathered basalt. Soil water, amounting to approximately 1-3 wt. percent as measured by the GCMS, was liberated mostly by heating to greater than or equal to 350 C, suggesting that it is present in a chemically bound form. Spectroscopic studies have detected ferric oxide, probably hematite, as well as molecular water. However, the identities of major silicate phases have been controversial, with conflicting evidence regarding phyllosilicates. Two main interpretations of this evidence have been proposed: Weathering of basaltic glasses by H2O and CO2 formed a mixture of oxides, salts, and metastable phyllosilicates such as montmorillonite and 'palagonite' formed when basaltic melt contacted ground ice or water. Palagonite is a hydrated basaltic glass containing dispersed ferric oxide, recrystallized in varying degrees to phyllosilicates. Typically it is aphanitic, although some examples contain phenocrysts. In either case, eolian redistribution is thought to have resulted in the material's global homogenization. Imaging spectroscopic data returned by the ISM instrument on Phobos 2 provide a powerful new basis for evaluating the composition and origin of martian soil because they are indicative of the presence and distribution of water- and Fe-bearing phases whose mineralogy is sensitive to the history of chemical weathering.

Murchie, Scott↗
NASA NTRS2009

Liquid Water on Enceladus from Observations of Ammonia and Ar-40 in the Plume

Jets of water ice from surface fractures near the south pole of Saturn's icy moon Enceladus produce a plume of gas and particles. The source of the jets may be a liquid water region under the ice shell-as suggested most recently by the discovery of salts in E-ring particles derived from the plume-or warm ice that is heated, causing dissociation of clathrate hydrates. Here we report that ammonia is present in the plume, along with various organic compounds, deuterium and, very probably, Ar-40. The presence of ammonia provides strong evidence for the existence of at least some liquid water, given that temperatures in excess of 180 K have been measured near the fractures from which the jets emanate. We conclude, from the overall composition of the material, that the plume derives from both a liquid reservoir (or from ice that in recent geological time has been in contact with such a reservoir) as well as from degassing, volatile-charged ice. As part of a general comprehensive review of the midsize saturnian satellites at the conclusion of the prime Cassini mission, PI McKinnon and co-I Barr contributed to three review chapters.

Waite, J. H., Jr.↗
NASA NTRS2004

Lunar and Planetary Science XXXV: Weird Martian Minerals: Complex Mars Surface Processes

The session "Complex Mars Surface" included the following reports:A Reappraisal of Adsorbed Superoxide Ion as the Cause Behind the Reactivity of the Martian Soils; Sub-Surface Deposits of Hydrous Silicates or Hydrated Magnesium Sulfates as Hydrogen Reservoirs near the Martian Equator: Plausible or Not?; Thermal and Evolved Gas Analysis of Smectites: The Search for Water on Mars; Aqueous Alteration Pathways for K, Th, and U on Mars; Temperature Dependence of the Moessbauer Fraction in Mars-Analog Minerals; Acid-Sulfate Vapor Reactions with Basaltic Tephra: An Analog for Martian Surface Processes; Iron Oxide Weathering in Sulfuric Acid: Implications for Mars; P/Fe as an Aquamarker for Mars; Stable Isotope Composition of Carbonates Formed in Low-Temperature Terrestrial Environments as Martian Analogs; Can the Phosphate Sorption and Occlusion Properties Help to Elucidate the Genesis of Specular Hematite on the Mars Surface?; Sulfate Salts, Regolith Interactions, and Water Storage in Equatorial Martian Regolith; Potential Pathways to Maghemite in Mars Soils: The Key Role of Phosphate; and Mineralogy, Abundance, and Hydration State of Sulfates and Chlorides at the Mars Pathfinder Landing Site.

Source record↗
DOE OSTI2025

Expedition UT-GOM2-2 Methods

Methods used during the University of Texas (UT) Deepwater Hydrate Coring Expedition (UT-GOM2-2) include work done onboard the Helix Q4000 in the offshore Gulf of America (Gulf of Mexico), herein “the Gulf”, “dockside” in Salt Lake City, Utah, and some shore-based work in individual laboratories. The goal of this report is two-fold: to provide enough detail on the methods so they can be repeated by others; and to provide a reference document for the team to enhance cross-disciplinary understanding and knowledge. Methods include drilling operations, depth references and depth modification, downhole tool deployment, coring tool performance assessment, core processing, lithostratigraphy, biostratigraphy, as well as physical properties, including core logging and imaging, rock magnetism, dissolved methane concentration, hydrate saturation, microbiology, and geochemistry. An extensive amount of operational work and planning was required before mobilization of the expedition to permit, build mobile labs, and test downhole tools for deepwater drilling.

03 NATURAL GAS↗
DOE OSTI2025

The effect of ion pairing on speciation and transport in ion exchange membranes at varying hydration levels: A four-state model

Understanding ion pairing in ion exchange membranes (IEMs) is essential for advancing IEM applications in energy and environmental technologies. Here, this study introduces a four-state molecular dynamics model to quantify speciation and transport within Nafion-117, specifically examining the role of ion pairing in monovalent and divalent counterions (NaCl, Na 2 SO 4 , and MgSO 4 ). By analyzing radial distribution functions (RDFs) and molecular snapshots, we distinguish ion pairing modes and classify counterions into four states: condensed counterion, condensed ion pair, free ion pair, and free counterion. A key finding is that while divalent counterions (e. g., Mg 2+ ) maintain stable speciation across hydration levels, monovalent counterions (e.g., Na + ) show notable speciation shifts with hydration. Both monovalent and divalent counterions are not diffusive when condensed onto the polymer (sorbed to membrane functional groups). In contrast, free counterions are diffusive across all hydration levels. To evaluate the overall diffusivity of counterions, four-state fractions and diffusivities are computed, each contributing to counterion transport. The condensed/free ion speciation for multivalent sulfate salts aligns with previous revisions to the Donnan-Manning framework that include ion pairing, thereby validating its relevance to established membrane theories. The four-state model's diffusivity results support several current ion exchange assumptions, including that the condensed counterions are immobile, while uncondensed counterions are mobile. The four-state model offers insights into contact ion pairing within IEMs, highlighting its potential even when undetected in aqueous solution experiments. This work advances the theoretical understanding of counterion speciation in IEMs while identifying model limitations that suggest avenues for refinement, such as distinguishing water-mediated ion pairs between fully hydrated ions.

Ion exchange membranes↗
DOE OSTI2022

Using Membranes with Internal Microchannels to Prevent Drying-out during CO 2 Electrolysis

Scaling up CO 2 electrolysis is a vital aspect in the transition to manufacturing sustainable fuels and chemical compounds, satisfying the demand for chemicals and demand for storing renewable electricity. Depending on the employed catalyst, different products can be produced, such as carbon monoxide and ethylene, by applying a voltage on a CO 2 and H 2 O fed electrolyzer. CO is a desirable product according to techno-economic analysis, because it can be produced selectively using a silver catalyst and is a precursor for hydrocarbons in the Fischer–Tropsch process. In a state-of-the-art CO 2 electrolyzer, two electrodes are directly pressed against an ion-exchange membrane – this is called a zero-gap configuration. Therefore, the membrane is a crucial component for the system, since it has the role of providing a conductive medium between the electrodes. One of the challenges in CO 2 electrolysis is that water is consumed in the reaction. At high current density, this may cause the membrane's surface near the cathode to dry out, lowering efficiency or perhaps stopping the process entirely, since there is no longer a conductive medium. As a result, water management is critical for this process. In this work, we approach the drying-out challenge by studying the novel concept of a membrane with internal microchannels. These channels allow the circulation of water or an electrolyte inside the membrane, which reduces the water diffusion path and affects the membrane’s conductivity. The effects of channel geometry, location, and concentrations of electrolyte inside on water content, conductivity and overall performance are studied in a 2D COMSOL model. In addition, the effect of internal concentration of electrolyte on the membrane’s resistance, on the process performance and the K + cross-over to cathode side were investigated experimentally. Our modeling results prove that the presence of the channels can keep the membrane hydrated. The highest current densities are observed when the channel is closest to the cathode, and with smaller pores. Smaller pores are advantageous due to the trade-off between enhanced membrane conductivity and the lower conductivity of the liquid itself. If water is circulated in a large channel, it increases the membrane’s ionomer conductivity due to hydration but the overall conductivity is decreased since water is not highly conductive. Nonetheless, the results also show that a higher concentration of electrolyte inside the microchannels can significantly increase the total conductivity of the membrane, and therefore the energy efficiency of the process. These effects are most significant at higher current densities. In the experimental results, we’ve observed similar effects in terms of membrane conductivity and current density of the process – the higher the electrolyte concentration the higher the current density. Furthermore, a low concentration decreases the amount of potassium which crosses over to the cathode side, inhibiting salt deposition. We’ve concluded that a small channel, up to 90 µm wide, close to the pore with an electrolyte with a concentration of up to 10 mM could be very beneficial for the water management and energy efficiency of the process. This helps to keep the membrane hydrated at higher current densities, improves the conductivity of the membrane, and it doesn’t have significant impacts on the salt deposition.

Petrov, Kostadin Veselinov↗
NASA NTRS1996

Lack of Evidence for Prenucleation Aggregate Formation in Lysozyme Crystal Growth Solutions

There have been numerous claims of large concentrations of prenucleation aggregates in supersaturated as well as undersaturated lysozyme solutions at high salt concentrations. The presence of these aggregates was derived from measurements of the light or neutron scattering intensity, ultracentrifugation and dialysis behavior, as well as over-simplified crystal growth kinetics considerations. In all these interpretations it has been assumed that lysozyme solutions are either ideal or that protein interactions are independent of salt concentration. Contrary to these presumptions, our static and dynamic light scattering experiments provide evidence that lysozyme forms highly non-ideal, strongly interacting solutions. At low salt concentrations, the scattering intensities fall well below the values expected for an ideal, monomeric solution at the same protein concentration, while diffusivities increase with increasing protein concentration. Upon increase in salt concentration, these trends are eventually reversed. This enhancement in scattering intensity and decrease in diffusivity was widely interpreted as sign of aggregate formation. Yet, a quantitative interpretation of the scattering behavior over the whole salt concentration range can only be given in terms of a transition from net repulsion to net attraction between lysozyme monomers. Increased salt screening of the electrostatic repulsion among the protein macro-ions, together with attractive protein interactions, such as van der Waals, hydrophobic and hydration forces, provide an unambiguous mechanism for the observed transition and a more physical interpretation of the various observations.

Muschol, Martin↗
DOE OSTI2021

Effect of seawater as mixing water on the hydration behaviour of tricalcium aluminate

This study explored the mechanism of the effect of seawater on tricalcium aluminate (C{sub 3}A) hydration. The results showed that seawater retarded C{sub 3}A hydration and reduced the reaction degree of C{sub 3}A. The co-existence or ion pairing of Ca{sup 2+} and SO{sub 4}{sup 2−} onto the surface of C{sub 3}A poisoning the reactive sites is the main reason for this retardation. Besides, the precipitation of Mg(OH){sub 2} on the surface of C{sub 3}A would prolong the induction period for another 30 min and then consequently decrease the dissolution rate of C{sub 3}A hydration. Trace amounts of MgSO{sub 4}{sup 0} and Mg{sup 2+} present in the alkaline solution had little retardation effect. It was also found that Cl{sup −} would preferentially react with C{sub 3}A to form Friedel's salt, rather than forming hydroxy-AFm as that in the C{sub 3}A-deionized water paste. The direct formation of Friedel's salt resulted in an accumulation of Al{sup 3+} in solution, which would also hinder the subsequent dissolution of C{sub 3}A.

36 MATERIALS SCIENCE↗