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At least 199 records · Page 11

Ab Initio Molecular Dynamics Insights into Stress Corrosion Cracking and Dissolution of Metal Oxides

Oxide phases such as α-Fe2O3 (hematite) and α-Al2O3 (corundum) are highly insoluble in water; however, subcritical crack growth has been observed in humidity nonetheless. Chemically induced bond breaking at the crack tip appears unlikely due to sterically hindered molecular transport. The molecular mechanics of a crack in corundum with a reactive force field reveal minimal lattice trapping, leading to bond breaking before sufficient space opens for water transport. To address this, we model a pre-built blunt crack with space for H2O molecule adsorption at the tip and show that it reduces fracture toughness by lowering the critical J-integral. Then, we explore stress-enhanced dissolution to understand the mechanism of crack tip blunting in the oxide/water system. Density functional theory combined with metadynamics was employed to describe atomic dissolution from flat hematite and corundum surfaces in pure water. Strain accelerates dissolution, stabilizing intermediate states with broken bonds before full atom detachment, while the free energy profile of unstrained surfaces is almost monotonic. The atomistic calculations provided input for a kinetic model, predicting the shape evolution of a blunt crack tip, which displays three distinct regimes: (i) dissolution primarily away from the tip, (ii) enhanced blunting near but not at the apex, and (iii) sharpening near the apex. The transition between regimes occurs at a low strain, highlighting the critical role of water in the subcritical crack growth of oxide scales, with dissolution as the fundamental microscopic mechanism behind this process.

Chemistry↗

Development of a Nuclear Fuel Dissolution Monitor Based on Raman Spectroscopy

The processing of spent nuclear fuel and other nuclear materials is a critical component of nuclear material management with implications for global security. The first step of fuel processing is dissolution, with several charges of fuel sequentially added to a batch of solvent. The incomplete dissolution of a charge precludes the addition of the next charge. As the dissolution takes place in a heated, highly corrosive and radiological vessel, direct monitoring of the process is not possible. We discuss the use of Raman spectroscopy to indirectly monitor dissolution through an analysis of the gaseous emissions from the dissolver. Challenges associated with the implementation of Raman spectroscopy include the composition and physical characteristics of the offgas stream and the impact of operating conditions. Nonetheless, we observed that NO2 concentrations serve as a reliable indicator of process activity and correlate to the amount of fuel material that remains undissolved. These results demonstrate the promise of the method for monitoring nuclear material dissolution.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Mineral Dissolution upon Alkaline Treatment and Variable Redox Conditions

Over 200.000 kg of uranium released to vadose zone from historic leaks and improper disposal of wastes from plutonium production. U highly mobile due to presence of carbonates and oxidizing conditions with partition coefficients k{sub d} of 0.11-8 mL/g at pH 8. Ammonia (NH{sub 3}) gas injection investigated as an in situ remediation technique that will not introduce additional liquid to the subsurface. Objectives: Understand the impact of remediation with base injection on geochemical process in Hanford site vadose zone. Understand effects of different base treatments on mineral dissolution. Results: - incongruent dissolution based on mineral stoichiometry: if ratio = 1 congruent dissolution occurs, if ratio <1.0 greater leaching of Si and Al and incongruent dissolution occurs. Conclusions: incongruent dissolution occurred for both alkaline treatments and redox conditions across all minerals. By 1440 hr. all normalised Al:Si ratios were <1 representing less [Al]{sub aq} and suggesting formation of secondary Al precipitates as a function of time. [Si]{sub aq} increased and [Al]{sub aq} decreased with increasing contact time with both alkaline treatments. NaOH dissolved slightly more than NH{sub 4}OH especially for [Al]{sub aq} in all investigated minerals. No clear trend for muscovite and montmorillonite for redox conditions but slightly greater Si dissolved under anaerobic conditions for illite. Ammonia gas injection increases the pH and dissolves aluminosilicate minerals in the vadose zone. U is likely to coprecipitate with secondary minerals forming at elevated pH and as the system reequilibrates at natural neutral pH. Further, U solids may be coated with low solubility, secondary precipitates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Dissolution and Separation of Aluminum and Aluminosilicates

The selection of an aluminum alloy for target irradiation affects post-irradiation target dissolution and separations. Recent tests with aluminum alloy 6061 yielded greater than expected precipitation in the dissolver, forming up to 10 wt.% solids of aluminum hydroxides and aluminosilicates. Aluminosilicate dissolution presents challenges in a number of different areas, metals extraction from minerals, flyash treatment, and separations from aluminum alloys. We present experimental work that attempts to maximize dissolution of aluminum metal, along with silicon, magnesium, and copper impurities, through control of temperature, the rate of reagent addition, and incubation time. Aluminum phase transformations have been identified as a function of time and temperature, using X-ray diffraction. Solutions have been analyzed using wet chemical methods and X-ray fluorescence. Our data have been compared with published calculations of aluminum phase diagrams. Approaches are given to enhance the dissolution of aluminum and aluminosilicate phases in caustic solution.

36 MATERIALS SCIENCE↗

In Situ Observation of Calcium Aluminate Inclusions Dissolution into Steelmaking Slag

The dissolution rate of calcium aluminate inclusions in CaO-SiO{sub 2}-Al{sub 2}O{sub 3} slags has been studied using confocal scanning laser microscopy (CSLM) at elevated temperatures: 1773 K, 1823 K, and 1873 K (1500 °C, 1550 °C, and 1600 °C). The inclusion particles used in this experimental work were produced in our laboratory and their production technique is explained in detail. Even though the particles had irregular shapes, there was no rotation observed. Further, the total dissolution time decreased with increasing temperature and decreasing SiO{sub 2} content in the slag. The rate limiting steps are discussed in terms of shrinking core models and diffusion into a stagnant fluid model. It is shown that the rate limiting step for dissolution is mass transfer in the slag at 1823 K and 1873 K (1550 °C and 1600 °C). Further investigations are required to determine the dissolution mechanism at 1773 K (1500 °C). The calculated diffusion coefficients were inversely proportional to the slag viscosity and the obtained values for the systems studied ranged between 5.64 × 10{sup −12} and 5.8 × 10{sup −10} m{sup 2}/s.

36 MATERIALS SCIENCE↗

Dissolution Behavior of Iron and Steel Materials in Liquid Magnesium

The dissolution of metallic elements from Fe and steel materials into pure liquid Mg was investigated with the aim of improving control of impurities in Mg during processes such as Mg-alloy production and Ti smelting. Pure Mg was melted between 1073 and 1323 K (800 and 1050 °C) for 24 to 96 hours in closed crucibles made of pure Fe, low-carbon steel, or austenitic stainless steel SUS316. From the experiments using the pure Fe crucible, the relationship between the solubility of Fe in liquid Mg [C{sub sol,Fe} (mass pct)] and temperature [T (K)] was determined to be log(C{sub sol,Fe}) = − 3.67 × 10{sup 3}/T + 2.48 (± 0.06), from which the standard Gibbs energy of Fe dissolution in liquid Mg was evaluated. The amount of Fe dissolved from low-carbon steel was the same as that from pure Fe. From SUS316, not only Fe but also Cr and Ni dissolved into liquid Mg; the Fe and Cr concentrations in liquid Mg did not change significantly over time, whereas the Ni concentration increased monotonically. Preferential Ni dissolution resulted in a Ni-poor layer on the SUS316 surface. Finally, using the experimental data of Fe dissolution from low-carbon steel, the Fe contamination route in the current Ti smelting process, where a large amount of Mg is used as a reducing agent, is discussed.

36 MATERIALS SCIENCE↗

Kinetics and Mechanisms of Dolime Dissolution in Steelmaking Slag

The kinetics of dolime dissolution containing 20 and 50 pct of magnesium oxide in steelmaking slags has been studied in a high-temperature experiment. The dissolution tests were carried out under static conditions at temperatures of between 1573 K and 1873 K (1300 °C to 1600 °C). Cylindrical samples of dolime were introduced into pre-melted slag at predetermined time intervals. The changes in mass and geometrical parameters of the samples, as well as CaO and MgO concentrations in the melt, were determined to calculate mass transfer and diffusion coefficients. The results revealed that the rate-limiting step in the process of dolime dissolution is diffusion. The increase in MgO content in the initial sample caused a drop in dolime dissolution rate and diffusion coefficients. The prediction of MgO solubility in steel slag, as well as the effect of slag basicity, was carried out using the thermodynamic software FactSage 7.1. In addition, the activation energy of diffusion has been calculated using the dependence of the logarithm of diffusion coefficients on the inverse temperature.

36 MATERIALS SCIENCE↗

Calcium nitrate: A chemical admixture to inhibit aggregate dissolution and mitigate expansion caused by alkali-silica reaction

Alkali-silica reaction (ASR) is a significant cause of the degradation of concrete structures. ASR results from the dissolution of reactive silicate aggregates and the subsequent formation of damaging, expansive ASR gels. Despite the prevalence of ASR, so far only lithium-based chemical admixtures have been shown to be successful in mitigating its deleterious effects. Herein, dissolved calcium nitrate (Ca(NO 3 ) 2 : CN) is demonstrated to reduce ASR-induced expansion caused by the use of sodium borosilicate (NBS) glass as a model reactive aggregate. The significance of reductions of NBS-glass dissolution and mortar-bar expansion rates is discussed, with special focus on highlighting the mechanism by which calcium nitrate mitigates ASR, i.e., by the inhibition of aggregate dissolution. This study reveals a new and cost-effective pathway to suppress aggregate dissolution and ASR in concrete based on the dosage of soluble alkaline-earth additives.

36 MATERIALS SCIENCE↗

Structural changes in C–S–H gel during dissolution: Small-angle neutron scattering and Si-NMR characterization

Flow-through experiments were conducted to study the calcium–silicate–hydrate (C–S–H) gel dissolution kinetics. During C–S–H gel dissolution the initial aqueous Ca/Si ratio decreases to reach the stoichiometric value of the Ca/Si ratio of a tobermorite-like phase (Ca/Si = 0.83). As the Ca/Si ratio decreases, the solid C–S–H dissolution rate increases from (4.5 × 10{sup −} {sup 14} to 6.7 × 10{sup −} {sup 12}) mol m{sup −} {sup 2} s{sup −} {sup 1}. The changes in the microstructure of the dissolving C–S–H gel were characterized by small-angle neutron scattering (SANS) and {sup 29}Si magic-angle-spinning nuclear magnetic resonance ({sup 29}Si-MAS NMR). The SANS data were fitted using a fractal model. The SANS specific surface area tends to increase with time and the obtained fit parameters reflect the changes in the nanostructure of the dissolving solid C–S–H within the gel. The {sup 29}Si MAS NMR analyses show that with dissolution the solid C–S–H structure tends to a more ordered tobermorite structure, in agreement with the Ca/Si ratio evolution.

36 MATERIALS SCIENCE↗

Intrinsic reactivity and dissolution characteristics of tetracalcium aluminoferrite

Tetracalcium aluminoferrite is one of the main phases of Portland cement, the dissolution characteristics of which however have not been fully revealed. This work adopted first-principles calculations and Mössbauer spectroscopy as well as X-ray diffraction analysis to clarify the intrinsic reactivity of different species of tetracalcium aluminoferrite crystals. Ca ions are the most reactive species of tetracalcium aluminoferrite and Al ions are slightly more reactive than Fe ions. Moreover, the tetrahedral Al and Fe ions are more reactive than the octahedral Al and Fe ions. These indicate dissolution characteristics of tetracalcium aluminoferrite crystals, namely, Ca ions dissolve first and the tetrahedral species dissolve faster than the octahedral species. After the initial dissolution, the dissolved ions nucleate and grow on the defective surface of C{sub 4}AF and the C{sub 4}AF residues are fully hydroxylated. The further hydration thereafter becomes the complex dissolution with the nucleation and growth of hydration products.

36 MATERIALS SCIENCE↗

Chemical affinity and pH effects on chlorite dissolution kinetics under geological CO 2 sequestration related conditions

The kinetic dissolution of Flagstaff Hill chlorite (CCa-2 from Clay Minerals Society), (Mg 4.55 Al 1.23 Fe 0.12 )(Al 1.04 Si 2.96 )O 10 (OH) 8 , was investigated using a well-mixed flow-through reactor at 100 °C, pH values ranging from 3.0 to 7.5, and variable saturation states. The objective was to measure the dependence of chlorite dissolution rate on pH as well as on degree of undersaturation under conditions applicable to geologic carbon storage. A batch experiment was conducted to determine the equilibrium constant of the dissolution reaction at 100 °C for the chlorite mineral phase used in this study. A series of experiments was run at varying CO 2 partial pressures (0–60 bars) and different flow rates (0.01–0.25 ml/min). Here, we use our experimental results in conjunction with previously published data to separate the effects of pH and solution saturation state. At constant pH, the chlorite dissolution rate decreases slowly as a function of the Gibbs free energy of reaction (ΔG r ), which is a quantitative measure of the degree of undersaturation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Is Pt dissolution a concern from the counter electrode in electrochemical oxygen evolution reaction?

The Pt metal and its oxides dissolution from the counter electrode (CE, in hydrogen evolution reaction (HER)) has been suspected to affect the non-noble metal catalysts toward oxygen evolution reaction (OER). However, little effort has been devoted to this concern, and this work aims to determine the effect. The influence of electrolytes (H 2 SO 4 and NaOH) and Pt CE (acid-treated and pristine) on the Pt dissolution and membrane separations (Nafion and PiperION) on preventing Pt species migration were evaluated. Here, the results indicate only 11.2 ppb Pt from the cathodic electrolyte with Nafion 211 and 5 M NaOH electrolyte is observed, and no Pt is found from all other samples with acid-treated Pt CE. Regarding pristine Pt CE, 0.4 and 4.4 ppb Pt are observed from 0.5 M H 2 SO 4 and 5 M NaOH electrolytes, respectively. The findings in this work include: (1) Nafion membrane can effectively prevent the migration of Pt species from the cathode to the anode side; (2) a simple acid treatment of Pt could minimize the Pt dissolution into the acid electrolyte while showing an opposite role in the alkaline electrolyte; (3) the Pt dissolution from all experiments is minor, indicating Pt is a suitable CE for OER.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Oxidative Dissolution of UO2 in a Simulated Groundwater Containing Synthetic Nanocrystalline Mackinawite

The long-term success of in situ reductive immobilization of uranium (U) depends on the stability of U(IV) precipitates (e.g., uraninite) under oxic conditions. Field and laboratory studies have implicated iron sulfide minerals as redox buffers or oxidant scavengers that may slow oxidation of reduced U(VI) solid phases by oxygen and Fe(III). Yet, the inhibition mechanism(s) and reaction rates of uraninite (UO2) oxidative dissolution by oxic species such as oxygen in FeS-bearing systems remain largely unresolved. To address this knowledge gap, abiotic batch experiments were conducted with synthetic UO2 in the presence and absence of synthetic mackinawite (FeS) under simulated groundwater conditions of pH = 7, PO2 = 0.02 atm, and PCO2 = 0.05 atm (equivalent to total dissolved carbonate of 0.01 M). The kinetic profiles of dissolved uranium indicate that FeS inhibited UO2 dissolution for 51 hr by effectively scavenging oxygen and keeping dissolved oxygen (DO) low. During this time period, oxidation of structural Fe(II) and S(-II) of FeS were found to control the DO levels, leading to the formation of iron oxyhydroxides and elemental sulfur, respectively, as verified by X-ray diffraction (XRD), Mössbauer and X-ray absorption spectroscopy (XAS). After FeS was depleted due to oxidation, DO levels increased and UO2 oxidative dissolution occurred at an initial rate of rm = 1.2 ± 0.4 ×10-8 mol•g-1•s-1, higher than rm = 5.4 ± 0.3 ×10-9 mol•g-1•s-1 in the control experiment where FeS was absent. Soluble U(VI) products were adsorbed by iron oxyhydroxides (i.e. nanogoethite and ferrihydrite) formed from FeS oxidation, which facilitated the detachment of U(VI) surface complexes and more rapid dissolution of UO2. XAS analysis confirmed the adsorption of U(VI) species, and also showed that U(VI) was not significantly incorporated into iron oxyhydroxide structure. This work reveals that both the oxygen scavenging by FeS and the adsorption of U(VI) to FeS oxidation products may be important in U reductive immobilization systems subject to redox cycling events.

Containing↗

Mineral dissolution and precipitation during CO 2 injection at the Frio-I Brine Pilot: Geochemical modeling and uncertainty analysis

During the Frio-I Brine Pilot CO 2 injection experiment in 2004, distinct geochemical changes in response to the injection of 1600 tons of CO 2 were recorded in samples collected from the monitoring well. Previous geochemical modeling studies have considered dissolution of calcite and iron oxyhydroxides, or release of adsorbed iron, as the most likely sources of the increased ion concentrations. We explore in this modeling study possible alternative sources of the increasing calcium and iron, based on the data from the detailed petrographic characterization of the Upper Frio Formation “C”. Particularly, we evaluate whether dissolution of pyrite and oligoclase (anorthite component) can account for the observed geochemical changes. Due to kinetic limitations, dissolution of pyrite and anorthite cannot account for the increased iron and calcium concentrations on the time scale of the field test (10 days). However, dissolution of these minerals is contributing to carbonate and clay mineral precipitation on the longer time scales (1000 years). The one-dimensional reactive transport model predicts carbonate minerals, dolomite and ankerite, as well as clay minerals kaolinite, nontronite and montmorillonite, will precipitate in the Frio Formation “C” sandstone as the system progresses towards chemical equilibrium during a 1000-year period. Cumulative uncertainties associated with using different thermodynamic databases, activity correction models (Pitzer vs. B-dot), and extrapolating to reservoir temperature, are manifested in the difference in the predicted mineral phases. Furthermore, these models are consistent with regards to the total volume of mineral precipitation and porosity values which are predicted to within 0.002%.

54 ENVIRONMENTAL SCIENCES↗

Facile synthesis of hollow zeolite microspheres through dissolution–recrystallization procedure in the presence of organosilanes

Hollow zeolite microspheres have been hydrothermally synthesized in the presence of organosilanes via a dissolution–recrystallization procedure. In the presence of organosilanes, zeolite particles with a core/shell structure formed at the first stage of hydrothermal treatment, then the core was consumed and recrystallized into zeolite framework to form the hollow structure during the second hydrothermal process. The influence of organosilanes was discussed, and a related dissolution–recrystallization mechanism was proposed. In addition, the hollow zeolite microspheres exhibited an obvious advantage in catalytic reactions compared to conventional ZSM-5 catalysts, such as in the alkylation of toluene with benzyl chloride. - Graphical abstract: Hollow zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure in the presence of organosiline. Highlights: ► Hollow zeolite spheres with aggregated zeolite nanocrystals were synthesized via a dissolution–recrystallization procedure. ► Organosilane influences both the morphology and hollow structure of zeolite spheres. ► Hollow zeolite spheres showed an excellent catalytic performance in alkylation of toluene with benzyl chloride.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Cr(III) Adsorption on the Dissolution of Boehmite Nanoparticles in Caustic Solution

Incorporation of relatively minor impurity metals onto metal (oxy)hydroxides can strongly impact solubility. In complex highly alkaline multicomponent tank waste such as that at the Hanford Nuclear Reservation, tests indicate that the surface area-normalized dissolution rate of boehmite ($γ$-AlOOH) nanomaterials is at least an order of magnitude lower than that predicted for the pure phase. In this work we examine the dissolution kinetics of boehmite coated by adsorbed Cr(III), which adheres at saturation coverages as sparse chemisorbed monolayer clusters. Using 40 nm boehmite nanoplates as a model system, temperature-dependent dissolution rates of pure versus Cr(III)-adsorbed boehmite showed that the initial rate for the latter is consistently several times lower, with an apparent activation energy 16 kJ·mol -1 higher. Although the surface coverage is only around 50%, solution analytics coupled to multimethod solids characterization reveals a phyicochemical armoring effect by adsorbed Cr(III) that substantially reduces the number of dissolution-active sites on particle surfaces. Such findings could help improve kinetics models of boehmite and/or metal ion adsorbed boehmite nanomaterials, ultimately providing a stronger foundation for the development of more robust complex radioactive liquid waste processing strategies.

54 ENVIRONMENTAL SCIENCES↗

Formate-Induced Dissolution and Reprecipitation of a Copper Electrocatalyst during Electrochemical CO 2 Reduction Reaction

Catalyst size, morphology, and crystal structure play crucial roles in determining the activity and selectivity of electrochemical CO 2 reduction reactions, which are known to change during the reaction process. A comprehensive understanding of how, when, and why these parameters evolve under operational conditions is essential for developing stable, efficient, and selective catalysts. In this study, we reveal that formate, one of the reaction products, contributes to the degradation of copper catalysts through a ligand-assisted dissolution mechanism. Utilizing in situ electrochemical atomic force microscopy and ex-situ scanning and transmission electron microscopies, we observed a significant reduction in the size of copper nanoparticles, which decreased from over 30 nm to less than 10 nm in diameter within 60 min of CO 2 RR. The temporal production of formate correlated with the particle size changes. Furthermore, analysis of the electrolyte using inductively coupled plasma optical emission spectroscopy confirmed the dissolution of copper nanoparticles. Control experiments involving various reaction products (H 2 , CO, and HCOO – ) demonstrated that formate significantly promotes copper dissolution, thereby highlighting its role in the ligand-assisted dissolution mechanism of copper electrocatalysts. In conclusion, our findings provide critical insights into copper catalyst behavior during electrochemical CO 2 reduction, facilitating the design of more resilient and effective electrocatalysts.

Catalysts↗

Large-scale computational polymer solubility predictions and applications to dissolution-based plastic recycling

Dissolution-based plastic recycling is a promising approach to separate and recover high quality pure polymer resins from multicomponent plastic waste by exploiting differences in polymer solubility. The design of a dissolution-based polymer recycling process requires the selection of appropriate solvent systems and operating temperatures to dissolve only target polymers. Determining these parameters experimentally is challenging due to the wide range of solvents and temperatures possible for a given set of target polymers. In this work, we report a computational scheme that employs molecular dynamics simulations and the Conductor-like Screening Model for Realistic Solvents to predict polymer solubilities. Using this scheme, we established a computational solubility database for 8 common polymers and 1007 solvents at multiple temperatures and measured selected solubilities experimentally to validate computational predictions. Analysis of functional groups within this large database then provides chemical heuristics relating the molecular structures of good and non-solvents for selected polymers. We further developed a tool that automates the selection of solvents for all possible sequences in which target polymers can be selectively dissolved to guide the design of dissolution-based plastic recycling processes. Here, we demonstrate the application of these methods via multiple experimental case studies of representative dissolution-based polymer recycling processes in which pure polymer resins were successfully recovered from physical mixtures of polymers.

42 ENGINEERING↗