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Chemical processing of highly radioactive materials commonly takes place in heavily shielded hot cells. The remote, real-time monitoring of chemical processing streams via optical spectroscopic techniques in hot cells may be particularly useful. Here, we describe the implementation of Raman spectroscopy and chemometric analysis to monitor the dissolution of aluminum-clad targets containing irradiated aluminum-neptunium oxide cermet pellets in caustic solutions in a hot cell environment. Partial least squares regression analysis was used to generate calibration models to quantify the concentration of dissolved aluminum, nitrate, and hydroxide in solutions within the radiochemical hot cell. This work explored a systematic approach to optimize a matrix of calibration standards using a D-optimal experimental design. The Design of Experiments-based regression model, in comparison to more traditional analytical approaches, was found to be the more practical method for building calibration models, with fewer samples, to obtain informative analytical data from Raman spectra.
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BACKGROUND: Controlled self-assembly using molecules/nanoparticles as building block materials represents an important approach for nanofabrication. METHOD: We present a "bottom-up" fabrication approach to first grow a new class of inorganic (silica) long hair-like microfibrils or microwires and then to form monolithic solid pellet that contains parallel arrays of bundled microfibrils with a controlled orientation. During the sol-gel solution processing, reactive precursor species are utilized as molecular "building blocks" for the field-directed assembly growth of microfibrils driven by an electric field of pulsed direct current (dc) with controlled frequency. RESULTS: We have demonstrated a novel reactive electrofibrilation process that combines an external field with a solid-phase nucleation and growth process which in principle has no limitation on the type of reactions (such as the one here that involves sol-gel reaction chemistry) and on materials compositions (such as the example silica oxide), thus will enable bulk production of long microfibrils of wide variety of inorganic materials (other oxides or metals). Furthermore, we have fabricated uniquely architectured monolithic solid materials containing aligned microfibrils by "wet press" of the in-situ grown microfibril structure in the electric field. The consolidated monolithic slabs (1 cm × 1 cm × 3 mm) have shown anisotropic properties and desirable retention of DNA molecule fragments, thus, could serve as a platform stationary-phase materials for future development of capillary electrochromatography for biomolecule separations. CONCLUSION: Electrical field-guided self-assembly is an effective approach in producing long (hair-like) ceramic microfibrils, which can be further used in consolidation fabrication of oriented structured ceramic monoliths with potential for capillary electrophoretic chromatography and other separations applications. This original work was recorded through a patent application to understand the fibril formation mechanism and its process.
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Neutron imaging is presented as a tool for quantifying the diffusion of ions inside porous materials, such as carbon electrodes used in the desalination process via capacitive deionization and in electrochemical energy-storage devices. Monolithic mesoporous carbon electrodes of â¼10 nm pore size were synthesized based on a soft-template method. The electrodes were used with an aqueous solution of gadolinium nitrate in an electrochemical flow-through cell designed for neutron imaging studies. Sequences of neutron images were obtained under various conditions of applied potential between the electrodes. The images revealed information on the direction and magnitude of ion transport within the electrodes. From the time-dependent concentration profiles inside the electrodes, the average value of the effective diffusion coefficient for gadolinium ions was estimated to be 2.09 ± 0.17 × 10(-11) m(2) s(-1) at 0 V and 1.42 ± 0.06 × 10(-10) m(2) s(-1) at 1.2 V. The values of the effective diffusion coefficient obtained from neutron imaging experiments can be used to evaluate model predictions of the ion transport rate in capacitive deionization and electrochemical energy-storage devices.
RESUMEN
Six laboratory scale biogas mixed anaerobic digesters were operated to study the effect of biogas recycling rates and draft tube height on their performance. The digesters produced methane at 0.40-0.45 L per liter of digester volume per day. A higher methane production rate was observed in unmixed digesters, while increased biogas circulation rate reduced methane production. However, different draft tube heights caused no difference in the methane production rate. Air infiltration (up to 15% oxygen in the biogas) was observed in the digesters mixed by biogas recirculation. Slight air permeability of tubing or leakage on the vacuum side of the air pump may have caused the observed air infiltration. The similar performance of the mixed and unmixed digesters might be the result of the low solids concentration (50 g dry solids per liter of slurry) in the fed animal slurry, which could be sufficiently mixed by the naturally produced biogas.