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All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Nuclear Thermal Energy Storage Configurations for Industrial Combined Heat and Power Supply: Conceptual Study and Engineering Designs

The industries examined in this report primarily rely on moderate-temperature heat provided by gas- or coal-fired boilers and combined heat and power (CHP) plants, delivered through standard process steam systems. High-temperature energy demands are often industry-specific and typically exceed the capabilities of high-temperature gas-cooled reactors (HTGRs). While it is technically feasible to replace process steam from fossil-based heat sources with nuclear energy, certain industries, such as methanol production and pulp and paper, face technoeconomic challenges in integrating nuclear energy without major changes or a technological shift. This is mainly due to the limited external energy demand remaining after the use of internal byproducts, waste heat recovery, and simple efficiency improvements. Achieving full decarbonization of these processes with nuclear energy would require significant technological advancements, involving experimental technology and substantial investments, making widespread adoption in existing industrial plants unlikely in the near term. This study reviews TES options in the context of enabling a flexible CHP supply while maintaining a steady nuclear heat input. Heat storage systems that interface between the reactor primary fluid and the CHP system offer superior performance and flexibility. Specifically, steam extraction downstream of the reheater with a two-tank molten-salt TES appears as the best solution regarding thermodynamic system benefits and system drawbacks. Using selected system configurations, a conceptual design of an industrial energy park was developed for industries with varying energy demands, such as steel production plants utilizing electric arc furnaces (EAFs) and chemical plants, as well as for those with constant energy demands, like petroleum refineries. This design highlights the capabilities of TES and explores its potential business cases. The study also conceptually develops the potential for integrating additional energy sources with nuclear systems through the implementation of TES. The potential of the HTGR-TES-CHP system was also evaluated considering key uncertainties such as industrial demand profiles, external grid access availability, and eligible tax credit levels, using the Holistic Energy Resource Optimization Network. Sensitivity of net present value to these uncertainties was analyzed to determine the optimal number of nuclear reactors (and CHP systems) and the suitable TES capacity. The results were interpreted from a decision-maker’s perspective, focusing on three key areas: deployment strategy (oversized units vs. undersized units with TES support), industrial process characteristics (thermal-intensive single profiles vs. electricity-intensive combined profiles), and operational goals (maximizing profits vs. minimizing natural gas (NG) consumption or external grid dependence). The optimization results indicate that the HTGR-TES-CHP system significantly reduces reliance on NG boilers for individual industrial processes by 9-60% (in NG capacity factor), with an average reduction of 38%, compared to standalone NG boiler operation case (Business As Usual [BAU]). For combined industrial processes, the reduction ranges from 37-77%, with an average of 60%. Additionally, the system greatly reduces dependence on external grids. In meeting industrial electrical demands, a 33-100% self-sufficient internal electricity supply is achieved for single industrial process, with an average of 74%, compared to the BAU scenario, where 100% of electricity is imported. For combined processes, 35-100% of internal electricity demands are met by the reactor, with an average of 73%. At last, the relative NG price levels at which the proposed HTGR-TES-CHP system can cost-effectively enter the market currently dominated by existing NG boilers were estimated. For a moderate HTGR CAPEX level ($\$$2500/kWth, $\$$6329/kWe), the analysis suggests that NG prices must be 2.5 to 7 times higher than HTGR variable operating and maintenance costs for single industrial process, and 5.5 to 9.5 times higher for a combined process scenario. Tax credit modeling shows that the Investment Tax Credit significantly reduces the price threshold needed to break even, making the system competitive with NG boilers in certain cases.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2019

In Stream Monitoring of Off-Gasses from Plutonium Fluorination

Technology enabling real-time analysis is currently being developed to assess and advance processes used for the fluorination of actinides, which have increasing demands in the fields of forensics and molten salt reactor applications. Well established methods of fluorination use HF, a toxic and corrosive gas, which greatly limits materials of construction for probes and interfaces and is typically incompatible with detectors at greater than part per million quantities. The technology being developed utilizes Raman spectroscopy interrogation of the off-gas stream, providing detailed instantaneous process information in conditions up to 100% HF. The real-time data not only provides detailed reaction information, but also allows for a reduction, via process optimization, in the use of HF benefitting worker health and safety, minimizing waste, and prolonging equipment life.

PuF4, actinide fluorination, Raman↗
DOE OSTI2019

Fuel Cycle Performance of Fast Spectrum Molten Salt Reactor Designs

In the search for new ways to generate low-carbon, reliable base-load power, a resurgence of interest in advanced nuclear energy technologies, including Molten Salt Reactors (MSRs), has produced multiple new conceptual MSRs including fast neutron spectrum designs. The fuel cycle performance of four historical fast MSR designs is analyzed using a recently developed SCALE/TRITON 6.2.4 Alpha with a continuous online reprocessing functionality. The fast spectrum and continuous feed and removal of material enable these concepts to have remarkable fuel cycle metrics: (1) resource utilization is approximately 18 times better than for a typical low-enriched thermal spectrum once-through fuel cycle (i.e., from approximately 180 t/GWe-year to 1 t/GWe-year); (2) fast MSRs generate approximately 25 times less nuclear waste than the current once-through fuel cycle. These metrics are consistent with the Evaluation and Screening Study, which produced a technology-agnostic quantification of the characteristic performance of alternate fuel cycles. Additionally, full-core and unit cell transport models were created and compared to verify the viability of using simplified unit cell geometries for long-term depletion simulation. The unit cell approximation provided a speedup of 20 times relative to the full-core simulation, with depleted mass relative error for major isotopes of less than 2%. Additional fast MSRs design and analysis challenges associated with different fuel cycles and the use of MSR technology are addressed and discussed.

Rykhlevskii, Andrei↗
DOE OSTI2018

FY18 Status Report: SNL Research into Stress Corrosion Cracking of SNF Interim Storage Canisters

This progress report describes work done in FY18 at Sandia National Laboratories (SNL) to assess the localized corrosion performance of container/cask materials used in the interim storage of spent nuclear fuel (SNF). The work focuses on stress corrosion cracking (SCC), the only mechanism by which a through-wall crack could potentially form in a canister outer wall over time intervals that are shorter than possible dry storage times. Work in FY18 continued several studies initiated in FY17 that are aimed at refining the understanding of the chemical and physical environment on canister surfaces, and evaluating the relationship between chemical and physical environment and the form and extent of corrosion that occurs. The SNL canister environment work focused on evaluating the stability of sea-salt deliquescent brines on the heated canister surface; an additional opportunity to analyze dusts sampled from an inservice spent nuclear fuel storage canister also arose. The SNL corrosion work focused predominantly on pitting corrosion, a necessary precursor for SCC, and process of pit-to-crack transition. SNL is collaborating with several university partners to investigate SCC crack growth experimentally, providing guidance for design and interpretation of experiments. The scope of these efforts targets near-marine Independent Spent Fuel Storage Installation environments which are generally considered to be most aggressive for pitting and SCC. Work to define the chemical and physical environment that could develop on storage canister surfaces in near-marine environments included experiments to evaluate the thermal stability of magnesium chloride brines, representative of the first brines to form when sea-salts deliquesce, with the specific goal of understanding and interpreting results of sea-salt and magnesium chloride corrosion experiments carried out under accelerated conditions. The experiments showed that magnesium chloride brines, and by extension, low RH sea-salt deliquescent brines, are not stable at elevated temperatures, losing chloride via degassing of HC1 and conversion to Mg-hydroxychlorides and carbonates. The experiments were carried out on an inert substrate to eliminate the effects of corrosion reactions, simulating brine stabilities in the absence of, or prior to, corrosion. Moreover, analysis of salts recovered from actively corroding metal samples shows that corrosion also supports or drives conversion of magnesium chloride or sea-salt brines to less deliquescent salts. This process has significant implications on corrosion, as the secondary phases are less deliquescent than magnesium chloride; the conversion reaction results in decreases in brine volume, and potentially results in brine dry-out. The deliquescence properties of these reaction products will be a topic of active research in FY19.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2021

Hydrogenous Content in Residues from Aqueous Chloride Pu and Am Recovery Operations

Byproduct residues generated from Aqueous Chloride Pu and Am recovery operations at Los Alamos National Laboratory have been investigated and determined to contain high weight % chloride salts and minimal hydrogen content. Hydrogen content is the result of limited surface area adsorption of ambient moisture. The assumption used in technical analysis NCS-TECH-19-029 to model potentially hydrogenous items as mixtures of polyethylene is shown to be overly conservative. Our results and literature precedent indicate that water adsorption of 1-3 % by weight is expected for hydroxide cakes and Pu oxides, and a conservative bounding assumption for these materials is 5% water by weight. LOH results for a dissolution heel stored long term showed 6.25% weight loss, which was conservatively assumed to be water. A conservative bounding assumption for dissolution heels is 8 wt.% water content. This equates to 0.55 % hydrogen by weight for hydroxide cakes, and 0.88% hydrogen by weight for dissolution heels. The bulk composition of dissolution heels reflects the composition of the original byproduct feed material, chloride salts of potassium, sodium, magnesium and calcium. The bulk composition of calcined hydroxide precipitation residues is composed of potassium chloride as a result of potassium hydroxide neutralization of hydrochloric acid solutions. Metal hydroxides generated during the hydroxide precipitation process are decomposed under the conditions of calcination to metal oxide forms.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Carbon electrodes based capacitive deionization for the desalination of water

A capacitive deionization system includes first and second electrodes comprising tire derived carbon particles obtained from a carbonaceous waste-tire source material containing carbon black. A conductive polymer coating on the carbon particles forms coated carbon particles. The first electrode and the second electrode define a flow channel there between, having a first opening for conducting saline solution into the flow channel and a second opening for conducting treated saline solution from the flow channel. A first current collector is provided for the first electrode and a second current collector is provided for the second electrode. An electrical connection between the first and second electrodes. A method of making a system for the capacitive deionization of a salt from a liquid, and a method for the capacitive desalination of a saline solution are also disclosed.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Summary of Expedited Results from Samples Supporting Tank Closure Cesium Removal (TCCR) Batch 3

Savannah River Remediation (SRR) is currently operating the Tank Closure Cesium Removal (TCCR) process to remove 137 Cs from tank waste supernate using an ion exchange process. As part of that process, Savannah River National Laboratory (SRNL) receives and analyzes samples in support of the qualification of each batch to be processed. SRNL recently received supernate samples retrieved from Tank 10H as well as in-tank batch contact samples for characterization in support of qualifying Batch 3 for processing through the TCCR unit. SRNL received and characterized a set of dip samples collected from Tank 10H (one surface and one variable depth sample). No solids were observed in either sample and therefore the samples were combined, and a suite of analyses were performed on the composite sample. The density of the combined sample was 1.174 g/mL (0.18 %RSD), which was consistent with the measured sodium concentration of 3.54 M (0.08 %RSD). The 137Cs activity in the sample was 4.75E+07 dpm/mL (4.28 %RSD) and the total Cs concentration was calculated to be 1.54 mg/L (1.16E-05 M). The in-tank batch contact samples consist of 0.1 g of crystalline silicotitanate (CST) contained within a teabag device. Duplicate samples were submerged in Tank 10H supernate for a period of about 13 days, after which time they were retrieved and transferred to SRNL for analysis. At SRNL the CST was rinsed to remove excess salt solution and the CST was then air dried before being digested for analysis. Results of the analysis indicated a 137 Cs loading of 3.66E+10 ± 1.40E+09 dpm/g or 16.5 ± 0.63 Ci/kg CST . This value represents a bounding upper limit as it includes the addition of two sigma uncertainty from replicate analysis of the individual teabag samples as well as the addition of the small amount of 137 Cs activity measured in the rinse solutions. The above values are based on the air-dried mass of CST. Correcting to the true dry mass using a F-factor of 0.8191 results in a maximum loading of 20.2 ± 0.77 Ci/kg CST .

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2020

Solid-State Recrystallization Pathways of Sodium Aluminate Hydroxy Hydrates

Crystallization of Al-bearing solid phases from highly alkaline Na 2 O:Al 2 O 3 :H 2 O solutions commonly necessitates an Al 3+ coordination change from tetrahedral to octahedral, but intermediate coordination states are often difficult to isolate. Here, a similar Al 3+ coordination change process is examined during the solid-state recrystallization of sodium oxohydroxoaluminate hydrate (MSA) to nonasodium bis(hexahydroxy aluminate) trihydroxide hexahydrate (NSA) at ambient temperature. While the MSA structure contains solely polymerized tetrahedral Al 3+ , the NSA structure is a molecular aluminate salt solely based upon monomeric octahedral Al 3+ . Spontaneous recrystallization of MSA and excess sodium hydroxide hydrate into NSA over 3 days of reaction time was clearly evident in X-ray diffractograms and in Raman spectra. In situ 27 Al multiple quantum MAS NMR spectroscopy showed no evidence of intermediate aluminates, suggesting that intermediates, such as pentacoordinate Al 3+ , are short-lived and require more highly time resolved spectroscopies to detect. Such research is advancing upon detailed mechanistic understanding of Al 3+ coordination change mechanisms in these highly alkaline systems, with relevance to aluminum refining, corrosion sciences, and nuclear waste processing.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1993

Kinetic Tetrazolium Microtiter Assay

Kinetic tetrazolium microtiter assay (KTMA) involves use of tetrazolium salts and Triton X-100 (or equivalent), nontoxic, in vitro color developer solubilizing colored metabolite formazan without injuring or killing metabolizing cells. Provides for continuous measurement of metabolism and makes possible to determine rate of action of antimicrobial agent in real time as well as determines effective inhibitory concentrations. Used to monitor growth after addition of stimulatory compounds. Provides for kinetic determination of efficacy of biocide, greatly increasing reliability and precision of results. Also used to determine relative effectiveness of antimicrobial agent as function of time. Capability of generating results on day of test extremely important in treatment of water and waste, disinfection of hospital rooms, and in pharmaceutical, agricultural, and food-processing industries. Assay also used in many aspects of cell biology.

Pierson, Duane L.↗
NASA NTRS2012

Investigation of Supercritical Water Phenomena for Space and Extraterrestrial Application

The cost of carrying or resupplying life support resources for long duration manned space exploration missions such as a mission to Mars is prohibitive and requires the development of suitable recycling technologies. Supercritical Water Oxidation (SCWO) has been identified as an attractive candidate for these extended missions because (i) pre-drying of wet waste streams is not required, (ii) product streams are relatively benign, microbially inert, and easily reclaimed, (iii) waste conversion is complete and relatively fast, and (iv) with proper design and operation, reactions can be self-sustaining. Initial work in this area at NASA was carried out at the Ames Research Center in the 1990 s with a focus on understanding the linkages between feed stock preparation (i.e., particle size and distribution) of cellulosic based waste streams and destruction rates under a range of operating temperatures and pressures. More recently, work in SCWO research for space and extra-terrestrial application has been performed at NASA s Glenn Research Center where various investigations, with a particular focus in the gravitational effects on the thermo-physical processes occurring in the bulk medium, have been pursued. In 2010 a collaborative NASA/CNES (the French Space Agency) experiment on the critical transition of pure water was conducted in the long duration microgravity environment on the International Space Station (ISS). A follow-on experiment, to study the precipitation of salt in sub-critical, trans-critical and supercritical water is scheduled to be conducted on the ISS in 2013. This paper provides a brief history of NASA s earlier work in SCWO, discusses the potential for application of SCWO technology in extended space and extraterrestrial missions, describes related research conducted on the ISS, and provides a list of future research activities to advance this technology in both terrestrial and extra-terrestrial applications.

Hicks, Michael C.↗
DOE OSTI2022

Application of Ionic Liquids for the Recycling and Recovery of Technologically Critical and Valuable Metals

Population growth has led to an increased demand for raw minerals and energy resources; however, their supply cannot easily be provided in the same proportions. Modern technologies contain materials that are becoming more finely intermixed because of the broadening palette of elements used, and this outcome creates certain limitations for recycling. The recovery and separation of individual elements, critical materials and valuable metals from complex systems requires complex energy-consuming solutions with many hazardous chemicals used. Significant pressure is brought to bear on the improvement of separation and recycling approaches by the need to balance sustainability, efficiency, and environmental impacts. Due to the increase in environmental consciousness in chemical research and industry, the challenge for a sustainable environment calls for clean procedures that avoid the use of harmful organic solvents. Ionic liquids, also known as molten salts and future solvents, are endowed with unique features that have already had a promising impact on cutting-edge science and technologies. This review aims to address the current challenges associated with the energy-efficient design, recovery, recycling, and separation of valuable metals employing ionic liquids.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Determination and Comparison of Parameters from Cyclic Voltammetry of LaCl 3 in Eutectic LiCl-KCl

Electrochemical measurements of LaCl 3 were obtained in eutectic LiCl-KCl at 773 K. Cyclic voltammetry data were acquired using a tungsten electrode LaCl 3 amounts in the molten salt in the range of 0.5 to 3.0 wt%. Both cyclic voltammetry and Tafel analyses of the data resulted in calculation of values for the charge transfer coefficient (0.262), diffusion coefficient (1.67 × 10 -5 cm 2 s -1 ), exchange current density (0.0148 to 0.0473 A cm -2 ), and charge transfer resistance (0.404 to 1.99 Ω) related to lanthanum ions in the molten salt. Calculated values were compared to those available in the literature. The values of parameters found in literature varied significantly in comparison to those in the present study due to dissimilar experimental conditions, e.g., electrode material, temperature, and LaCl 3 concentration.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2018

Coordination Chemistry of a Strongly-Donating Hydroxylamine with Early Actinides: An Investigation of Redox Properties and Electronic Structure

Separations of f-block elements are a critical aspect of nuclear waste processing. Redox-based separations offer promise, but challenges remain in stabilizing and differentiating actinides in high oxidation states. The investigation of new ligand types that provide thermodynamic stabilization to high-valent actinides is essential for expanding their fundamental chemistry and to elaborate new separation techniques and storage methods. We report herein the preparation and characterization of Th and U complexes of the pyridyl-hydroxylamine ligand, N-tert-butyl-N-(pyridin-2-yl)hydroxylamine (pyNO–). Electrochemical studies performed on the homoleptic complexes [M(pyNO) 4 ] (M = Th, U) revealed significant stabilization of the U complex upon one-electron oxidation. The salt [U(pyNO) 4 ] + was isolated by chemical oxidation of [U(pyNO) 4 ]; spectroscopic and computational data support assignment as a U V cation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2017

Advanced, Energy-Efficient Hybrid Membrane System for Industrial Water Reuse

In the U.S. manufacturing sector, current industrial water use practices are energy-intensive and utilize and discharge high volumes of waters, rendering them not sustainable especially in light of the growing scarcity of suitable water supplies. To help address this problem, the goal of this project was to develop an advanced, cost-effective, hybrid membrane-based water treatment system that can improve the energy efficiency of industrial wastewater treatment while allowing at least 50% water reuse efficiency. This hybrid process would combine emerging Forward Osmosis (FO) and Membrane Distillation (MD) technology components into an integrated FO-MD system that can beneficially utilize low-grade waste heat (i.e., T < 450 °F) in industrial facilities to produce distilled-quality product water for reuse. In this project, laboratory-, bench-, and pilot-scale experiments on the hybrid FO-MD system were conducted for industrial wastewater treatment. It was demonstrated at laboratory, bench, and pilot scales that FO-MD membrane technology can concentrate brine to very high total dissolved solids (TDS) levels (>200,000 ppm) that are at least 2.5 times higher than the TDS level to which RO can achieve. In laboratory testing, currently available FO and MD membranes were tested to select for high-performing membranes with high salt rejection and high water flux. Multiple FO membrane/draw-salt solution combinations that gave high water flux with higher than 98% salt rejection were also identified. Reverse draw-salt fluxes were observed to be much lower for divalent salts than for monovalent salts. MD membranes were identified that had 99.9+% salt rejection and water flux as high as 50-90 L/(m 2 ·h) for flat-sheet membranes and >20 L/(m 2 ·h) for hollow fibers. In bench-scale testing, a single unit of commercially available FO and MD membrane modules were evaluated for continuous, integrated operation. Using the laboratory- and bench-scale test data, numerical modeling was performed on the FO and MD processes to estimate engineering parameters for a larger-scale pilot unit. Based on the experimental studies and modeling results, a pilot-scale, integrated FO-MD prototype unit was designed and built for trailer-mounted operation. This prototype system was fed real industrial wastewater, which could not be further treated by conventional technologies, from an oil production facility and was successfully operated for over 15 weeks without major stoppage. About 90% water recovery was possible, while concentrating the TDS from 12,000 ppm up to 190,500 ppm. The FO-MD prototype rejected most wastewater contaminants while producing water with <300 ppm TDS, even when the feed TDS was higher than 150,000 ppm. No chemical cleaning was necessary during the pilot testing period. Flushing the system with dechlorinated tap water was sufficient to reset the membranes for the next set of test conditions. Pilot performance and membrane autopsy showed that, even though the feed was concentrated more than 10 times, membrane fouling was unnoticeable and no defects were detected on the FO and MD membrane surfaces. This project demonstrated the technical feasibility of the hybrid FO-MD process by taking water already treated to the limit with the highest level of current technologies and further concentrating it 10-fold by using mostly low-cost materials. Because no membranes suitable for full-scale plant applications are available at present, economical feasibility of the hybrid technology is still uncertain, but it is expected that broader industry participation can further reduce FO-MD process costs.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2018

Regulatory Gap Analysis of Select NUREG-0800 Chapters for Applicability to Molten Salt Reactors

The past licensing approach for advanced reactors was based on adapting the current LWR-based NRC process that exists today to the advanced reactor concept. This is the approach used by advanced technologies such as the Pebble Bed Reactor licensing application, the Clinch River Breeder Reactor licensing application, and more recently the NuScale licensing application. Current Standard Review Plan (SRP) guidance for large LWRs is available in NUREG-0800, Standard Review Plan for the Review of Safety Analysis Reports for Nuclear Power Plants: Light Water Reactor (LWR) Edition. However, the SRP is cumbersome to apply to liquid-fueled molten salt reactor (MSR) technologies. Therefore, a thoughtful licensing approach for MSRs is necessary.This report documents for DOE-NE an additional regulatory gap analysis of select chapters from the LWR SRP to further inform a generic nonpower MSR test program. Although the review process outlined in NUREG-0800 is LWR-specific, the plant functions and processes to be reviewed will be similar for the MSR. Therefore, a well-planned nonpower MSR test program can provide the performance data needed to better facilitate the eventual commercial-sized MSR review. The LWR SRP chapters dealing with the reactor, reactor coolant, engineered safety features, auxiliary systems, and waste management systems were reviewed.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2020

Benzenesulfonamide Derivatives as Complexants and Extractants for Addressing the Mercury Problem at the Savannah River Site

Mercury (Hg) is a major global pollutant arising from both natural and anthropogenic sources. Its widespread use in medicinal and industrial applications makes it a common chemical exposure and environmental pollutant. It can exist in several forms which include: Metallic mercury (Hg{sup 0}), mercurous (Hg{sub 2}{sup 2+}), mercuric salts (Hg{sup 2+}), and organic mercury (e.g. CH{sub 3}Hg{sup +}), with the latter being the most toxic of all the species. Due to mercury's high toxicity, new approaches towards its detection has received significant attention in the scientific community. Mercury exposure at the Savannah River Site (SRS) has been a recent concern especially with increasing amounts of organic mercury in the saltstone. It originates mainly from its use as an acidic dissolution catalyst of aluminum cladding from target fuels within the uranium and plutonium processing operations [1]. It is present to an amount of about 60 metric tons in the high-level waste (HLW) tanks. Organic Mercury species have been found in low activity waste (LAW) at the site that eventually ends up in the saltstone. Therefore, there is a need for: i) Converting organic mercury to other less toxic forms and ii) Complexation and removal of Hg prior of disposal of LAW in saltstone. Various methods have been developed for selective sensing of mercury in the presence of other toxic metals. These methods include using ligands that can form organo-soluble metal complexes with different optical and spectroscopic properties that can be used for toxic metal sensing. In 2005, our group pioneered an ion-exchange extraction method, in which o-phenylenediamine-derived disulfonamides were used to complex and selectively extract and sense Pb{sup 2+} from aqueous solutions into an organic phase [2,3]. Herein, a disulfonamide and a bis-dansylamide have been shown to extract, complex and sense Hg(II). Ligand 1: The crystal structure of the disulfonamide-Hg complex confirms the complexation of Hg(II) with the ligand. Complexation was corroborated by the {sup 1}H-NMR spectra obtained after contacting solutions of various concentrations of Hg{sup 2+} with 2 mM ligand in chloroform. Distinct resonances are observed at Hg/L ratio of 0.5 that are also observed for the isolated 1:2 complex. In the presence of excess mercury, new resonances, as well as the movement of Et{sub 3}N resonances indicate the formation of a different Hg-sulfonamide-triethylamine complex, presumably having 1:1 Hg:L stoichiometry. The electronic spectra of aqueous phases after extraction show that there was no free ligand absorption at 0.5 eq of Hg, indicating a complete complexation. Complexation was also confirmed by the UV-visible titrations with Hg{sup 2+} at constant ligand concentration. pH-dependent extraction carried out shows that extraction of Hg(II) by ligand 1 was over 90% for most alkaline pHs. Ligand 2: The crystal structure of the Ligand 2 complex formed with Hg(OAc){sub 2} shows a remarkable coordination pattern with 4:2 metal:ligand stoichiometry. The fluorescent bis-dansyl disulfonamide derivative was found to complex and sense HgCl{sub 2} and Hg(OAc){sub 2} by demonstrating fluorescence quenching upon Hg(II) addition in comparison with other metals (Zn(II), Cd(II), Pb(II)). No were observed for Cu(II), Ag(I) and Co(II). We have shown the complexation of Hg(II) by a disulfonamide and a bis-dansyl disulfonamide ligand using several spectroscopic methods. Ligand 1 was able to extract mercury into chloroform and form a complex in the presence of excess mercury by synergistic complexation with triethylamine acting as a co-ligand. X-ray and NMR both confirm a 1:2 HgL{sub 2} stoichiometry. Ligand 2 can be used for sensing of Hg(II) as fluorescence quenching was observed after addition of Hg(II)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS2021

Supercritical Water Oxidation (SCWO) Trade Study and 2021 Final Report

SCWO is a promising technology whose main benefits is that it is capable of completely mineralizing organic compounds in wastewater and separating inorganic salts. This means that SCWO can theoretically function as a single step water treatment system. It performs the functions of both the primary treatment system and the secondary brine drying function to achieve near 100% water recovery. It can also handle solids so no pretreatment of the feed is required. A preliminary trade study indicates that SCWO could be competitive with the ISS state of the art if its power consumption could be reduced. Thermal and mechanical energy recovery system exist that could reduce SCWO energy consumption to a level that is competitive with the state of the art. In addition, increasing the feed wastewaters organic content by including other wastes, such as feces, could produce a reactor that is thermally self-sustaining. There are 5 different types of SCWO reactors. They are; tubular, tank, impingement, transpiring wall reactors (TWR) and super critical water mixing (SCWM) reactors. Of these the best suited for NASA missions are the impingement and SCWM reactors. The impingement reactor is best suited for near term missions because it can treat the low organic content wastewaters such as are expected for initial Lunar and Mars missions and has the ability to remove precipitated inorganic solids. The SCWM reactor is best suited for longer duration CELSS type missions where high organic content wastewater is available and will resolve solids fouling and corrosion issues. In addition, these two reactors have a long NASA heritage and have been developed specifically for space flight application. Tubular reactors suffer from plugging issues which is a safety concern. Tank reactors will increase in size inversely with gravity, which will trade poorly in Lunar and Mars environments where gravity is reduced. TWR reactors require high organic content wastewater feed and the SCWM reactor is an optimized version of the TWR for NASA applications. It is recommended that in FY 2022 NASA continue to fully evaluate the ability of SCWO to produce potable water and remove inorganics as a solid byproduct. This should be done using the impingement reactor for near term missions and SCWM for longer duration missions. NASA should also develop optimized recuperative heat exchangers and pressure recovery devices to reduce power consumption and investigate inclusion of feces and other organic wastes into the wastewater model to increase its organic content and further reduce thermal energy requirements.

Supercritical Water Oxidation↗
DOE OSTI2022

Volatility of sodium, potassium, and cesium perrhenates determined by thermogravimetry

Here, in this study, we investigated the volatility of sodium, potassium, and cesium perrhenates using thermogravimetry (TG) performed on single salts and their binary mixed salts. We performed simultaneous TG and differential scanning calorimetry under a ramp heating condition at 10°C/min up to 1200°C to characterize volatilization behavior as a function of temperature. We also performed isothermal TG over a temperature range of 700 to 975°C to estimate the vapor pressures of the alkali perrhenates based on a modified Langmuir equation that relates the rate of free evaporation from the open surface to vapor pressure. In this paper, we discuss the results of our study on the temperature of evaporation and temperature-dependent vapor pressure of sodium, potassium, and cesium perrhenates in relation to rhenium volatilization behavior observed during melting of simulated waste glass.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗