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Initial Testing of a Full-Scale Ultrasonic Clothes Washer/Dryer for Moon, Mars, ISS and Beyond

This study investigates the effectiveness of an ultrasonic-based combo garment washing and drying system for space applications. The system leverages our technological innovations in direct-contact ultrasonic fabric drying in combination with ultrasonic fabric washing. The main objective of this investigation is to gauge the effectiveness of washing and drying medium-size T-shirts ultrasonically. This paper will report the results of experiments conducted to assess the effectiveness of washing clothes ultrasonically, including ultrasonic intensity testing, stain removal testing, and fabric degradation testing. The outcome of this study could lead to the design and development of the first ultrasonic clothes washer and dryer for space applications that would reduce clothing resupply costs for crewed missions to the moon, Mars, and micro-gravity space stations.

Crew systems↗

NASA NTRSDate not supplied

Initial Testing of a Full-Scale Ultrasonic Clothes Washer/Dryer for Moon, Mars, ISS and Beyond

Crew systems↗

DOE OSTI2015

Waste Isolation Pilot Plant Salt Decontamination Testing

On February 14, 2014, americium and plutonium contamination was released in the Waste Isolation Pilot Plant (WIPP) salt caverns. Several practical, easily deployable methods of decontaminating WIPP salt, using a surrogate contaminant and americium (241Am), were developed and tested. The effectiveness of the methods is evaluated qualitatively, and to the extent practical, quantitatively. Of the methods tested (dry brushing, vacuum cleaning, water washing, mechanical grinding, strippable coatings, and fixative barriers), the most practical seems to be water washing. Effectiveness is very high, and water washing is easy and rapid to deploy. The amount of wastewater produced (~2 L/m2) would be substantial and may not be easy to manage, but the method is the clear winner from a usability perspective. Removable surface contamination levels (smear results) from water washed coupons found no residual removable contamination. Thus, whatever contamination is left is likely adhered to (or trapped within) the salt. The other option that shows promise is the use of a fixative barrier. Bartlett Nuclear, Inc.’s Polymeric Barrier System proved the most durable of the coatings tested. The coatings were not tested for contaminant entrapment, only for coating integrity and durability.

Decontamination↗

DOE OSTI2013

Sludge Settling Rate Observations and Projections at the Savannah River Site - 13238

Since 2004, sludge batches have included a high percentage of stored sludge generated from the H- modified (HM) process. The slow-settling nature of HM sludge means that the settling is often the major part of the washing tank quiescent period between required pump runs to maintain flammability control. Reasonable settling projections are needed to wash soluble salts from sludge in an efficient manner, to determine how much sludge can be washed in a batch within flammability limits, and to provide composition projections for batch qualification work done in parallel with field preparation. Challenges to providing reasonably accurate settling projections include (1) large variations in settling behavior from tank-to-tank, (2) accounting for changing initial concentrations, sludge masses, and combinations of different sludge types, (3) changing the settling behavior upon dissolving some sludge compounds, and (4) sludge preparation schedules that do not allow for much data collection for a particular sludge before washing begins. Scaling from laboratory settling tests has provided inconsistent results. Several techniques have been employed to improve settling projections and therefore the overall batch preparation efficiency. Before any observations can be made on a particular sludge mixture, projections can only be made based on historical experience with similar sludge types. However, scaling techniques can be applied to historical settling models to account for different sludge masses, concentrations, and even combinations of types of sludge. After sludge washing/settling cycles begin, the direct measurement of the sludge height, once generally limited to a single turbidity meter measurement per settle period, is now augmented by examining the temperature profile in the settling tank, to help determine the settled sludge height over time. Recently, a settling model examined at PNNL [1,2,3] has been applied to observed thermocouple and turbidity meter readings to quickly provide settling correlations to project settled heights for other conditions. These tools improve the accuracy and adaptability of short and mid-range planning for sludge batch preparation. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Development of a Thermodynamic Model for the Hanford Tank Waste Operations Simulator - 12193

The Hanford Tank Waste Operations Simulator (HTWOS) is the current tool used by the Hanford Tank Operations Contractor for system planning and assessment of different operational strategies. Activities such as waste retrievals in the Hanford tank farms and washing and leaching of waste in the Waste Treatment and Immobilization Plant (WTP) are currently modeled in HTWOS. To predict phase compositions during these activities, HTWOS currently uses simple wash and leach factors that were developed many years ago. To improve these predictions, a rigorous thermodynamic framework has been developed based on the multi-component Pitzer ion interaction model for use with several important chemical species in Hanford tank waste. These chemical species are those with the greatest impact on high-level waste glass production in the WTP and whose solubility depends on the processing conditions. Starting with Pitzer parameter coefficients and species chemical potential coefficients collated from open literature sources, reconciliation with published experimental data led to a self-consistent set of coefficients known as the HTWOS Pitzer database. Using Gibbs energy minimization with the Pitzer ion interaction equations in Microsoft Excel,1 a number of successful predictions were made for the solubility of simple mixtures of the chosen species. Currently, this thermodynamic framework is being programmed into HTWOS as the mechanism for determining the solid-liquid phase distributions for the chosen species, replacing their simple wash and leach factors. Starting from a variety of open literature sources, a collection of Pitzer parameters and species chemical potentials, as functions of temperature, was tested for consistency and accuracy by comparison with available experimental thermodynamic data (e.g., osmotic coefficients and solubility). Reconciliation of the initial set of parameter coefficients with the experimental data led to the development of the self-consistent set known as the HTWOS Pitzer database. Using Microsoft Excel to formulate the Gibbs energy minimization method and the multi-component Pitzer ion interaction equations, several predictions of the solubility of solute mixtures at various temperatures were made using the HTWOS Pitzer database coefficients. Examples of these predictions are shown in Figure 3 and Figure 4. A listing of the entire HTWOS Pitzer database can be found in RPP-RPT-50703. Currently, work is underway to install the Pitzer ion interaction model in HTWOS as the mechanism for determining the solid-liquid phase distributions of select waste constituents during tank retrievals and subsequent washing and leaching of the waste. Validation of the Pitzer ion interaction model in HTWOS will be performed with analytical laboratory data of actual tank waste. This change in HTWOS is expected to elicit shifts in mission criteria, such as mission end date and quantity of high-level waste glass produced by WTP, as predicted by HTWOS. These improvements to the speciation calculations in HTWOS, however, will establish a better planning basis and facilitate more effective and efficient future operations of the WTP. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Mercury Recovery at Former Lithium Production Site at the Miramas in France - 18529

The former Lithium production facility located at Miramas in the South-East of France recently completed a 10-year program of process equipment removal, building demolition and soil remediation to recover mercury (Hg) that had been lost during operations at the site. After over 100 years ago chemical production, all production activities stopped in 2009, and immediately afterwards the clean-up project began. The main project focused on the demolition of all facilities and the decontamination of building materials and soil clean-up, with the goal of remediating the site for future industrial purposes. Prior to starting the decommissioning and clean-up work at the site a detailed site survey was conducted to identify the extent of the contamination of the site. After investigations into available technologies, the decision was made to install on-site treatment processes. This resulted in fewer residual environmental effects (trucking pollution, shipping containers, volume of materials, etc), a reduction in logistic complications, and, importantly, was cost effective compared to sending all untreated material to external processing facilities. This decision resulted in a need to optimize demolition waste management, while ensuring the highest clean-up and safety levels. A variety of treatment processes were investigated and compared and two technologies were finally selected and implemented. The first process was a 'thermal desorption unit (TDU),' which heated excavated soils and captured the vaporized mercury. The second was a washing process that was used to remove surface contamination. After the contaminated areas were excavated, materials were crushed, screened and sorted into different sizes, with each pile being routed to the appropriate process. The smaller-sized particles were treated in the TDU. A batch of around 12 MT was fed into a moisture evaporator and then into a mercury evaporator. The soils were then cooled, sampled to ensure no residual Hg contamination before being mixed with a binding agent, and returned to the excavation site. Larger materials with surface contamination were washed to remove the contamination. The liquid effluents were sent to a tank where the contaminated fines were removed, dried, pressed and sent for processing. If the washed, coarse materials failed to reach acceptable mercury levels, they were crushed again and sent to be treated in the TDU. The washing fluid was recycled for the next batch. (author)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2015

Approach on environmental risk assessment of nanosilver released from textiles

Based on the increased utilization of nanosilver (silver nanomaterials=AgNM) as antibacterial agent, there is the strong need to assess the potential environmental implication associated with its new application areas. In this study an exemplary environmental risk assessment (ERA) of AgNM applied in textiles was performed. Environmental exposure scenarios (via municipal sewage treatment plant (STP)) with wastewater supply from domestic homes) were developed for three different types of textiles equipped with AgNM. Based on these scenarios predicted environmental concentrations (PECs) were deduced for STPs and for the environmental compartments surface water, sediment as well as soil. These PECs were related to PNECs (predicted no effect concentrations). PNECs were deduced from results of ecotoxicity tests of a selected AgNM (NM-300K). Data on ecotoxicology were derived from various tests with activated sludge, cyanobacteria, algae, daphnids, fish, duckweed, macrophytes, chironomids, earthworms, terrestrial plants as well as soil microorganisms. Emission data for the AgNM NM-300K from textiles were derived from washing experiments. The performed ERA was based on the specifications defined in the ECHA Guidances on information requirements and chemical safety assessment. Based on the chosen scenarios and preconditions, no environmental risk of the AgNM NM-300K released from textiles was detected. Under conservative assumptions a risk quotient for surface water close to 1 indicated that the aquatic compartment may be affected by an increased emission of AgNM to the environment due to the high sensitivity of aquatic organisms to silver. Based on the successful retention of AgNM in the sewage sludge and the still ongoing continual application of sewage sludge on farmland it is recommended to introduce a threshold for total silver content in sewage sludge into the respective regulations. Regarding potential risk mitigation measures, it is emphasized to preferably directly introduce AgNM into the textile fiber since this will strongly minimize the release of AgNM during washing. If this is not possible due to technical limitations or other reasons, the introduction of a threshold level controlling the release of AgNM from textiles is suggested. It has to be noted that this study is a case study which is only valid for the investigated NM-300K and its potential application in textiles. - Highlights: • Washing: release rates of AgNM depend on furnishing in textiles. • Calculated PNECs for the aquatic compartment were low. • For the chosen scenarios no environmental risk of AgNM from textiles was observed. • AgNM is retained in sewage sludge. • In WWTP most of the silver adsorbs to sewage sludge and thus, may reach farmland.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2012

Recovery of solid fuel from municipal solid waste by hydrothermal treatment using subcritical water

Highlights: Black-Right-Pointing-Pointer Hydrothermal treatment using subcritical water was studied to recover solid fuel from MSW. Black-Right-Pointing-Pointer More than 75% of carbon in MSW was recovered as char. Black-Right-Pointing-Pointer Heating value of char was comparable to that of brown coal and lignite. Black-Right-Pointing-Pointer Polyvinyl chloride was decomposed at 295 Degree-Sign C and 8 MPa and was removed by washing. - Abstract: Hydrothermal treatments using subcritical water (HTSW) such as that at 234 Degree-Sign C and 3 MPa (LT condition) and 295 Degree-Sign C and 8 MPa (HT condition) were investigated to recover solid fuel from municipal solid waste (MSW). Printing paper, dog food (DF), wooden chopsticks, and mixed plastic film and sheets of polyethylene, polypropylene, and polystyrene were prepared as model MSW components, in which polyvinylchloride (PVC) powder and sodium chloride were used to simulate Cl sources. While more than 75% of carbon in paper, DF, and wood was recovered as char under both LT and HT conditions, plastics did not degrade under either LT or HT conditions. The heating value (HV) of obtained char was 13,886-27,544 kJ/kg and was comparable to that of brown coal and lignite. Higher formation of fixed carbon and greater oxygen dissociation during HTSW were thought to improve the HV of char. Cl atoms added as PVC powder and sodium chloride to raw material remained in char after HTSW. However, most Cl originating from PVC was found to converse into soluble Cl compounds during HTSW under the HT condition and could be removed by washing. From these results, the merit of HTSW as a method of recovering solid fuel from MSW is considered to produce char with minimal carbon loss without a drying process prior to HTSW. In addition, Cl originating from PVC decomposes into soluble Cl compound under the HT condition. The combination of HTSW under the HT condition and char washing might improve the quality of char as alternative fuel.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2011

SLUDGE BATCH 7B QUALIFICATION ACTIVITIES WITH SRS TANK FARM SLUDGE

Waste Solidification Engineering (WSE) has requested that characterization and a radioactive demonstration of the next batch of sludge slurry - Sludge Batch 7b (SB7b) - be completed in the Shielded Cells Facility of the Savannah River National Laboratory (SRNL) via a Technical Task Request (TTR). This characterization and demonstration, or sludge batch qualification process, is required prior to transfer of the sludge from Tank 51 to the Defense Waste Processing Facility (DWPF) feed tank (Tank 40). The current WSE practice is to prepare sludge batches in Tank 51 by transferring sludge from other tanks. Discharges of nuclear materials from H Canyon are often added to Tank 51 during sludge batch preparation. The sludge is washed and transferred to Tank 40, the current DWPF feed tank. Prior to transfer of Tank 51 to Tank 40, SRNL typically simulates the Tank Farm and DWPF processes with a Tank 51 sample (referred to as the qualification sample). With the tight schedule constraints for SB7b and the potential need for caustic addition to allow for an acceptable glass processing window, the qualification for SB7b was approached differently than past batches. For SB7b, SRNL prepared a Tank 51 and a Tank 40 sample for qualification. SRNL did not receive the qualification sample from Tank 51 nor did it simulate all of the Tank Farm washing and decanting operations. Instead, SRNL prepared a Tank 51 SB7b sample from samples of Tank 7 and Tank 51, along with a wash solution to adjust the supernatant composition to the final SB7b Tank 51 Tank Farm projections. SRNL then prepared a sample to represent SB7b in Tank 40 by combining portions of the SRNL-prepared Tank 51 SB7b sample and a Tank 40 Sludge Batch 7a (SB7a) sample. The blended sample was 71% Tank 40 (SB7a) and 29% Tank 7/Tank 51 on an insoluble solids basis. This sample is referred to as the SB7b Qualification Sample. The blend represented the highest projected Tank 40 heel (as of May 25, 2011), and thus, the highest projected noble metals content for SB7b. Characterization was performed on the Tank 51 SB7b samples and SRNL performed DWPF simulations using the Tank 40 SB7b material. This report documents: (1) The preparation and characterization of the Tank 51 SB7b and Tank 40 SB7b samples. (2) The performance of a DWPF Chemical Process Cell (CPC) simulation using the SB7b Tank 40 sample. The simulation included a Sludge Receipt and Adjustment Tank (SRAT) cycle, where acid was added to the sludge to destroy nitrite and reduce mercury, and a Slurry Mix Evaporator (SME) cycle, where glass frit was added to the sludge in preparation for vitrification. The SME cycle also included replication of five canister decontamination additions and concentrations. Processing parameters were based on work with a nonradioactive simulant. (3) Vitrification of a portion of the SME product and characterization and durability testing (as measured by the Product Consistency Test (PCT)) of the resulting glass. (4) Rheology measurements of the SRAT receipt, SRAT product, and SME product. This program was controlled by a Task Technical and Quality Assurance Plan (TTQAP), and analyses were guided by an Analytical Study Plan. This work is Technical Baseline Research and Development (R&D) for the DWPF. It should be noted that much of the data in this document has been published in interoffice memoranda. The intent of this technical report is bring all of the SB7b related data together in a single permanent record and to discuss the overall aspects of SB7b processing.

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DOE OSTI2016

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Sludge batch 9 (SB9) accepance evaluation: Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a compositioniv expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Demonstration of sulfur solubility determinations in high waste loading, low-activity waste glasses

A method recommended by Pacific Northwest National Laboratory (PNNL) for sulfate solubility determinations in simulated low-activity waste glasses was demonstrated using three compositions from a recent Hanford high waste loading glass study. Sodium and sulfate concentrations in the glasses increased after each re-melting step. Visual observations of the glasses during the re-melting process reflected the changes in composition. The measured compositions showed that the glasses met the targeted values. The amount of SO 3 retained in the glasses after washing was relatively high, ranging from 1.6 to 2.6 weight percent (wt %). Measured SnO 2 concentrations were notably low in all of the study glasses. The composition of the wash solutions should be measured in future work to determine whether SnO 2 is present with the excess sulfate washed from the glass. Increases in batch size and the amount of sodium sulfate added did not have a measureable impact on the amount of sulfate retained in the glass, although this was tested for only a single glass composition. A batch size of 250 g and a sodium sulfate addition targeting 7 wt %, as recommended by PNNL, will be used in future experiments.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2010

FRIT DEVELOPMENT FOR SLUDGE BATCH 6

The Savannah River National Laboratory (SRNL) evaluated a large number of Sludge Batch 6 (SB6) composition projections to support frit optimization for SB6 vitrification at the Defense Waste Processing Facility (DWPF). The evaluations discussed in this report occurred over a period of about 4 months, and included about 40 composition projections, developed by both Savannah River Remediation (SRR) and SRNL. Paper study assessments were used to evaluate the sludge composition projections with arrays of potential frit compositions using the predictive models in the DWPF Product Composition Control System (PCCS). Both nominal sludge compositions and sludge compositions with anticipated compositional variation were considered. The model predictions were used to identify candidate frit compositions for each SB6 projection and to provide some guidance to SRR on washing and blending strategies for SB6 preparation. This report presents a chronological review of this process and summarizes the findings at each stage. Following initial feedback from this work, the number of washes in Tank 51 was reduced to increase the projected sodium concentration in SB6. Analyses of predicted frit performance before and after a potential decant of Tank 40 showed that the post-decant SB6 composition would be difficult to process with any frit composition and that this scenario should be avoided. Based on the most recent SB6 projections (February 2010 SB6 composition projections developed at SRNL using the measured SB6 qualification sample composition and the revised Tank Farm washing plan), Frit 418 appears to be viable for SB6 processing at a target waste loading of 36%. A Nominal Stage PCCS Measurement Acceptability Region (MAR) assessment gave projected operating windows of 25-41% waste loading, limited by predictions of nepheline crystallization. The projected operating window is reduced to 25-38% waste loading when anticipated compositional variation is considered, again limited by predictions of nepheline crystallization. Blend points between 62 and 40 inches of Sludge Batch 5 (SB5) heel in Tank 40 had no practical impact on the projected performance of Frit 418. This assessment is made from a paper study approach only and assumes that no decant of Tank 40 will occur during SB6 processing. A decant of Tank 40 would reduce the Na2O concentration in Tank 40 to a point where it would be very difficult to target a waste loading of 36% for SB6 with Frit 418. The performance of Frit 418 with SB6 is limited by predictions of nepheline crystallization, which is a durability limiting constraint. Alternatives to Frit 418 are available that can provide equivalent projected operating windows and are limited by process related constraints (i.e., liquidus temperature predictions) rather than durability limiting constraints. A separate memorandum has recently been issued that discusses the use of Frit 418 for SB6 vitrification.1 potential differences in melt rate among these alternative frits will be discussed in a forthcoming technical report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2011

TESTING OF THE SECOND GENERATION SPINTEK ROTARY FILTER -11357

The SpinTek rotary microfilter has been developed under the Department of Energy (DOE) Office of Environmental Management (EM) for the purpose of deployment in radioactive service in the DOE complex. The unit that was fabricated and tested is the second generation of the filter that incorporates recommended improvements from previous testing. The completion of this test satisfied a key milestone for the EM technology development program and technology readiness for deployment by Savannah River Remediation in the Small Column Ion Exchange and Sludge Washing processes at the Savannah River Site (SRS). The Savannah River National Laboratory (SRNL) contracted SpinTek Filtration to fabricate a full scale 25 disk rotary filter and perform a 1000 hour endurance test with a simulated SRS sludge. Over 1500 hours of operation have been completed with the filter. SpinTek Filtration fabricated a prototypic 25 disk rotary filter including updates to manufacturing tolerances, an updated design to the rotary joint, improved cooling to the bottom journal, decreases in disk and filter shaft hydraulic resistances. The filter disks were fabricated with 0.5 {micro} pore size, sintered-metal filter media manufactured by Pall Corporation (M050). After fabrication was complete, the filter passed acceptance tests demonstrating rejection of solids and clean water flux with a 50% improvement over the previous filters. Once the acceptance test was complete, a 1000 hour endurance test was initiated simulating a sludge washing process. The test used a simulated SRS Sludge Batch 6 recipe. The insoluble solids started at 5 wt% and were raised to 10 and 15 wt% insoluble solids to simulate the concentration of a large volume tank. The filter system was automated and set up for 24 hour unattended operation. To facilitate this, process control logic was written to operate the filter. During the development it was demonstrated that the method of starting and stopping the filter can affect the build up of filter cake on the disks and therefore the performance of the filter. The filter performed well with the simulant. Very little drop in production was noticed between the 5 and 10 wt% insoluble solids feed. Increasing to 15 wt% had a more pronounced impact due to the rheology of the feed. Acid cleaning was used to clean the filter disks in-situ and restore filtration rate to almost 90% of the initial clean disk rate. Eighty liters of 0.2 M nitric acid in conjunction with water rinses were used to clean the filter in less than 2 hours. Filter testing was completed after 1000 hours of operation were performed on the final filter assembly configuration. The total run time for the testing was over 1500 hours. At the end of the test, the sludge washing was performed successfully from approximately 5.6 M to less than 1 M sodium.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2013

Decontamination of Radioactive Cesium Released from Fukushima Daiichi Nuclear Power Plant - 13277

Peculiar binding of Cesium to the soil clay minerals remained the major obstacle for the immediate Cs-decontamination of soil and materials containing clay minerals like sludge. Experiments for the removal of Cesium from soil and ash samples from different materials were performed in the lab scale. For soil and sludge ash formed by the incineration of municipal sewage sludge, acid treatment at high temperature is effective while washing with water removed Cesium from ashes of plants or burnable garbage. Though total removal seems a difficult task, water-washing of wood-ash or garbage-ash at 40 deg. C removes >90% radiocesium, while >60% activity can be removed from soil and sludge-ash by acid washing at 95 deg. C. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Addressing Inherent Challenges to Chemical Relithiation of Cycled End‐of‐Life Cathode Materials

Recycling end‐of‐life (EOL) lithium‐ion batteries (LIBs) is important to retain valuable resources from critical materials present in EOL battery waste. Direct recycling methods offer an opportunity to recover intact valuable cathode materials with minimal re‐processing. An important step of the direct recycling process is relithiation which is used to restore lithium content to EOL cathode materials. However, little has been done to study how preprocessing steps such as washing or binder removal may affect relithiation methods in the direct recycling process. Here, the evolution of fluorine byproducts left over from preprocessing steps during a low‐temperature chemical redox mediator relithiation process is tracked. A facile washing step is presented as a solution for mediating adverse effects of surface contamination on the chemical relithiation performance. The structure, lithium content, and electrochemical performance of relithiated EOL NMC 622 material that underwent a pre‐relithiation washing step to remove fluorine byproducts is shown to match that of pristine NMC 622. In this work, it is showed that redox mediator relithiation as a part of a direct recycling process is a promising low energy method that can be applied to EOL material with inherent surface impurities if the proper pre‐relithiation processing steps are implemented.

25 ENERGY STORAGE↗

DOE OSTI2018

Novel Rapid Screening of Basic Immobilized Amine Sorbent/Catalyst Water Stability by a UV/Vis/Cu 2+ Technique

Abstract Time‐consuming thermogravimetric analysis (TGA) decomposition study is a typical practice to assess the stability of fresh and water‐treated basic immobilized amine sorbents (BIAS)/catalysts. This work presents a faster and more precise spectroscopic UV/Vis/Cu 2+ sorbent screening technique that quantifies aqueous amines washed from the BIAS by using UV‐active amine/Cu 2+ complexes. Six BIAS‐based catalysts, containing different amine species and a crosslinker within silica, were treated with ultrapure water and then analyzed for their CO 2 capture performance and amine leach resistance/stability by using TGA (catalysts, approximately 4 h) and UV/Vis/Cu 2+ techniques (wash solution, few minutes). A comparative analysis revealed that directly quantifying washed amines with UV/Vis/Cu 2+ is 9–127 times more precise than indirect testing of the sorbents by TGA. Similar trends in the H 2 O stability profiles of the catalysts [organic content retained values (OCR)] were reported by both analysis methods, allowing UV/Vis/Cu 2+ to replace TGA for quantifying unstable leached amines. The UV/Vis/Cu 2+ OCR results could be used to predict the CO 2 ‐capture stability profile of the sorbents, confirming the reliability of this technique to rapidly screen catalyst stability and performance.

Wilfong, Walter Christopher↗

DOE OSTI2016

Evolution of N-Coordinated Iron–Carbon (FeNC) Catalysts and Their Oxygen Reduction (ORR) Performance in Acidic Media at Various Stages of Catalyst Synthesis: An Attempt at Benchmarking

The objective of this study was to understand the role of iron and the heat treatment steps involved in nitrogen-coordinated iron-carbon (FeNC) catalyst synthesis. We have studied the oxygen reduction reaction (ORR) performance of these catalysts as they evolve from their most crude and inactive form to their most active form. Electrochemical half-cell and fuel cell tests suggest that the presence of Fe was crucial in these samples. The high-temperature heat treatment (once in argon and then in ammonia) at temperatures ≥950 °C were also critical in imparting these catalysts with their highest activity; however, significant loss of activity was observed with cycling and potential hold at 0.5 V for 100 h. In addition, acid-washing after the first or the second pyrolysis steps produced a marked decrease in ORR activity relative to their unwashed counterparts. We also report findings from our efforts towards benchmarking FeNC catalysts for oxygen reduction reaction electrocatalysis. Specifically, we focus on correlating the specific kinetic current (iK) at 0.75 V to electrochemically accessible surface area (EASA) and roughness factor (RF) determined from electrochemical double layer capacitance measurements. 57 Fe Mössbauer spectroscopy was employed to shed light into the nature of active sites in FeNC catalysts and provide insights into their deactivation behavior caused by acid-washing. The results suggest planar FeN 4 doublet (Fe 2+ , low spin) as an active site in these materials, which may be leached away in acid, explaining their decreased activity after acid washing. Results for characterization experiments using X-ray photoelectron spectroscopy, temperature programmed oxidation and X-ray absorption spectroscopy, superconducting quantum interference device magnetometry are also presented.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗