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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Evaluations of the Fates of Alkali Metals, Actinides, Mercury, and Iodine During DWPF Recycle Diversion

The fates of alkali metals, actinides, mercury, and iodine in the Defense Waste Processing Facility Recycle Diversion process (as currently conceptualized) have been evaluated through paper studies based on available knowledge of the chemistry, physical properties, solubility, and volatility of the various species involved. The effect of pH in the range from 9 to 13 has been discussed. Recommendations for additional studies to close technology gaps have been provided, many of which are contingent upon the results of pending testing and sample characterization efforts. There is uncertainty in the amounts of soluble actinides passing through the process filter, though the bulk of the actinides should be captured on the filter with the Recycle Collection Tank solids and the total amounts of actinides should be relatively low. The Recycle Collection Tank pH could impact the fraction of actinides reaching the evaporator, but the primary factors determining the actinide fate are expected to be the amount of CO 2 sorption from air sparging or, for certain actinides (such as plutonium), oxidation and/or sorption to MnO 2 solids from permanganate additions to destroy the glycolate anion. Process optimization could minimize the amounts of actinides passing the filter. Depending upon the levels of mercury observed in recycle stream samples and because of the volatility of mercury, the evaporator should be designed with the capability to remove dense mercury phases from the condensate to avoid exceeding ETP WAC limits. The facility design must be adequate to transfer dense mercury phases and testing to confirm mercury transfer is needed. Simulant containing mercury is recommended for both filtration and evaporation testing. OLI Modeling of the various recycle streams is recommended to provide insight on the fate of iodine. Iodine-spiked simulants are recommended for upcoming evaporation tests. The pro) ect should consider the likelihood and impact of NAS scale formation in the evaporators. Process optimization may be needed to minimize the accumulation of NAS scale and possibly the sorption of actinides in the evaporator. Actual waste testing of the Recycle Diversion filtration and evaporation should include the analysis of actinides, mercury, and iodine to determine their partitioning.

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

High Solids Performance Testing in a Scaled TSCR System

The Tank Side Cesium Removal (TSCR) project is a technology demonstration that will pretreat Hanford tank waste supernatant in support of the Direct Feed Low-Activity Waste (DFLAW) mission. The TSCR system employs two key separation technologies: dead-end filtration (DEF) and ion exchange (IX) using crystalline silicotitanate (CST) media. DEF will be used to remove undissolved solids from tank waste to protect the functionality of the IX columns and the IX system will remove Cs-137 from tank waste. The separation technologies (DEF and IX) used in TSCR are technically mature and have also been successfully deployed at the Savannah River site in a similar facility known as the Tank Closure Cesium Removal (TCCR) system. While testing with simulants and real waste has been successfully performed under conditions expected during the initial operation of TSCR, test data is absent for assessing off normal high solids loading that may be in the TSCR waste feed. Normal TSCR treatment operations are expected to handle wastes with solids content on the order of 200 ppm, and off normal solids loading could be much larger than the nominal level. The testing program described in this report was conducted to understand the consequence of operating the TSCR system at elevated solids loadings up to the high-solids limit of 15,000 ppm [i.e., 1.5-wt%] identified in the TSCR design basis. Although the system is not required to make throughput above the nominal solids loading, the testing was intended to provide important information related to potential off normal operations. At off normal levels near the high-solids limit, there are potential implications for TSCR performance in the areas of throughput, DEF pressure drop, filter backflush frequency, and IX column pressure drop. In addition, intrusion of solids into the IX column was postulated to impact the Cs-137 loading behavior by promoting channeling or flow maldistribution in the column; since the magnitude of the postulated effect was unknown, assessing it was also of interest. The testing was performed using representative waste simulants and a prototypic, integrated TSCR system designed and assembled specifically to conduct the high solids performance assessment. Overall, the scaled TSCR testing demonstrated that full-scale unit operations can succeed in fulfilling their processing objectives in the presence of solids up to 3,000 ppm, but there are potential performance challenges to filtration operations at solids loadings as low as ~500 ppm. The severity of the challenge is likely to be dependent on the type and size distribution of solids, of which the current testing only examined a single type and size distribution. To provide some flexibility for future full-scale operations, the results of the testing suggest two possible risk reduction strategies that can be implemented without any changes in TSCR design or configuration. One option would be to enact an administrative limit on the solids loading to protect TSCR from feeds that are likely to require a high DEF swap frequency. Another option is to permit operation of the DEFs at differential pressures greater than 2 psid before swapping filters. The selection of a higher differential pressure target is not anticipated to adversely impact DEF backflushing efficacy and would reduce both swap frequency and the amount of waste sent to AP-108.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
NASA NTRS2003

Development of a pilot system for converting sweet potato starch into glucose syrup

Sweet potato has been chosen as one of NASA's crops to support human beings in future space missions. One of the possible uses is to make syrup that can be used as a general sweetener. In this work a simple engineering system for converting sweet potato starch into glucose syrup was studied on a laboratory scale. The system comprises the following main units: a blender, continuous stirred tank reactor (CSTR), centrifugal and vacuum filters, deionization column and vacuum evaporator. The system was tested by carrying out conversion processes from fresh sweet potato roots. The roots were pealed, sliced, homogenized, heated and hydrolyzed by diastase of malt and Dextrozyme C (Novo Nordisk BioChem, North America, Inc.) enzymes in the CSTR. After hydrolysis the slurry was filtered, de-ionized and concentrated to get glucose syrup. The performance of the system was evaluated based on the quality of the conversion. The main factor was the level of reducing sugars except for the deionization where ash content and color were the main factors. Through careful control of the system units, good heating performance in the CSTR was obtained and the hydrolysis process attained sufficient conversion. The filtration process that incorporated the centrifuge was faster than when it was by-passed to the vacuum filter but losses in sugars were higher. Deionization removed more than 90% of the ash and reduced pigmentation, with probable insignificant losses in sugars during the deionization process. Recovery levels when the centrifuge was used and when it was by-passed could reach about 65% and 78%, respectively. These correspond to reducing sugar concentration of 259 and 310 mg/ml in 150-ml syrups from 300 g of sweet potatoes in each process. However, from concentration trials, syrups with volumes of 100 and 70 ml with the respective dextrose equivalence of 281 and 213 mg/ml were obtained. The syrups obtained were brownish in color and the process that employed centrifugal filtration gave a product with color that resembled the original color of the sweet potatoes. Further work is required to improve the overall system performance.

Non-NASA Center↗
NASA NTRS2016

Filter Media Tests Under Simulated Martian Atmospheric Conditions

Human exploration of Mars will require the optimal utilization of planetary resources. One of its abundant resources is the Martian atmosphere that can be harvested through filtration and chemical processes that purify and separate it into its gaseous and elemental constituents. Effective filtration needs to be part of the suite of resource utilization technologies. A unique testing platform is being used which provides the relevant operational and instrumental capabilities to test articles under the proper simulated Martian conditions. A series of tests were conducted to assess the performance of filter media. Light sheet imaging of the particle flow provided a means of detecting and quantifying particle concentrations to determine capturing efficiencies. The media's efficiency was also evaluated by gravimetric means through a by-layer filter media configuration. These tests will help to establish techniques and methods for measuring capturing efficiency and arrestance of conventional fibrous filter media. This paper will describe initial test results on different filter media.

Martian Atmosphere↗
NASA NTRS2016

Filter Efficiency and Leak Testing of Returned ISS Bacterial Filter Elements After 2.5 Years of Continuous Operation

The atmosphere revitalization equipment aboard the International Space Station (ISS) and future deep space exploration vehicles provides the vital functions of maintaining a habitable environment for the crew as well as protecting the hardware from fouling by suspended particulate matter. Providing these functions are challenging in pressurized spacecraft cabins because no outside air ventilation is possible and a larger particulate load is imposed on the filtration system due to lack of sedimentation in reduced gravity conditions. The ISS Environmental Control and Life Support (ECLS) system architecture in the U.S. Segment uses a distributed particulate filtration approach consisting of traditional High-Efficiency Particulate Adsorption (HEPA) filters deployed at multiple locations in each module. These filters are referred to as Bacteria Filter Elements (BFEs). As more experience has been gained with ISS operations, the BFE service life, which was initially one year, has been extended to two to five years, dependent on the location in the U.S. Segment. In previous work we developed a test facility and test protocol for leak testing the ISS BFEs. For this work, we present results of leak testing a sample set of returned BFEs with a service life of 2.5 years, along with particulate removal efficiency and pressure drop measurements. The results can potentially be utilized by the ISS Program to ascertain whether the present replacement interval can be maintained or extended to balance the on-ground filter inventory with extension of the lifetime of ISS to 2024. These results can also provide meaningful guidance for particulate filter designs under consideration for future deep space exploration missions.

ISS Air Quality↗
NASA NTRS2017

International Space Station (ISS) Bacterial Filter Elements (BFEs): Filter Efficiency and Pressure Testing of Returned Units

The air revitalization system aboard the International Space Station (ISS) provides the vital function of maintaining a clean cabin environment for the crew and the hardware. This becomes a serious challenge in pressurized space compartments since no outside air ventilation is possible, and a larger particulate load is imposed on the filtration system due to lack of sedimentation due to the microgravity environment in Low Earth Orbit (LEO). The ISS Environmental Control and Life Support (ECLS) system architecture in the U.S. Segment uses a distributed particulate filtration approach consisting of traditional High-Efficiency Particulate Adsorption (HEPA) media filters deployed at multiple locations in each U.S. Segment module; these filters are referred to as Bacterial Filter Elements, or BFEs. These filters see a replacement interval, as part of maintenance, of 2-5 years dependent on location in the ISS. In this work, we present particulate removal efficiency, pressure drop, and leak test results for a sample set of 8 BFEs returned from the ISS after filter replacement. The results can potentially be utilized by the ISS Program to ascertain whether the present replacement interval can be maintained or extended to balance the on-ground filter inventory with extension of the lifetime of ISS beyond 2024. These results can also provide meaningful guidance for particulate filter designs under consideration for future deep space exploration missions.

Filtration↗
NASA NTRS2017

Filter Efficiency and Pressure Testing of Returned ISS Bacterial Filter Elements (BFEs)

The air quality control equipment aboard the International Space Station (ISS) and future deep space exploration vehicles provide the vital function of maintaining a clean cabin environment for the crew and the hardware. This becomes a serious challenge in pressurized space compartments since no outside air ventilation is possible, and a larger particulate load is imposed on the filtration system due to lack of sedimentation. The ISS Environmental Control and Life Support (ECLS) system architecture in the U.S. Segment uses a distributed particulate filtration approach consisting of traditional High-Efficiency Particulate Air (HEPA) filters deployed at multiple locations in each U.S. Seg-ment module; these filters are referred to as Bacterial Filter Elements, or BFEs. In our previous work, we presented results of efficiency and pressure drop measurements for a sample set of two returned BFEs with a service life of 2.5 years. In this follow-on work, we present similar efficiency, pressure drop, and leak tests results for a larger sample set of six returned BFEs. The results of this work can aid the ISS Program in managing BFE logistics inventory through the stations planned lifetime as well as provide insight for managing filter element logistics for future exploration missions. These results also can provide meaningful guidance for particulate filter designs under consideration for future deep space exploration missions.

ISS Air Quality↗
NASA NTRS2017

International Space Station (ISS) Bacterial Filter Elements (BFEs): Filter Efficiency and Pressure Drop Testing of Returned Units

The air quality control equipment aboard the International Space Station (ISS) and future deep space exploration vehicles provide the vital function of maintaining a clean cabin environment for the crew and the hardware. This becomes a serious challenge in pressurized space compartments since no outside air ventilation is possible, and a larger particulate load is imposed on the filtration system due to lack of sedimentation. The ISS Environmental Control and Life Support (ECLS) system architecture in the U.S. Segment uses a distributed particulate filtration approach consisting of traditional High-Efficiency Particulate Air (HEPA) filters deployed at multiple locations in each U.S. Seg-ment module; these filters are referred to as Bacterial Filter Elements, or BFEs. In our previous work, we presented results of efficiency and pressure drop measurements for a sample set of two returned BFEs with a service life of 2.5 years. In this follow-on work, we present similar efficiency, pressure drop, and leak tests results for a larger sample set of six returned BFEs. The results of this work can aid the ISS Program in managing BFE logistics inventory through the stations planned lifetime as well as provide insight for managing filter element logistics for future exploration missions. These results also can provide meaningful guidance for particulate filter designs under consideration for future deep space exploration missions.

ISS Air Quality↗
DOE OSTI2015

Development and Optimization of a Flocculation Procedure for Improved Solid-Liquid Separation of Digested Biomass

One viable treatment method for conversion of lignocellulosic biomass to biofuels begins with saccharification (thermochemical pretreatment and enzymatic hydrolysis), followed by fermentation or catalytic upgrading to fuels such as ethanol, butanol, or other hydrocarbons. The post-hydrolysis slurry is typically 4-8 percent insoluble solids, predominantly consisting of lignin. Suspended solids are known to inhibit fermentation as well as poison catalysts and obstruct flow in catalyst beds. Thus a solid-liquid separation following enzymatic hydrolysis would be highly favorable for process economics, however the material is not easily separated by filtration or gravimetric methods. Use of a polyacrylamide flocculant to bind the suspended particles in a corn stover hydrolyzate slurry into larger flocs (1-2mm diameter) has been found to be extremely helpful in improving separation. Recent and ongoing research on novel pretreatment methods yields hydrolyzate material with diverse characteristics. Therefore, we need a thorough understanding of rapid and successful flocculation design in order to quickly achieve process design goals. In this study potential indicators of flocculation performance were investigated in order to develop a rapid analysis method for flocculation procedure in the context of a novel hydrolyzate material. Flocculation conditions were optimized on flocculant type and loading, pH, and mixing time. Filtration flux of the hydrolyzate slurry was improved 170-fold using a cationic polyacrylamide flocculant with a dosing of approximately 22 mg flocculant/g insoluble solids at an approximate pH of 3. With cake washing, sugar recovery exceeded 90 percent with asymptotic yield at 15 L wash water/kg insoluble solids.

09 BIOMASS FUELS↗
DOE OSTI2013

Results from Evaluation of Proposed ASME AG-1 Section FI Metal Media Filters - 13063

High efficiency particulate air (HEPA) filtration technology is commonly used in Department of Energy (DOE) facilities that require control of radioactive particulate matter (PM) emissions due to treatment or management of radioactive materials. Although HEPA technology typically makes use of glass fiber media, metal and ceramic media filters are also capable of filtering efficiencies beyond the required 99.97%. Sintered metal fiber filters are good candidates for use in DOE facilities due to their resistance to corrosive environments and resilience at high temperature and elevated levels of relative humidity. Their strength can protect them from high differential pressure or pressure spikes and allow for back pulse cleaning, extending filter lifetime. Use of these filters has the potential to reduce the cost of filtration in DOE facilities due to life cycle cost savings. ASME AG-1 section FI has not been approved due to a lack of protocols and performance criteria for qualifying section FI filters. The Institute for Clean Energy Technology (ICET) with the aid of the FI project team has developed a Section FI test stand and test plan capable of assisting in the qualification ASME AG-1 section FI filters. Testing done at ICET using the FI test stand evaluates resistance to rated air flow, test aerosol penetration and resistance to heated air of the section FI filters. Data collected during this testing consists of temperature, relative humidity, differential pressure, flow rate, upstream particle concentration, and downstream particle concentration. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2017

Hydrophobic Filter Material for Nuclear Material Transportation and Storage Containers - 17518

Los Alamos National Laboratory has begun development of hydrophobic or super-hydrophobic inorganic filter materials that resist water ingress after exposure to radiation and/or elevated temperature. Filters that are currently available depend on carbon composites and/or organic polymers for their water resistant/hydrophobic properties to minimize water ingress. However, facility and transportation accident scenarios often include fire, impact and subsequent water spray or flooding conditions. A purely inorganic hydrophobic filter material could have enhanced resistance to fire and radiation damage, and continue to minimize water ingress after such an accident. Such filters could broaden the use of filtered containers in the transportation and storage of nuclear materials, and could have broader implications in other industrial applications. The goal is to create a porous inorganic material with hydrophobic properties that maintains or exceeds the current performance criteria for particulate filtration efficiency, pressure differential, air flow and hydrogen diffusion. The materials developed in this project show promise in evaluations for use as enhancements to the SAVY 4000 nuclear storage container that is becoming widely used around the DOE complex. Preliminary results indicate that the treated filters provide resistance to a water column pressure test and have filtration efficiencies and air flow pressure drops that meet the current performance criteria. There are various treatment options being tested to help determine the best path forward. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Operating experience in the treatment and storage of LLW in Turkey - 15010

Treatment and storage of low-level radioactive wastes (LLW) are being carried out in Radioactive Waste Management Unit (RWMU) at Cekmece Nuclear Research and Training Center (CNRTC) in Istanbul. The wastes are generated from nuclear research and nuclear applications mainly in medicine, biology, ng to these specifications, LLW are classified as exempt waste, very low level waste (VLLW) etc. Decay storage is applied at a designated area for short lived radionuclide. Long lived spent radioactive sources are immobilized in retrievable packages. Generally liquid radioactive wastes are decontaminated by filtration or chemical precipitation. The radioactive sludge or filtration media from liquid waste processing is solidified using cementation. Solid waste is compacted into drums for size reduction. TENORM wastes and contaminated metal wastes are handled for decontamination and size reduction. Then these types of waste are placed in 20 ton bulk containers for long term storage. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

WIPP Safety Significant Confinement Ventilation System Design - 18490

A large exhaust ventilation system has been designed to provide continuous HEPA filtration of the exhaust from the Waste Isolation Pilot Plant (WIPP) underground while meeting the demand for expanded waste emplacement and mining operations over the next 40 years. The WIPP Safety Significant Confinement Ventilation System (SSCVS) design provides secondary confinement to mitigate the consequences of a postulated radiological release in the underground. The SSCVS design specifically addresses the radiological incident that occurred in 2014 by providing Safety Significant secondary confinement and continuous HEPA filtration over a wide range of operating and environmental conditions. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2018

Radioactive Test Platform Demonstrating the Direct Feed Low-Activity Waste Process at Hanford - 18628

The Hanford Site is implementing a phased process for treating liquid legacy radioactive waste. The process is called the Direct Feed Low-Activity Waste process (DFLAW). The DFLAW includes a filtration and ion-exchange unit in the Low-Activity Waste Pretreatment System (LAWPS) that removes solids and cesium. This pretreat feed is then sent to a vitrification facility where glass-forming solids are added and the waste is turned into glass in a melter. The melter off-gas liquid condensate is evaporated in the Effluent Management Facility (EMF), with the concentrate recycled back into the feed. A laboratory-scale test platform has been built to test various aspects of the DFLAW process using samples of actual radioactive waste. The current platform represents four of the major unit operations: filtration, ion-exchange, vitrification, and off-gas condensation. A lab scale EMF is being designed to supplement the current platform. The platform is expandable to add any or all unit operations. The radioactive test platform has three missions. The first is simply to demonstrate the DFLAW process with real waste. A second objective is to address flowsheet gaps and opportunities, some of which require testing with real waste. Some gaps and opportunities include addressing the fate of mercury in the flowsheet, evaluating salt and aluminum precipitation, and proving new glass formulations with real waste. A third objective of the radioactive test platform is to demonstrate or evaluate future operations and alternative flowsheets. Some of the future operations evaluated will be the life expectancy of the resin in real waste, resin sampling, evaluation of how waste affects melter throughput, and grouting various primary and secondary waste streams. The radioactive test platform is therefore a crucial tool for verifying and optimizing the DFLAW flowsheet at Hanford with real waste. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Understanding and Controlling Cesium Loading on Crystalline Silicotitanate - 19601

Savannah River Remediation (SRR) contracted with Westinghouse Electric Corporation (WEC), Columbia Energy and Environmental Services (CEES), to build and deliver a modular ion exchange process that will be used to remove radioactive cesium from dissolved salt solution contained in Tank 10 at the Savannah River Site (SRS). The resulting decontaminated salt solution will be sent to Tank 11 and then to Tank 50 for final disposition in grout at the Saltstone facility. At the end of processing, the loaded ion exchange (IX) columns are drained, rinsed, and dried. The IX columns are removed from the modular unit and stored at Interim Safe Storage (ISS). This ion exchange process is called the Tank Closure Cesium Removal (TCCR) system. The TCCR system consists of several unit operations and process monitoring capability housed within three modular units. The first modular unit contains the process control computer, the second modular unit contains the main process equipment (two prefilters, four IX columns, and resin trap (post filtration)), and the third modular unit is the ventilation system. The main unit operations of the TCCR system are filtration, ion exchange, and ventilation. The ion exchange media utilized is a form of inorganic Crystalline Silicotitanate (CST), IONSIV{sup TM} R9120-B supplied by UOP Honeywell. CST has a high selectivity for cesium (Cs) and has some affinity for other Group IA alkali metals on the periodic chart (hydrogen, lithium, sodium, potassium, rubidium, and francium). CST has also been shown to have affinity for strontium and actinides. Cesium loading on the CST is dependent on many factors including chemical composition (cations and anions), temperature, and pH of the salt solution. The actual amount of Cs loaded onto an IX column is dependent on the factors above along with the salt solution volume fed to the IX column. Because of CST's high selectivity for Cs, the Cs-137 equilibrium loading can contribute enough decay heat to result in an ion exchange column boiling event under no flow conditions in the IX column. The boiling event under no flow is a safety concern that must be prevented from occurring. To prevent boiling of the column under no flow conditions, the Cs-137 equilibrium loading must be determined and understood. Several methodologies were evaluated for performing the Cs-137 equilibrium loading determination for CST. After review of available research and development (R and D), batch equilibrium contact test data, and Zheng Anthony Miller (ZAM) model predictions for the salt solution chemistry in Tank 10, a methodology for determining the Cs-137 equilibrium loading on CST was selected. The methodology selected involves an in-tank batch equilibrium contact test performed in duplicate that considers additional corrections to account for anticipated operational evolutions. The in-tank batch equilibrium contact test utilizes ∼0.1 grams of CST secured in a slotted sample vial. The slotted sample vial design allows for salt solution to be in contact with the CST. The slotted sample vials containing the CST are submerged in Tank 10 and exposed to the salt solution for ten days. After ten days, the samples are retrieved and sent to the Savannah River National Laboratory (SRNL) for analysis of the Cs-137 equilibrium loading. Additional corrections are then made to the Cs-137 results to account for anticipated operational evolutions. Anticipated operational evolutions include external additions (water/caustic) to Tank 10 that result in a change to its chemical composition, tank temperature effects, departures from the laboratory testing (mixed vs. stagnant tank conditions), and IX column flushes. A description of the methodologies considered, feasibility of methodology deployment, and the down select process (benefits vs. risks) is discussed in this paper. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2019

Mercury Speciation via Direct Mercury Analyzer

Mercury has no known biological role, but is present in every living thing and widespread in the environment. As mercury enters an aqueous system, it is subject to methylation or demethylation. Methylmercury selectively partitions into biota and biomagnifies through the food chain. Nearly all methylmercury exposures in the U.S. occur through eating fish and shellfish that contain higher levels of methylmercury. Methyl mercury and other organomercury compounds are more toxic than inorganic mercury. Thus, monitoring and understanding mercury speciation are key to effective environmental management. It is particularly important to be able to separate and measure bioaccumulative-toxic species of mercury such as methyl mercury. We are developing a protocol for utilizing the Direct Mercury Analyzer (DMA-80) for mercury speciation of water samples and to monitor methylmercury (meHg). Objectives: - Advance the understanding of the performance of the direct mercury analysis (DMA) under a range of DOE relevant water chemistry conditions to quantify total mercury: - Demonstrate the applicability of DMA to analysis of typical DOE high level liquid 'tank' waste samples using nonradioactive simulants; Test innovative sorbents to extend the range of the direct mercury analyzer to environmental concentration levels. - Perform scoping tests to demonstrate proof of principle for the chemical reduction amalgamation modular microcolumns for mercury speciation: Examine various microcolumn configurations and document speciation performance for typical DOE high level liquid 'tank' waste samples using nonradioactive simulants; Perform tests to examine extending the speciation paradigm to environmental concentration levels. General Method: all samples analyzed using a direct mercury analyzer (DMA 80) which automates the following steps: 1) pyrolysis to release the mercury, 2) catalysis to convert all mercury to elemental, 3) amalgamation to trap the mercury, 4) desorption to release the mercury as a pulse and 5) spectroscopy to detect the mercury.. Instrument analyzes all mercury species in solids and liquids. The DMA 'eliminates' sample preparation, reduces labor, decreases waste, and results in more practical and cost effective methods. To test the performance of the DMA for DOE relevant conditions, we analyzed samples representative of at high (mg/L) tank waste concentrations in water and in diluted tank waste simulant and analyzed samples representative of environmental (ng/L levels) in water. High concentration samples were analyzed directly in the instrument. Low concentration samples were analyzed by concentrating the mercury onto sorbents such as silica thiol or a mixture of silica thiol and copper. The concentration was performed using microcolumns and placing the columns into the DMA (see below) or by mixing the sorbent into the bulk sample and then filtering ad analyzing the filter in the DMA. Speciation Methods: The speciation tests were based on the selective reduction of inorganic mercury ions - Hg{sup (+} {sup or} {sup 2+)} - to elemental mercury - Hg(0). The elemental mercury is then trapped by amalgamation into the metal. These reactions do not impact methyl mercury allowing for separation. All reactions were performed using powdered elemental copper. To demonstrate proof-of-principle for the selective collection of inorganic mercury, samples were exposed to different amounts of powdered copper (and a control with no copper). This was done using microcolumns and a vacuum box. The columns were placed directly on the DMA for analysis. All materials and conditions were tested using solutions of both inorganic mercury and methyl mercury and all trials were in triplicate. Results and Observations: Validated DMA for high concentration Hg samples such as DOE tank waste: - Liquid inHg - samples were stable on autosampler carousel and results were accurate; - Liquid meHg - samples required a stabilizer. Si-Thiol (0.02 g) in the sample boat generated reliable meHg results. Stabilizer can be added for routine operations. Successful 'proof of principal' in extending DMA range to near environmental levels - using both microcolumns and filtration; - Filtration - Adding Si-Thiol (0.5 g) to sample extracted both inHg and meHg and preserved sample. Handling filters was labor intensive. - Microcolumns - best performance using a combination of copper and Si-Thiol - columns clogged and flowed slowly in some cases; - Practical limit may be in the range of 1 to 5 ng/L due to blanks; - Path Forward - Test additional packing materials and methods to improve flow and consistency, and approaches to minimize blanks. Successful 'proof of principal' for Hg speciation using chemical reduction and amalgamation; - Copper microcolumns (0.5 g Cu) selectively trapped inHg for high concentration mercury samples; - Copper microcolumns (0.5 g Cu selectively trapped inHg for large volume samples at environmental concentrations; - Some sorption of me Hg so that separations not quantitative; - Path Forward - test additional packing materials and alternate eluents to better trap inHg and minimize meHg retention in column.

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

Alternative Treatment of Defense Waste Processing Facility Recycle via Reuse of Existing Liquid Waste Facilities - 20097

The Defense Waste Processing Facility (DWPF) at Savannah River Site (SRS) has been immobilizing high level waste since 1996. The chemical process within DWPF generates a large volume of condensate, which is recycled to the SRS H-Area Tank Farm. The recycle stream includes a small quantity of sludge solids, as well as soluble cesium that is volatilized during melter operation. The recycle waste is currently received into a large, underground waste tank that separates insoluble solids via decanting. The supernate is treated by an evaporator with a concentrate stream that is stored for future processing. The evaporator overheads are collected and sent to the Effluent Treatment Project (ETP) for final polishing and testing prior to discharge to local surface water. Recycle storage and treatment as described above complicates the overall mission within the tank farms, which are primarily engaged in waste retrieval and preparation activities that support sludge and salt disposition, as well as tank characterization and closure. The need to devote a portion of available storage space to recycle treatment limits operational flexibility, and ultimately the DWPF recycle stream must be diverted to fully close all the SRS waste tanks. An alternative treatment process is being explored to decouple the recycle stream from the tank farm. The proposed treatment process will accomplish solids separation via crossflow filtration and will utilize a wiped film evaporator to volume-reduce the filtrate stream. Evaporator overheads will continue to be further processed in ETP while the solids stream and evaporator concentrate stream will be returned for reprocessing with the DWPF and Salt Waste Processing Facility (SWPF). This process will utilize existing facilities within DWPF and the tank farm that were previously dedicated to Interim Salt Disposition (ISD), but no longer have an identified mission with the startup of SWPF. The reuse of these facilities will remove several constraints from the current Liquid Waste (LW) System Plan without expanding the current footprint of Department of Energy Environmental Management (EM) infrastructure within LW. (authors)

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

Proposed Analytical Methods for Determining Filter Media Properties

High Efficiency Particulate Air (HEPA) filters, commonly used in nuclear filtration applications, are an integral part of the waste management processes in nuclear plants. HEPA filters are 99.97% efficient filtration devices characterized by their high resistance to air flow, or pressure drop. From theoretical models, the initial pressure drop across a clean filter is proven to be a function of the filter media fiber diameters and porosity of the media. These filter properties are relatively difficult to obtain with traditional manual methods; therefore, there is a need to develop analytical methods to find the fiber diameter and porosity to determine the pressure drop. Typically, these values can be found by substituting a calculated representative value based upon measured values, such as equivalent fiber diameter based upon a clean pressure drop. However, these values may also be directly recorded and measured by incorporating Scanning Electron Microscope (SEM) image analysis and other measurement methods to analyze the filter media and determine its physical properties without the need for media testing. DiameterJ, an open source Java plug-in, used with ImageJ, can process images of filter media taken by an SEM to find statistical data such as mean fiber diameter and porosity. To produce the raw data, SEM images of two filter media type samples are taken and segmented in DiameterJ using the traditional and statistical region merging segmentation algorithms. Manual segmentation is necessary after the initial segmentation by the algorithms as the images tend to be too complex for the algorithms to output with the necessary accuracy. However, complications exist in the manual segmentation process as these methods can be time intensive and prone to the individual bias of the user. This in turn can skew the final mean fiber diameter result, and lead to either an over or under prediction of the pressure drop. It was also discovered that the porosity data produced by DiameterJ is inaccurate, as the SEM analyzes the three-dimensional filter media by projecting its geometry onto a plane and analyzing it as a two-dimensional binary image. Thus, the porosity is artificially inflated through the segmentation process, rendering this result incorrect. Alternatively, density determination, gravimetric analysis, and thickness testing of the filter media is collectively used to determine the filter fiber porosity. Together, the SEM image analysis and analytical lab methods produce results through direct measurements which allow for the prediction of the initial pressure drop from clean filter media without the need for prior media testing to collect pressure data. By improving upon this proposed analytical method in the future, there is potential to streamline the process of finding these filter properties into a more direct methodology for determining the pressure drop across HEPA filters.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗