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At least 1,621 records · Page 90

Geothermometry Mapping of Deep Hydrothermal Reservoirs in Southeastern Idaho: Final Report

The Eastern Snake River Plain (ESRP) in southern Idaho is a region of high heat flow. Sustained volcanic activities in the wake of the passage of Yellowstone Hotspot have turned this region into an area with great potential for geothermal resources. Numerous hot springs with temperatures up to 75 ºC are scattered along the margins of the plain. Similarly, several hot-water producing wells and few hot springs are also present within the plain. The geothermal reservoirs in the area are likely to be hosted at depth in the felsic volcanic rocks underneath the thick sequences of basalts within the plain and the Paleozoic rocks underneath both basalts and felsic volcanic rocks along the margins. The heat source to these geothermal resources is thought to be the mid-crustal sill complex which sustains high heat flow in the ESRP. Several thermal anomaly areas are believed to be associated with the local thermal perturbation because of the presence of favorable structural settings. However, it is hypothesized that the pervasive presence of an overlying groundwater aquifer in the region effectively masks thermal signatures of deep-seated geothermal resources. The dilution of deeper thermal water and re-equilibration at lower temperatures are significant challenges for the evaluation of potential resource areas in the ESRP. To address this issue, this project, led by the Idaho National Laboratory (INL), aimed at applying advanced geothermometry tools including temperature-dependent mineral and isotopic equilibria with mixing models that account for processes such as boiling and dilution with shallow groundwater that could affect calculated temperatures of underlying deep thermal waters. Over the past several years, we collected approximately 100 water samples from springs/wells for chemical analysis as well as assembled existing water chemistry data from literature. We applied several geothermometric and geochemical modeling tools to the compositions of ESRP water samples. Geothermometric calculations based on principle of multicomponent equilibrium geothermometry with inverse geochemical modeling capability (e.g., Reservoir Temperature Estimator, RTEst) have been useful for evaluation of reservoir temperatures. Similarly, sulfate-water oxygen isotope geothermometry was also applied to several samples in tandem with RTEst. In summary, geothermometric calculations of ESRP thermal water samples indicated numerous potential geothermal areas with elevated reservoir temperatures. Specifically, areas around southern/southwestern side of the Mount Bennet Hills and within the Camas Prairie in the southwestern portion of the ESRP suggest temperatures 140-190 °C. In the northern portion of the ESRP, Lidy Hot Springs, Ashton, Newdale, and areas east of Idaho Falls have expected reservoir temperature ?140 °C. In the southern ERSP, areas near Buhl and Twin Falls are found to have elevated temperatures as high as 160 °C. These areas are likely to host potentially economic geothermal resources; however, further detailed study is warranted to each site to evaluate hydrothermal suitability for economic use.

58 GEOSCIENCES↗

Candidate Low-Temperature Glass Waste Forms for Technetium-99 Recovered from Hanford Effluent Management Facility Evaporator Concentrate

Alternative treatment and disposition options may exist for technetium-99 (99Tc) in secondary liquid waste from the Hanford Direct-Feed Low-Activity Waste (DFLAW) process. One approach includes development of an alternate glass waste form that is suitable for on-site disposition of technetium, including salts and other species recovered by ion exchange or precipitation from the EMF evaporator concentrate. By recovering the Tc content from the stream, and not recycling the treated concentrate, the DFLAW process can potentially be operated in a more efficient manner that lowers the cost to the Department of Energy. This report provides a survey of candidate glass formulations and glass-making processes that can potentially incorporate technetium at temperatures <700 °C to avoid volatilization. Three candidate technetium feed streams are considered: (1) dilute sodium pertechnetate loaded on a non-elutable ion exchange resin; (2) dilute sodium-bearing aqueous eluent from ion exchange recovery of pertechnetate, or (3) technetium(IV) oxide precipitate containing Sn and Cr solids in an aqueous slurry. From the technical literature, promising candidate glasses are identified based on their processing temperatures and chemical durability data. The suitability and technical risk of three low-temperature glass processing routes (vitrification, encapsulation by sintering into a glass composite material, and sol-gel chemical condensation) for the three waste streams was assessed, based on available low-temperature glass data. For a subset of candidate glasses, their long-term thermodynamic behavior with exposure to water and oxygen was modeled using Geochemist’s Workbench, with and without addition of reducing stannous ion. For further evaluation and development, encapsulation of precipitated TcO2/Sn/Cr in a glass composite material based on lead-free sealing glasses is recommended as a high priority. Vitrification of pertechnetate in aqueous anion exchange eluent solution using a high lead content borate glass, or other low melting glass is also recommended for further evaluation and development. Additional laboratory studies of phase behavior and chemical durability of low-temperature glasses is also recommended to provide risk mitigation if one of the primary development paths proves infeasible. This report is a deliverable for the task “Candidate Low-T Glass Waste Forms for EMF Bottoms On-Site Disposition Alternative Option.”

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Gasoline Combustion Fundamentals DOE FY17 Report

Advanced automotive gasoline engines that leverage a combination of reduced heat transfer, throttling, and mechanical losses; shorter combustion durations; and higher compression and mixture specific heat ratios are needed to meet aggressive DOE VTP fuel economy and pollutant emission targets. Central challenges include poor combustion stability at low-power conditions when large amounts of charge dilution are introduced and high sensitivity of conventional inductive coil ignition systems to elevated charge motion and density for boosted high-load operation. For conventional spark ignited operation, novel low-temperature plasma (LTP) or pre-chamber based ignition systems can improve dilution tolerances while maintaining good performance characteristics at elevated charge densities. Moreover, these igniters can improve the control of advanced compression ignition (ACI) strategies for gasoline at low to moderate loads. The overarching research objective of the Gasoline Combustion Fundamentals project is to investigate phenomenological aspects related to enhanced ignition. The objective is accomplished through targeted experiments performed in a single-cylinder optically accessible research engine or an in-house developed optically accessible spark calorimeter (OASC). In situ optical diagnostics and ex situ gas sampling measurements are performed to elucidate important details of ignition and combustion processes. Measurements are further used to develop and validate complementary high-fidelity ignition simulations. The primary project audience is automotive manufacturers, Tier 1 suppliers, and technology startups—close cooperation has resulted in the development and execution of project objectives that address crucial mid- to long-range research challenges.

33 ADVANCED PROPULSION SYSTEMS↗

Analyzing Solutions High in Total Dissolved Solids for Rare Earth Elements (REEs) Using Cation Exchange and Online Pre-Concentration with the seaFAST2 Unit; NETL-TRS-7-2017; NETL Technical Report Series; U.S. Department of Energy, National Energy Technology Laboratory: Albany, OR, 2017; p 32

The accurate quantification of the rare earth element (REE) dissolved concentrations in natural waters are often inhibited by their low abundances in relation to other dissolved constituents such as alkali, alkaline earth elements, and dissolved solids. The high abundance of these constituents can suppress the overall analytical signal as well as create isobaric interferences on the REEs during analysis. Waters associated with natural gas operations on black shale plays are characterized by high salinities and high total dissolved solids (TDS) contents >150,000 mg/L. Methods used to isolate and quantify dissolved REEs in seawater were adapted in order to develop the capability of analyzing REEs in waters that are high in TDS. First, a synthetic fluid based on geochemical modelling of natural brine formation fluids was created within the Marcellus black shale with a TDS loading of 153,000 mg/L. To this solution, 1,000 ng/mL of REE standards was added based on preliminary analyses of experimental fluids reacted at high pressure and temperature with Marcellus black shale. These synthetic fluids were then run at three different dilution levels of 10, 100, and 1,000–fold dilutions through cation exchange columns using AG50-X8 exchange resin from Eichrom Industries. The eluent from the cation columns were then sent through a seaFAST2 unit directly connected to an inductively coupled plasma mass spectrometer (ICP-MS) to analyze the REEs. Percent recoveries of the REEs ranged from 80–110% and fell within error for the external reference standard used and no signal suppression or isobaric interferences on the REEs were observed. These results demonstrate that a combined use of cation exchange columns and seaFAST2 instrumentation are effective in accurately quantifying the dissolved REEs in fluids that are >150,000 mg/L in TDS and have Ba:Eu ratios in excess of 380,000.

03 NATURAL GAS↗

Tests of a High Temperature Sample Conditioner for the Waste Treatment Plant LV-S2, LV-S3, HV-S3A and HV-S3B Exhaust Systems

Tests were performed to evaluate a sample conditioning unit for stack monitoring at Hanford Tank Waste Treatment and Immobilization Plant (WTP) exhaust stacks with elevated air temperatures. The LV-S2, LV-S3, HV-S3A and HV-S3B exhaust stacks are expected to have elevated air temperature and dew point. At these emission points, exhaust temperatures are too high to deliver the air sample directly to the required stack monitoring equipment. As a result, a sample conditioning system is considered to cool and dry the air prior to its delivery to the stack monitoring system. The method proposed for the sample conditioning is a dilution system that will introduce cooler, dry air to the air sample stream. This method of sample conditioning is meant to reduce the sample temperature while avoiding condensation of moisture in the sample stream. An additional constraint is that the ANSI/HPS N13.1-1999 standard states that at least 50% of the 10 μm aerodynamic diameter (AD) particles present in the stack free stream must be delivered to the sample collector. In other words, depositional loss of particles should be limited to 50% in the sampling, transport, and conditioning systems. Based on estimates of particle penetration through the LV-S3 sampling system, the diluter should perform with about 80% penetration or better to ensure that the total sampling system passes the 50% or greater penetration criterion.

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A measurement of the proton’s spin structure function g2 at low Q2

JLab E08-027, a measurement of g2p and the longitudinal-transverse (LT) spin polarizability, successfully collected data from March to May, 2012. Nucleon spin structure study has been an active research area, which has attracted a very large effort from both experimentalists and theorists. The spin structure study for the last 2 decades has provided us with many exciting and often surprising results. Recently, new precision results in the low-to-intermediate momentum transfer Q2 region from JLab have provided extensive information on the nucleon structure in the confinement region and the transition region between asymptotic free to confinement. In particular, the extensive comparisons of experimental results with Chiral Perturbation Theory (the effective theory of QCD at low energy) calculations show general good agreements, but strong disagreement in the case of the neutron LT spin polarizability. This experiment completed the measurements of gp2 and the LT spin polarizability on the proton in the low-to-intermediate Q2 region. The experiment used a polarized proton (NH3) target for the first time in Hall A. Scattered electrons were detected by a pair of Hall A high resolution spectrometer (HRS) with a pair of septum magnets. To avoid too much depolarization of the target, beam current was limited to 50-100 nA during the experiment. Since the existing beam current monitors (BCMs), beam position monitors (BPMs) and calibration methods did not work at such a low current range, new BPM and BCM receivers were designed and used for current condition. A pair of super-harps and a tungsten calorimeter were installed to calibrate the BPMs and BCMs. To compensate for the effect of the 2.5/5T transverse magnet field, two chicane dipole magnets were installed. A pair of slow rasters were installed for the first time in Hall A, combining with a pair of fast raster. The standard Hall A DAQ system and the improved high resolution DAQ system were used to record the detector information and the helicity dependent beam information, respectively. In order to achieve the required accuracy of the beam position and angle and reconstruct them event by event at the target location, the data of the BPMs and harps were carefully analyzed. The final uncertainty of BCM after the calibration using the tungsten calorimeter is below 1%, which is important for the asymmetry extraction. Before the acceptance and the dilution factor are available, the models from fitting to the world data were used instead to extract the unpolarized cross section and the dilution factor. The longitudinal and transverse physics asymmetries were extracted and compared with the model, with the study of the radiative correction. The preliminary g1 and g2 results were then extracted using the measured asymmetry and the model.

Zhu, Pengjia↗

Techno-economic Analysis of Advanced Zeolite Membranes for the Concentration of Tritiated Water

This report describes the techno-economic analysis of advanced molecular sieve zeolite membranes to separate and concentrate tritiated water (HTO) from dilute HTO-bearing aqueous streams. In the first phase of this effort, several monovalent and divalent cation-exchanged silicoalumino phosphate (SAPO- 34) molecular sieve zeolite membranes were synthesized on disk supports and characterized with gas and vapor permeation measurements. In the second phase, Linde Type A (LTA) zeolite membranes were synthesized on disk and tubular supports. The pervaporation process performance was evaluated for the separation and concentration of tritiated water. Techno-economic analysis (TEA) on SAPO-34 and LTA membrane based technologies was completed. However, compared to the SAPO-34 membranes, LTA zeolite membrane performance both with respect to separation factor and permeance was superior and encouraging. LTA zeolite membranes were selected as the preferred option for comparison with the Combined Electrolysis and Catalyst Exchange (CECE) process for the concentration of tritiated water from dilute HTO-bearing aqueous solutions. It is estimated that the total energy cost to process 10 L/min of tritiated water for the membrane cascade system is substantially lower compared to the CECE process. A preliminary capital cost estimate for the membrane based system and the CECE process is also reported.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Brazing Dissimilar Metals with a Novel Composite Foil

Reactive brazing is a novel technique in the joining industry that uses reactive materials to produce substantial amounts of heat locally to join components. In this project, we created mechanically processed dilute thermite foils (Redox Foils) that upon ignition selfpropagate to produce molten metal capable of joining dissimilar metal combinations. Due to the transient nature of the reaction, there is limited thermal damage to the base materials. Also, novel component combinations, that cannot be joined via tradition furnace brazing (such as magnesium alloys to steel), can be produced. Redox Foils are produced by mechanically processing and consolidating constituent powders. By adjusting the fabrication pathway and chemistry, the reaction products can be tailored to join specific material combinations. In addition to producing mechanically processed foils, we produce vapor processed foils with controlled microstructures to understand some of the mechanisms of the reaction. Over the course of the program, we worked to identify and enhance the properties of the Redox Foils so that they could produce strong braze bonds of dissimilar metals (steel, Al, and Mg alloys). In a first step, the reactivity of the powders, from which the foils were made, was enhanced by ball milling Al and metal oxide powders before consolidation. In a second step, Redox Foils were made by physical vapor deposition to identify what level of dilution is needed to prevent the formation of Cu vapor during the reaction of the Redox Foils. In a third step, we incorporated diluent powders within the milling process to improve homogeneity within the final foils. In addition, finite element model simulations of heat transfer were also combined with detailed microstructure studies to identify what level of homogeneity is needed to avoid the generation of Cu vapor. Lastly, we include Ag powders as a diluent to form a lower melting temperature braze. Unfortunately, none of these steps led to Redox Foils that could produce bonds with shear strengths greater than 10 MPa. The generation of oxygen vapor appears to be generating porous bond lines that are still relatively week. To circumvent this vapor generation, we investigated Ti:2B reactive scaffolds that provide a heated framework to enhance braze flow and minimize porosity. However, BM Ti:2B powders suffered ~8% mass loss due to surface adsorbed water resulting in porous and weak bonds. As an alternative solution, we developed Ti-C-Cu based reactive braze foils that rely on TiC formation reactions to melt the Cu braze material. In this system, the foils did not produce gas or vapor upon reaction but did form the desired TiC product with molten Cu. Unfortunately, the reaction temperatures and the duration of Cu melting were insufficient to produce effective bonds. The goal of achieving bond strengths of 20 MPa or higher was not achieved.

36 MATERIALS SCIENCE↗

Neutron Measurements from Boron Carbide Addition to a Plutonium Waste Form

The Department of Energy (DOE) has identified the Dilute and Dispose approach as the preferred method for the disposition of surplus plutonium materials. Dilute and Dispose requires surplus plutonium to be converted to an oxide product and then dry blended with a multi-component adulterant mixture to reduce the Safeguards and Security attractiveness level of the materials. The resulting product will be discarded in a geologic repository at the Waste Isolation Pilot Plant (WIPP).

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Broad Scope Analysis of the MOX Fuel Fabrication Facility and Disposition of Plutonium

The Plutonium Management and Disposition Agreement (PMDA), signed into effect in 2000, between the United States and Russia, was made in a post-Cold War effort to dispose of military-useable material, a combined 68 metric tons of weapon-grade plutonium. The United States has been pursuing a disposition path through conversion to MOX fuel for use in current commercial nuclear reactors. The Savannah River Site’s (SRS) MOX Fuel Fabrication Facility (MFFF, the MOX facility) began construction in 2007 with intent to uphold the United States’ half of the agreement. In the FY2017 budget, the Obama administration proposed a termination of the MFFF after lack of sufficient funding to the project, which caused paralyzing delays and drastically inflated costs for completion. Prolonged construction, piled costs, and divergent policies between shifting administrations have resulted in turmoil between the United States and Russia, culminating with the proposed abandonment of the MOX disposition path and being used as a justification by Russia to withdraw from the agreement until the United States is able to identify a clear plan, fulfilling the requirements set forth by the PMDA. The leading expedient to replace MOX fuel is the dilute and dispose method, which leaves uncertainty for the SRS MFFF and places reliance on New Mexico’s Waste Isolation Pilot Plant (WIPP) to legally accommodate the additional and unaccounted waste. If the current capacity of WIPP proves insufficient, construction of a new repository for transuranic waste would only incur additional costs and regulatory burdens, along with extreme schedule delays. Future proposed adaptations of the SRS MFFF include pit production, which would require complex and costly alterations to be operational at the current site. Restrictions from Congress, such as mandating the proposed solution to abandoning MFFF must equal half of the costs required for completing the facility, have fueled severely underestimated quotations of these alternatives. The increasing pressure from both Russia and South Carolina government officials to make a decision could result in the pursuit of another doomed project, leaving the United States with even further sunk costs and strained international relations. This paper will summarize the involved history of the MFFF, explicate the recourses to salvage the facility for pit production, and provide postulation on the dilute and dispose method.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Magnetic Microcalorimeter (MMC) Gamma Detectors with Ultra-High Energy Resolution

The goal of this LCP is to develop ultra-high resolution gamma-ray detectors based on magnetic microcalorimeters (MMCs) for accurate measurements of nuclear decay data and NDA of nuclear materials. For highest energy resolution, we are introducing erbium-doped silver (Ag:Er) as a novel sensor material and implement several geometry and design changes to improve the signal-to-noise ratio. The detector sensitivity will be increased by developing arrays of 32 Ag:Er pixels read out by 16 SQUID preamplifiers, and by developing a cryogenic Compton veto to reduce the spectral background. For highest energy resolution we will operate the MMC detector arrays in a dilution refrigerator with a base temperature <10 mK. The detector performance and utility will be demonstrated with radioactive sources of interest to the safeguards community. In FY16 and FY17, we had purchased a liquid-cryogen-free dilution refrigerator and installed 16 SQUID preamplifiers and writing for MMC detector operation at ~10 mK. We have also developed the process to fabricate the first Ag:Er-based MMCs, built prototype detector arrays and tested them with different radioactive sources. We have also shown that our MMC detectors can achieve the LCP goal of an energy resolution below 50 eV as needed to resolve most closelyspaced lines of interest for NDA. The goals for FY18 were then 1) to optimize the MMC design based on the measured detector characteristics and to increase the array size to 32-pixels for increased sensitivity, and 2) to demonstrate the utility of MMC gamma-ray detectors in applications relevant in nuclear safeguards.

42 ENGINEERING↗

Analysis of Tank 38H (HTF-38-19-18, -19) and Tank 43H (HTF-43-19-20, -21) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. Overall, the results of the analysis indicate the concentrations of species in the Tank 38H surface sample increased significantly from the previous sample with the sodium concentration increasing from 1.09 M in the previous sample to 3.19 M in the current sample. However, it should be noted that the previous Tank 38H surface sample was very dilute compared with typical Tank 38H samples of the recent past. The Tank 38H sub-surface sample shows a composition fairly similar to the previous sample’s composition. Both the Tank 43H surface and sub-surface samples appear slightly more dilute than the previous samples based on the sodium concentrations. For both Tank 38H and Tank 43H, the subsurface samples appear slightly more concentrated for most species than the surface samples. These results indicate some success in increasing the salt solution concentration and reducing stratification in Tank 38H, but some stratification is still evident in both Tank 38H and Tank 43H.

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MagMicro with Ultra-High Energy Resolution (Report Q1 FY19)

Progress report provides update on these tasks: Task 15 Fabricate 32-pixel Ag:Er MMC Arrays, Task 16 Demonstrate energy resolution <50 eV FWHM, Task 17 Integrate Compton Veto with MMC in Dilution Refrigerator, Task 18 Operate 32-MMC array in LLNL dilution refrigerator, Task 19 Acquire Gamma Spectrum from Safeguards-Relevant Sample, and Task 20 Present paper at INMM and report to NA-22.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

MagMicro with Ultra-High Energy Resolution (Q2 FY19)

Quarterly progress on six tasks: Task 15 Fabricate 32-pixel Ag:166Er MMC Arrays, Task 16 Demonstrate energy resolution <50 eV FWHM, Task 17 (Integrate Compton Veto with MMC in Dilution Refrigerator, Task 18 Operate 32-MMC array in LLNL dilution refrigerator, Task 19 (Acquire Gamma Spectrum from Safeguards-Relevant Sample, and Task 20 Present paper at INMM and report to NA-22.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Soluble and Particulate Mercury Deployment of Analytical Method for the Savannah River Site Liquid Waste System

Savannah River National Laboratory (SRNL) developed, tested, and deployed in a radiological containment unit (CU) an analytical method for quantifying particulate total mercury and soluble total mercury in radioactive samples such as the those generated by the dilution of Savannah River Site (SRS) High-Level Waste. This method relies on direct mercury analysis and other associated capabilities for matrix independent quantification of total mercury in solids or liquids (i.e., any sample that can be introduced into the instrument oven for pyrolysis to release all mercury for measurement). The matrix independence allows for discreet measurements of the starting sample, the collected particulates and the filtrate liquid, thus enabling a mass balance quality check. For example, an analysis of a diluted sample from the SRS liquid waste system (LWS) resulted in a measured total mercury value of 55.0 mg Hg/L and a nearly matching calculated total mercury value of 55.1 mg Hg/L (± 20% 2σ) from the summation of measured soluble mercury (47.8 mg Hg/L ± 20% 2σ) and measured particulate mercury (7.26 mg Hg/L ± 20% 2σ). The advantages of the particulate-soluble mercury analysis method are: waste minimization using small radioactive liquid volumes, minimal radiological sample processing and reduced handling steps protective of workers (ALARA) and improved data quality, syringe filter technology which eliminates vacuum filtration and the potential loss of volatile species, small diameter filters (13 mm nominal to 25 mm if needed to avoid clogging) and small disposable poly filter holders (no need to clean) which minimize waste, flexibility provided for a range of starting concentrations, particulate-soluble ratios, and sample matrix conditions, soluble and particulate are measured results that, when summed, and are in good agreement with the total mercury measurement.

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Cesium Removal Performance Comparisons of Crystalline Silicotitanate Media Batches with Savannah River Site Waste Simulant

The Tank Closure Cesium Removal (TCCR) system uses ion exchange columns filled with Crystalline Silicotitanate (CST) media to process radioactive waste solutions for the removal of Cs137. TCCR currently focuses on dissolving Savannah River Site (SRS) Tank 10H waste (primarily sodium salt cake solids) within the tank followed by at-tank ion exchange column treatment. Plans are underway to prepare and install a second TCCR unit at SRS. Capacity and particle size differences exist between archived (IE-911) and more recently-prepared CST media batches (9120- B and 9140-B). Side-by-side comparison testing was performed to evaluate the cesium removal performance of each batch to aid in selecting the preferred CST batch and media characteristics to load into the second TCCR unit. Batch contact equilibrium and flow-through column tests have been conducted with three CST batches using an SRS Average Simulant. Simulant batch contact equilibrium cesium loading results for the three CST batches (including two lots of one batch) are provided in Table ES-1. The 35 °C data indicates that the archived IE-911 batch has a higher cesium capacity than recently-prepared CST media and that the minor TCCR CST 9120-B media lot (2099000035) has similar cesium removal performance to the major TCCR lot (2099000034). Tests conducted at 25 ºC for the archived IE-911 CST batch indicated lower cesium removal performance with this simulant batch than was observed recently with a different SRS Average Simulant batch. A dilution factor (DF) is typically utilized when modeling engineered CST media cesium loading performance to account for mass contributions from the binder material. In cases where CST performance is lower than expected, this factor includes corrections for the binder and for low performance. The ZAM (Zheng, Anthony, and Miller) Isotherm Model DF values are provided in Table ES-1 for each simulant batch contact result. DF values near 0.5 were determined for the 9120-B and 9140-B CST batch contact tests while DF values near 0.6 (20% higher) were determined for the tests with IE-911. These dilution factors are lower than recently observed with a different SRS Average Simulant batch (9140-B DF = 0.68; IE-911 DF = 1.0). Based on these results, it appears that some component in the simulant solution used for equilibrium testing may have resulted in reduced cesium loading on the CST media.

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Testing of an AP-105 Precipitation Simulant

A tank AP-105 chemical simulant was developed and diluted with Washington River Protection Solutions (WRPS)-supplied raw water to evaluate the stability of AP Farm wastes with respect to precipitation under Direct Feed Low-Activity Waste (DFLAW)-typical waste feed staging operations. The current report provides a high-level summary of the basis for simulant selection, the recommended (and prepared) simulant chemistry, and observed stability with respect to solids formation upon simulant preparation and subsequent dilution with raw water.

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Glycolate Analysis in Tank 22: Developing and Testing Analytical Methods for the Savannah River Site Liquid Waste System

Researchers developed and tested a range of techniques to support a low mg/L Limit of Quantitation (LOQ) of glycolate in radioactive Tank 22 waste solution by Ion Chromatography (IC) and by proton NMR. For the IC method, Dionex OnGuard II cartridges were tested as a means of removing alkali earth and transition metals that can interfere during ion chromatography applications especially when analyzing for low-concentration, chelating analytes. Additionally, concentrations of nitrate in the raw Tank 22 sample (5,000 to 10,000 mg/L) were managed by using reasonable levels of sample dilution. The resulting IC performance quality was enhanced by improving the baseline, increasing sensitivity [Limit of Quantitation (LOQ) of 12 mg/L and Limit of Detection (LOD) of 4.0 mg/L], and resolving analytes into well-defined Gaussian peaks when using the Dionex OnGuard II H⁺ cartridges to remove matrix interferences. High concentrations of nitrate limited the performance of the IC method. To achieve an acceptable baseline, samples with high nitrate content require more dilution, resulting in higher detection limits. Tests on samples with higher concentrations of nitrate (Tank 30 and 32 supernate with approximately 150000 mg/L nitrate) suggested that IC detection limits for glycolate in these samples would be > 500 mg/L. Thus, an LOQ of 12 mg/L is not feasible by this IC method on evaporator feed samples. An alternative method of glycolate analysis, using proton nuclear magnetic resonance (H NMR), was developed by the research team. In initial tests, the H NMR technique provided reasonable quantitation of glycolate in Tank 22 conditions by direct observation of the liquid. The H NMR method may provide improved detection limits for solutions with higher nitrate concentrations. We recommend further development of this analysis for high nitrate LWS samples such as evaporator feed and evaporator drop tank content. A method for pretreatment of samples using crystalline silicotitanate (CST) was developed and tested. The objective of the pretreatment was to facilitate analysis of samples with higher levels of radioactivity. The pretreatment did not influence the glycolate concentration in solution, and the pretreatment is projected to reduce Cs 137 activity in a sample by a factor of 16,200. The double strike CST pretreatment was demonstrated and would allow milliliters of higher activity samples to be transferred from the Shielded Cells and handled in a containment unit for glycolate analysis. The various studies validated IC and H NMR methods for glycolate analysis, defined the range of applicability, and demonstrated key supporting analytical protocols. Based on the results, high quality glycolate analysis of Tank 22 is feasible down to approximately 12 mg/L, with the potential for broader applicability of the methods to other conditions in the Savannah River Site Liquid Waste System (LWS).

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