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All sourcesNASA NTRSDOE OSTI
DOE OSTI2012

Saltstone SDU6 Modeling Study

A new disposal unit, designated as Saltstone Disposal Unit 6 (SDU6), is being designed for support of site accelerated closure goals and salt waste projections identified in the new Liquid Waste System Plan. The unit is a cylindrical disposal cell of 375 ft in diameter and 43 ft in height, and it has a minimum 30 million gallons of capacity. SRNL was requested to evaluate the impact of an increased grout placement height on the flow patterns radially spread on the floor and to determine whether grout quality is impacted by the height. The primary goals of the work are to develop the baseline Computational Fluid Dynamics (CFD) model and to perform the evaluations for the flow patterns of grout material in SDU6 as a function of elevation of grout discharge port and grout rheology. Two transient grout models have been developed by taking a three-dimensional multiphase CFD approach to estimate the domain size of the grout materials radially spread on the facility floor and to perform the sensitivity analysis with respect to the baseline design and operating conditions such as elevation height of the discharge port and fresh grout properties. For the CFD modeling calculations, air-grout Volume of Fluid (VOF) method combined with Bingham plastic and time-dependent grout models were used for examining the impact of fluid spread performance for the initial baseline configurations and to evaluate the impact of grout pouring height on grout quality. The grout quality was estimated in terms of the air volume fraction for the grout layer formed on the SDU6 floor, resulting in the change of grout density. The study results should be considered as preliminary scoping analyses since benchmarking analysis is not included in this task scope. Transient analyses with the Bingham plastic model were performed with the FLUENT TM code on the high performance parallel computing platform in SRNL. The analysis coupled with a transient grout aging model was performed by using ANSYS-CFX code in the parallel computing platform in Mercer University. Recommended operational guidance was developed assuming that local shear rates and flow patterns related to radial spread along the SDU floor can be used as a measure of grout performance and spatial dispersion affected by the grout height and viscosity. The main conclusions drawn from the grout modeling and calculations are as follows: • The 5 ft height baseline results show that when the 150 gpm grout flow with a 5 Pa yield stress and a 60 cp viscosity is poured down through a 3 inch discharge port, the grout is spread radially up to about 64 ft distance from the pouring center after 2 hours’ pouring time. The air volume fraction of the grout layer is about 29% at 5 minutes’ transient time, and it is reduced by about 9% in 2 hours’ pouring time, resulting in the grout density consisting of about 80% grout and 20% air volume fractions. • The sensitivity results show that when the discharge port is located at a higher position, a larger amount of air is trapped inside the layer formed below the discharge port at the early transient time of less than 30 minutes because of the higher impinging momentum of the grout flow on the floor, resulting in the formation of less smooth layer. • The results clearly indicate that the radial spread for the 43 ft discharge port is about 10% faster than that of the 5 ft discharge port for the early transient period of 5 minutes. However, for the pouring time longer than half an hour, the discharge port height does not affect the radial distance spread on the disposal floor. • When grout quality is related to grout volume fraction, the grout volume fraction for the 43 ft discharge port has lower volume fraction than the 5 ft discharge port for the transient period of the first 5 minutes. However, for the pouring time longer than half an hour, the discharge port height does not affect the grout volume fraction for the layer accumulated on the disposal floor. • A modified Bingham plastic model coupled with time-dependent viscosity behavior was developed for conducting the initial scoping calculations to assess the impact of fluid residence time on radial spreading and basic flow patterns. • The results for the transient viscosity model show that when grout material becomes more viscous, the thickness of the grout layer accumulated on the floor becomes higher, but the radial distance spread on the horizontal floor becomes smaller. The early transient results for the grout density with about 32% air volume fractions are in reasonable agreement with those of the idealized Bingham plastic model. • It is recommended that the current models developed here be benchmarked against the experimental results for critical applications of the modeling results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2012

Evolution of Chemical Conditions and Estimated Plutonium Solubility in the Residual Waste Layer During Post-Closure Aging of Tank 18

This document updates the Eh-pH transitions from grout aging simulations and the plutonium waste release model of Denham (2007, Rev. 1) based on new data. New thermodynamic data for cementitious minerals are used for the grout simulations. Newer thermodynamic data, recommended by plutonium experts (Plutonium Solubility Peer Review Report, LA-UR-12-00079), are used to estimate solubilities of plutonium at various pore water compositions expected during grout aging. In addition, a new grout formula is used in the grout aging simulations and apparent solubilities of coprecipitated plutonium are estimated using data from analysis of Tank 18 residual waste. The conceptual model of waste release and the grout aging simulations are done in a manner similar to that of Denham (2007, Rev. 1). It is assumed that the pore fluid composition passing from the tank grout into the residual waste layer controls the solubility, and hence the waste release concentration of plutonium. Pore volumes of infiltrating fluid of an assumed composition are reacted with a hypothetical grout block using The Geochemist's Workbench{reg_sign} and changes in pore fluid chemistry correspond to the number of pore fluid volumes reacted. As in the earlier document, this results in three states of grout pore fluid composition throughout the simulation period that are termed Reduced Region II, Oxidized Region II, and Oxidized Region III. The one major difference from the earlier document is that pyrite is used to account for reducing capacity of the tank grout rather than pyrrhotite. This poises Eh at -0.47 volts during Reduced Region II. The major transitions in pore fluid composition are shown. Plutonium solubilities are estimated for discrete PuO2(am,hyd) particles and for plutonium coprecipitated with iron phases in the residual waste. Thermodynamic data for plutonium from the Nuclear Energy Agency are used to estimate the solubilities of the discrete particles for the three stages of pore fluid evolution. In Denham (2007, Rev. 1), the solubilities in the oxidized regions were estimated at Eh values in equilibrium with dissolved oxygen. Here, these are considered to be maximum possible solubilities because Eh values are unlikely to be in equilibrium with dissolved oxygen. More realistic Eh values are estimated here and plutonium solubilities calculated at these are considered more realistic. Apparent solubilities of plutonium that coprecipitated with iron phases are estimated from Pu:Fe ratios in Tank 18 residual waste and the solubilities of the host iron phases. The estimated plutonium solubilities are shown. Uncertainties in the grout simulations and plutonium solubility estimates are discussed. The primary uncertainty in the grout simulations is that little is known about the physical state of the grout as it ages. The simulations done here are pertinent to a porous medium, which may or may not be applicable to fractured grout, depending on the degree and nature of the fractures. Other uncertainties that are considered are the assumptions about the reducing capacity imparted by blast furnace slag, the effects of varying dissolved carbon dioxide and oxygen concentrations, and the treatment of silica in the simulations. The primary uncertainty in the estimates of plutonium solubility is that little is known about the exact form of plutonium in the residual waste. Other uncertainties include those inherent in the thermodynamic data, pH variations from those estimated in the grout simulations, the effects of the treatment of silica in the grout simulations, and the effect of varying total dissolved carbonate concentrations. The objective of this document is to update the model for solubility controls on release of plutonium from residual waste in closed F-Area waste tanks. The update is based on new information including a new proposed grout formulation, chemical analysis of Tank 18 samples and more current thermodynamic data for plutonium and grout minerals. In addition, minor changes to the modeling of the grout chemical evolution have been made. It should be noted that the intent is to provide bounding solubilities for plutonium to be used in Performance Assessment modeling rather than trying to identify an exact concentration of plutonium in pore fluids released from a tank at any given time. This document also considers suggestions and opportunities for improvement regarding the plutonium modeling assumptions from the Plutonium Solubility Peer Review Report, LA-UR-12-00079.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2012

Effect of Curing Temperature and Composition on the Performance Properties of Saltstone - 12473

When freshly mixed Saltstone is placed into a vault at the Savannah River Site, the heat of hydration produced during curing causes the temperature of the grout to increase. It is not uncommon for the temperature of the grout to increase by 30 to 50 deg. C above the starting temperature depending on the vault size and location, environmental conditions and pour schedule. For example, temperatures measured by thermocouples in one cell have exceeded 70 deg. C. The elevated temperatures, once reached, can extend for weeks or even months. Recent studies at Savannah River National Laboratory (SRNL) have shown that curing simulated Saltstone mixes at elevated temperatures can lead to reduced compressive strength and dynamic Young's modulus as well as increased total porosity when compared to the same grout mixes cured at 20 deg. C. Samples cured at 60 deg. C can have hydraulic conductivities approximately 600 times greater than samples cured at 20 deg. C. Previous studies have shown that the 60 deg. C cured mix had a dynamic Young's modulus that was half that of the mix cured at 20 deg. C. However, high temperature curing may not always have negative effects on the performance properties of the grout. These results indicate that higher curing temperatures can significantly alter the performance properties that are inputs for the Saltstone Performance Assessment. The Saltstone formulation (mix design) must produce a grout waste form that meets both placement and performance properties. A statistically designed set of mixes was developed to determine key process and compositional factors that affect the performance properties of Saltstone grout. A total of 27 mixes were batched and tested. There are eight baseline mixes that contain high and low values of aluminate concentration, varying w/p ratio, and varying fly ash content in the premix. Each of the eight mixes was cured at 22, 40 and 60 deg. C. The three additional reference mixes batched at the beginning, middle and end of testing showed good reproducibility throughout the study. The results of varying the operational and compositional factors on the performance properties of Saltstone grout are: - The Young's modulus is inversely affected by the curing temperature of the grout. - The aluminate content of the salt solution increases the Young's modulus of the Saltstone for samples cured at 20 and 40 deg. C. - All grouts cured at 60 deg. C have low Young's moduli and the composition of the grout mix did not have any positive effects on the performance properties after curing at this temperature. - The fly ash content in the premix had not discernible effect on the Young's modulus. - The water to premix ratio does not affect the Young's modulus. - Grouts made with the high aluminate salt solution have lower hydraulic conductivities than those made with the low aluminate simulant. - Temperature has an inverse effect on the hydraulic conductivity. - In general, increasing the water to premix ratio and the fly ash content will increase the hydraulic conductivity. - The porosity and cured density of the Saltstone grout are primarily a factor of the water to premix ratio of the grout formulation. The correlation between hydraulic conductivity and Young's modulus investigated in previous studies was evaluated further in this report. The current data as well as data from previous studies was fitted by a second degree polynomial function with a 77.1 % R-squared value. This model can be used to estimate the hydraulic conductivity of a sample based its Young's modulus for a limited range (E values up to 7 GPa). More data points should be included to further define the relationship between these performance properties are high Young's moduli and low hydraulic conductivities. The Young's modulus should still be measured on grouts formulated in future studies to be used as screening method for samples to be sent for hydraulic conductivity measurements. Saltstone grout has a complicated microstructure that is affected by the composition of the salt solution, the dry feed mixture composition, and the conditions under which it cures. The performance properties investigated are interrelated, which can make it difficult to determine individual relationships between various factors. Porosity is a large factor in determining both the Young's modulus and the hydraulic conductivity of the samples. Although the cured density is a straightforward measurement, it is not a significant performance property that needs further investigation. The porosity measurement provides similar and more meaningful data in relation to other performance properties. Based on the results of this study, the aluminate content of the salt solution does have an effect on the Young's modulus and the hydraulic conductivity and its effects should continue to be investigated. However, a new projection of aluminate contents should be used since projections change over time. The variability of fly ash in the premix did not prove to be a contributing factor that effects the performance properties of Saltstone and does not need to be included in future studies unless significant deviations from the baseline mix are proposed. The water to premix ratio has a significant effect on the performance properties of interest and the effects of varying this factor need further investigation. It is recommended that smaller ranges of w/p are investigated in order to provide data that is more relevant to the Saltstone being placed in the vaults. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2011

BENCH SCALE SALTSTONE PROCESS DEVELOPMENT MIXING STUDY

The Savannah River National Laboratory (SRNL) was requested to develop a bench scale test facility, using a mixer, transfer pump, and transfer line to determine the impact of conveying the grout through the transfer lines to the vault on grout properties. Bench scale testing focused on the effect the transfer line has on the rheological property of the grout as it was processed through the transfer line. Rheological and other physical properties of grout samples were obtained prior to and after pumping through a transfer line. The Bench Scale Mixing Rig (BSMR) consisted of two mixing tanks, grout feed tank, transfer pump and transfer hose. The mixing tanks were used to batch the grout which was then transferred into the grout feed tank. The contents of the feed tank were then pumped through the transfer line (hose) using a progressive cavity pump. The grout flow rate and pump discharge pressure were monitored. Four sampling stations were located along the length of the transfer line at the 5, 105 and 205 feet past the transfer pump and at 305 feet, the discharge of the hose. Scaling between the full scale piping at Saltstone to bench scale testing at SRNL was performed by maintaining the same shear rate and total shear at the wall of the transfer line. The results of scaling down resulted in a shorter transfer line, a lower average velocity, the same transfer time and similar pressure drops. The condition of flow in the bench scale transfer line is laminar. The flow in the full scale pipe is in the transition region, but is more laminar than turbulent. The resulting plug in laminar flow in the bench scale results in a region of no-mixing. Hence mixing, or shearing, at the bench scale should be less than that observed in the full scale, where this plug is non existent due to the turbulent flow. The bench scale tests should be considered to be conservative due to the highly laminar condition of flow that exists. Two BSMR runs were performed. In both cases, wall shearing was shown to reduce the rheological properties of the grout as it was processed through the transfer line. Samples taken at the static feed tank showed that gelling impacted the rheological properties of the grout before it was fed into the pump and transfer line. A comparison of the rheological properties of samples taken at the feed tank and transfer line discharge indicated shearing of the grout was occurring in the transfer line. Bench scale testing of different mixing methods with three different salt solutions showed that method of mixing influences the rheological properties of the grouts. The paddle blade mixing method of the salt solution used for the BMSR testing provided comparable rheological properties of the grout prepared in the BMSR after 14 minutes of processing, B3. The paddle blade mixing method can be used to represent BMSR results and mixing time can be adjusted to represent larger scale mixing.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2018

Silver-iodine secondary waste stabilization: multi-scale evaluation

Iodine-129 is a key risk driver in most low-level waste cementitious waste repositories. The objectives of this study were to determine iodine speciation in cementitious materials with slag (Grout+slag) and without slag (Grout–slag) and its impact on iodine immobilization. Additional studies were conducted to determine if grout was compatibility as a waste form for the most common adsorbent used to remove aqueous and gaseous radioiodine, silver-impregnated granular activated carbon (Ag-GAC). Rankings of iodine species by their tendency to bind to grout were: iodide << organo-iodine ≤ iodate. Similarly, ranking of grout formulations by their tendency to immobilize iodine were: Grout +slag < Grout -slag . Organo-iodine comprised >40% of the leachate solution from grout samples initially hydrated (cured) with iodide. The origin of the organic ligand comprising the organo-iodine was organic carbon in the grout material (~1200 mg/kg). Iodine in the solid phase, as determined by K-edge X-ray Absorption Near-Edge Spectroscopy, and aqueous phases were not in equilibrium and essentially no iodine speciation transformations occurred within the grout after one month of curing, irrespective of which iodine species was initially added to the mix. For the first time, these studies demonstrate that multiple iodine species can co-exist simultaneously in grout porewater, the iodine species initially added to the grout can greatly affect immobilization, and that Ag-GAC can be safely disposed in grout formulation, but not in the presence of slag. These results help explain previous data and reduce uncertainty associated with the disposal of nuclear waste.

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

Iodine speciation in cementitious environments

Iodine-129 is a key risk driver in most low-level waste cementitious waste repositories. Objectives of this study were to determine iodine speciation in cementitious materials with slag (Grout +slag ) and without slag (Grout –slag ) and its impact on iodine immobilization. Irrespective of which iodine species was amended to the aqueous phase, there were no significant differences in uptake-K d values (~3 L/kg). However, when the various iodine species were hydrated with the grout, the release-K d values (6.1–121.8 L/kg) were significantly greater than the uptake-K d values, and the amended iodine speciation (I – << org-I ≤ IO 3 – ) and grout formulation (Grout –slag < Grout +slag ) had a significant impact on release-Kd values. In grout samples amended with I – and IO 3 – , org-I was formed and comprised a majority of the iodine in the leachate after 28 days of equilibration. The formed org-I originated from organic carbon (C) in the grout material (~1200 mg/kg C). For the first time, these studies demonstrate that multiple iodine species can co-exist simultaneously in grout porewater, the iodine species initially added to the grout can greatly affect iodine immobilization, and the addition of slag to the grout formulation increased iodine immobilization. Furthermore, these results may have important implications on radioiodine waste disposal.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2012

Evolution of chemical conditions and estimated solubility controls on radionuclides in the residual waste layer during post-closure aging of high-level waste tanks

This document provides information specific to H-Area waste tanks that enables a flow and transport model with limited chemical capabilities to account for varying waste release from the tanks through time. The basis for varying waste release is solubilities of radionuclides that change as pore fluids passing through the waste change in composition. Pore fluid compositions in various stages were generated by simulations of tank grout degradation. The first part of the document describes simulations of the degradation of the reducing grout in post-closure tanks. These simulations assume flow is predominantly through a water saturated porous medium. The infiltrating fluid that reacts with the grout is assumed to be fluid that has passed through the closure cap and into the tank. The results are three stages of degradation referred to as Reduced Region II, Oxidized Region II, and Oxidized Region III. A reaction path model was used so that the transitions between each stage are noted by numbers of pore volumes of infiltrating fluid reacted. The number of pore volumes to each transition can then be converted to time within a flow and transport model. The bottoms of some tanks in H-Area are below the water table requiring a different conceptual model for grout degradation. For these simulations the reacting fluid was assumed to be 10% infiltrate through the closure cap and 90% groundwater. These simulations produce an additional four pore fluid compositions referred to as Conditions A through D and were intended to simulate varying degrees of groundwater influence. The most probable degradation path for the submerged tanks is Condition C to Condition D to Oxidized Region III and eventually to Condition A. Solubilities for Condition A are estimated in the text for use in sensitivity analyses if needed. However, the grout degradation simulations did not include sufficient pore volumes of infiltrating fluid for the grout to evolve to Condition A. Solubility controls for use in a flow and transport model were estimated for 27 elements in each of the chemical stages generated in the grout simulations plus local groundwater. The grout simulations were run with the initial infiltrating fluid in equilibrium with atmospheric oxygen to account for degradation of the reduction capacity of the grout. However, a lower Eh was used in pore fluids in the oxidizing conditions used to estimate solubilities to be more consistent with measured Eh values and natural systems. Solubilities of plutonium are affected by this decision, but those of other elements are not. In addition, the baseline for H-Area tanks is that they will be washed with oxalic acid prior to being filled with grout. Hence, oxalate was included in the pore fluids by assuming equilibrium with calcium oxalate. Solubility estimates were done by equilibrating a solubility controlling phase for each element with the pore fluid compositions using The Geochemist’s Workbench®. Condition B pore fluids are similar to Condition D. Therefore, solubilities for Condition B were not estimated, but assumed to be the same as in Condition D. In general solubility controlling phases were selected to bias solubilities to higher values. Several elements had no solubility controls and solubility estimates for other elements were omitted because the elements had short half-lives or were present in residual waste in very low amounts. For these it is recommended that release from the tank be instantaneous when the tank liner is breached. There is considerable uncertainty in this approach to enabling a flow and transport model to account for variable waste release. Yet, it is also flexible and requires much less computing time than a fully coupled reactive transport model. This allows some of the uncertainty to be addressed by multiple flow and transport sensitivity cases. Some of the uncertainties are addressed within this document. These include uncertainty in infiltrate composition, grout mineralogy, and disposition of certain components during the simulations. Uncertainty in the solubility estimates is addressed in part by examining sensitivity of solubilities for four key elements to uncertainty in thermodynamic data, pH, Eh, total inorganic carbon concentration, and oxalate concentration. In addition, the solubilities for the elements estimated here are compared to two other compilations of solubilities in cementitious materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Alternate paddle configuration for improved wear resistance in the saltstone mixer

The Saltstone Production Facility has a 10-inch Readco-Kurimoto continuous mixer that mixes the premix dry feeds and low-level waste salt solution to make fresh (uncured) saltstone. Inspection of the mixer in January 2013 showed significant wear on the third, fourth and fifth paddle pairs after the conveying augers. A 2-inch Readco-Kurimoto continuous mixer was used to test alternate paddle configurations for use in the 10-inch mixer to decrease the wear rate on the paddles. Two wear tests were conducted to investigate a method of reducing wear on the mixer paddles. The first test (wear test 2a) had a paddle configuration similar to the currently installed 10-inch mixer in the SPF. This test established baseline wear. The second test (wear test 2b) had a reconfigured paddle arrangement that replaced the flat paddles with helical paddles for paddle pairs 2 - 6 and aligned paddle pair 1 with the augers. The intent of the reconfiguration was to more effectively convey the partially wetted dry feeds through the transition region and into the liquid feed where paddle wear is reduced due to dry feeds and salt solution being mixed at the intended water to premix ratio. The design of the helical paddles provides conveyance through the transition region to the liquid feed inlet. The alignment with the auger is aimed to provide a smoother transition (minimizing the discontinuity between the auger and paddle pair 1) into the downstream paddles. A soft metal with low wear resistance (6000 series aluminum) was used for the wear testing paddles to determine wear patterns while minimizing run time and maximizing wear rate. For the two paddle configurations tested using the scaled 2-inch Readco-Kurimoto continuous mixer, with the first six paddles after the augers replaced by the wear paddles and the remaining paddles were stainless steel. Since the 10-inch SPF mixer is designed with the liquid inlet centered over paddle pairs 5 and 6, the scaled 2-inch mixer was configured the same way. The wear rate from wear test 2a was approximately double the wear rate from wear test 2b for paddle pairs 4 and 5. For both configurations, there was little or no wear on paddle pairs 1, 2, 3 and 6 based on mass change, indicating that the un-wetted and fully wetted premix materials cause less wear than the partially wetted premix. Additionally, inspection of the wear surface of the paddles showed more deformation on the flat paddles than the helical paddles which was consistent with the wear rates. Aligning of the auger discharge flight with paddle pair 1 resulted in a lower wear rate paddle pair 1 rather than having them misaligned with the feed augers. During the paddle wear tests, polishing wear was observed on the inside barrel of the mixer. The polishing wear is evident on the upper housing clamshell and the lower housing clamshell primarily at paddle pairs 4 and 5, which is the transition region of the mixer. Wear on the mixer barrel increases the space between the paddles and the barrel, resulting in increased grout build up on the barrel. Since the mixer barrel cannot be reconfigured or replaced in the SPF, the method for mitigating wear on the barrel is to move the more viscous grout through the transition region as quickly as possible. In addition, the location of the liquid inlet does not allow for sufficient cleaning of the mixer since residual grout remains on paddle pairs 1 - 4. As the paddles continue to wear and the self-cleaning capability of the paddles is lost, the lack of sufficient flushing would aid in grout build up between the barrel and the paddles which could eventually lead to decreased throughput capacity of the dry feeds. Changing the paddle configuration from flat to helical resulted in no change to the rheological properties of the grout mixture. Both tests produced a grout that is within the processing range of the SPF. Based on the results of this testing, it is recommended for the currently installed SPF mixer that paddle pairs 1 through 6 be helical rather than flat, with the paddle pair 1 aligned with the feed augers in order to minimize the wear occurring in the SPF mixer. Based on the results of this testing, it is recommended that the mixer be inspected and critical measurements be taken whenever the SPF processing schedule allows in order to establish a wear rate of the 10-inch mixer paddles.5 Based on these measurements, the lifetime of paddles in the transition region can be established in order to set up a maintenance schedule for the mixer. Since replacing the entire mixer is very expensive and time intensive, replacing the worn paddles after a specific time period would allow for planned shutdowns as well as process optimization such that the mixer throughput is not compromised. In addition, further testing should be performed to determine an alternate liquid inlet location to better flush the mixer of residual grout at the end of processing. Sufficiently cleaning the mixer will help eliminate another potential source of wear. Another potential method for reducing the wear rate in the mixer is to reduce the mixer speed without affecting the throughput capacity. Since wear rate is a function of impact velocity of the grout and mixing paddles, testing could be done using the 2-inch mixer determine the optimum mixer speed to reduce wear but not adversely impact facility operations (e.g. throughput capacity and grout properties).

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Nitrate and Nitrite at Hanford – From Tanks to Natural Attenuation

Washington River Protection Solutions, LLC (WRPS) contracted Pacific Northwest National Laboratory (PNNL) in support of their maturation testing and analysis to develop and deploy an ambient temperature solidification/stabilization process for low-activity waste (LAW) (referred to as “grout” in this report). The intent of this effort is to support a sample-and-send regulatory and processing strategy in the Hanford 200 West Area, specifically considering grout waste forms disposal at Hanford in the Integrated Disposal Facility (IDF). Currently the disposal of grouted LAW is not an option because the IDF is not permitted to receive this waste form. The material presented in this report is intended to help inform the U.S. Department of Energy (DOE), the site operating contractors, regulatory agencies, and stakeholders of the future implications of IDF disposal of a grouted LAW waste form, specifically for the behavior of nitrate (NO 3 - ) and nitrite (NO 2 - ) at the Hanford. The only calculation of nitrate release from a hypothetical grouted LAW inventory in the IDF showed that the overall release was slightly above the compliance limit of 45 mg/L nitrate and 3.32 mg/L nitrate after 1000 years (Asmussen et al. 2019). As such, uncertainty around the impact of nitrate and nitrite release from the IDF was identified in the recent National Academies of Sciences study of Hanford supplemental LAW by both the national laboratory team and Hanford stakeholders (Bates et al. 2023). However, these calculations (and others for the IDF involving secondary waste grout) may be conservative as no nitrate and nitrite retention in the grout waste form was assumed, nor any attenuation in the subsurface. There is evidence from the literature of processes that can attenuate nitrate migration both in the waste form and in the Hanford subsurface. If found to be technically defensible and likely to occur in the IDF and associated subsurface, then these processes should be included in modeling of the IDF to represent the behavior of nitrate and nitrite more accurately. Doing so would remove unnecessary conservatism in the modeling projections and reduce the uncertainty in assessments of facility compliance of a grouted LAW waste form in the IDF.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2013

Sensor Network Demonstration for In Situ Decommissioning - 13332

Florida International University's (FIU's) Applied Research Center is currently supporting the Department of Energy's (DOE) Environmental Management Office of D and D and Facility Engineering program. FIU is supporting DOE's initiative to improve safety, reduce technical risks, and limit uncertainty within D and D operations by identifying technologies suitable to meet specific facility D and D requirements, assessing the readiness of those technologies for field deployment, and conducting feasibility studies and large scale demonstrations of promising technologies. During FY11, FIU collaborated with Savannah River National Laboratory in the development of an experimental test site for the demonstration of multiple sensor systems for potential use in the in situ decommissioning process. In situ decommissioning is a process in which the above ground portion of a facility is dismantled and removed, and the underground portion is filled with a cementious material such as grout. In such a scenario, the question remains on how to effectively monitor the structural health of the grout (cracking, flexing, and sinking), as well as track possible migration of contaminants within and out of the grouted monolith. The right types of sensors can aid personnel in better understanding the conditions within the entombed structure. Without sensors embedded in and around the monolith, it will be very difficult to estimate structural integrity and contaminant transport. Yet, to fully utilize the appropriate sensors and the provided data, their performance and reliability must be evaluated outside a laboratory setting. To this end, a large scale experimental setup and demonstration was conducted at FIU. In order to evaluate a large suite of sensor systems, FIU personnel designed and purchased a pre-cast concrete open-top cube, which served as a mock-up of an in situ DOE decommissioned facility. The inside of the cube measures 10 ft x 10 ft x 8 ft. In order to ensure that the individual sensors would be immobilized during the grout pouring activities, a set of nine sensor racks were designed. The 270 sensors provided by Idaho National Laboratory (INL), Mississippi State University (MSU), University of Houston (UH), and University of South Carolina (USC) were secured to these racks based on predetermined locations. Once sensor racks were installed inside the test cube, connected and debugged, approximately 32 cubic yards of special grout material was used to entomb the sensors. MSU provided and demonstrated four types of fiber loop ring-down (FLR) sensors for detection of water, temperature, cracks, and movement of fluids. INL provided and demonstrated time differenced 3D electrical resistivity tomography (ERT), advanced tensiometers for moisture content, and thermocouples for temperature measurements. University of Houston provided smart aggregate (SA) sensors, which detect crack severity and water presence. An additional UH sensor system demonstrated was a Fiber Bragg Grating (FBG) fiber optic system measuring strain, presence of water, and temperature. USC provided a system which measured acoustic emissions during cracking, as well as temperature and pH sensors. All systems were connected to a Sensor Remote Access System (SRAS) data networking and collection system designed, developed and provided by FIU. The purpose of SRAS was to collect and allow download of the raw sensor data from all the sensor system, as well as allow upload of the processed data and any analysis reports and graphs. All this information was made available to the research teams via the Deactivation and Decommissioning Knowledge Management and Information Tool (D and D KM-IT). As a current research effort, FIU is performing an energy analysis, and transferring several sensor systems to a Photovoltaic (PV) System to continuously monitor energy consumption parameters and overall power demands. Also, One final component of this research is focusing on developing an integrated data network to capture, log and analyze sensor system data in near real time from a single interface. FIU personnel and DOE Fellows monitored the progress and condition of the sensors for a period of six months. During this time, the sensors recorded data pertaining to strain, compression, temperature, crack detection, moisture presence, fluid mobility, shock resistance, monolith movement, and electrical resistivity. In addition, FIU regularly observed the curing process of the grout and documented the cube condition via the nine racks of sensors. The sensors held up throughout the curing process, withstood the natural elements for six months, and monitored the integrity of the grout. The large scale experiment and demonstration conducted at FIU was the first of its kind to demonstrate the feasibility of state of the art sensors for in situ decommissioning applications. These efforts successfully measured the durability, performance, and precision of the sensors in question as well as monitored and recorded the curing process of the selected grout material under natural environmental conditions. The current energy analysis work is resulting in data on the constraints placed by some of the sensor systems on a power network that requires high reliability and low losses. In addition, a sensor system demonstration has determined that it is feasible to develop an integrated data network where data can be accessed in near real-time from all systems, thereby allowing for larger-scale integrated system testing to be performed. Information collected during the execution of this research project will aid decision makers in the identification of sensors to be used in nuclear facilities selected for in situ decommissioning. (authors)

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

Simulating field conditions for the curing of salt-stone - 15501

salt-stone is a cementitious, low-level waste (LLW) material processed and stored at the Savannah River Site (SRS). It consists of fly ash (FA), blast furnace slag (BFS), and Portland cement that are blended with LLW salt solution. The dry feed materials and the salt solution are mixed at the salt-stone Production Facility (SPF), and the fresh grout subsequently pumped into a salt-stone Disposal Unit (SDU) in the salt-stone Disposal Facility (SDF) where it cures to form a rigid, cementitious monolith. In order to demonstrate the long-term performance of salt-stone, non-radioactive simulant samples are processed and cured in a laboratory environment and subsequently tested with respect to key performance properties. Of particular relevance to assessing the long-term stabilization and immobilization of radionuclides in salt-stone is the permeability, or saturated hydraulic conductivity, which determines the rate of infiltration for oxygen-bearing ground waters that can affect redox sensitive contaminants, such as {sup 99}Tc. Environmental conditions in the SDU, in particular temperature and humidity, are believed to affect the cured properties of salt-stone. With respect to humidity it has been determined that the average vapor space humidity in an SDU is at least 95%, and in addition the assumption can be made that underlying grout is subjected to a moisture-saturated environment by the grout poured over it. With respect to temperature, the SDUs contain thermo-well arrays that provide detailed vertical, and to a lesser degree radial, temperature profiles. Temperature data from the SDUs have subsequently been utilized to better simulate curing temperatures for simulant salt-stone in the laboratory. However, no two thermal profiles are the same, varying with respect to the following parameters: initial temperature, rate of temperature increase, maximum temperature attained, time at maximum temperature, and cooling rate. These temperature variables are dependent on the depth of grout (due to insulating effects of underlying and overlying grout), frequency of grout addition to the SDU (with more frequent additions causing grout temperatures to rise due to the exothermic hydration reactions), and, to a lesser degree, the ambient temperature of the external environment. Due to the variability in each thermal profile recorded in an SDU, the question arises as to which profile (or profiles) should be used in the simulated laboratory environment to best mimic the curing of field emplaced salt-stone, such that there is confidence that the properties measured for laboratory-prepared samples are representative of the grout in the SDU. Since the current SDU design contains sixty-six thermo-wells it is obviously not practical to process simulant samples according to each profile. Rather the aim would be to choose a reduced number of profiles that adequately encompass the range of recorded profiles, or to choose a single profile that is considered most conservative with respect to the resulting properties of interest. This is typically thought to be the profile exhibiting the highest peak temperature since for cement-based materials higher curing temperatures (> 60 deg. C), while resulting in enhanced reaction kinetics and strength development for short curing durations (∼28 days), have been shown to adversely affect the physical properties of the material after extended cure times. In choosing representative profiles it is important to consider not only the maximum temperature, but also the influence of rate of temperature rise to the maximum temperature, and time at or close to the maximum temperature on the post-cured properties. The intent of this paper is to consider the varied curing temperature profiles to which the salt-stone is exposed in an SDU, and to analyze the currently available data for elevated temperature curing of salt-stone to determine the potential thermal effects on the saturated hydraulic conductivity of salt-stone emplaced in an SDU. This may subsequently facilitate a more informed approach to simulating the curing of salt-stone in a laboratory environment. (authors)

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

Thermal Analysis Of Saltstone Disposal Units

SRR requested that SRNL develop a two-dimensional computer simulation model to be capable of predicting grout temperatures attained in Saltstone Disposal Units (SDUs) during the transient addition of saltstone grout and its subsequent storage period. A simulation model was developed to calculate the transient grout temperatures of the SDU facility by taking an axisymmetric and two-dimensional Computational Fluid Dynamics (CFD) approach. The final performance calculations were based on the conduction and radiation model without a convection cooling mechanism for conservative estimate of the grout temperatures and computational efficiency. While convection within the SDU is disabled in the current calculations, the simulation model has the capability of turning convection back on if desired by the user. Hence, the thermal model in its current configuration is best characterized as a finite-volume heat transfer model. However, given that the model can account for convection if desired by the user, it will be referred to as a CFD model. The grout material contains a transient heat source due to the exothermic hydration reactions of the cementitious material mixed with salt solution. The model can predict the transient temperatures at point locations within the poured grout and the overlying vapor space, and at the interior and exterior surfaces of the structure. The thermal model has been developed for two SDUs at the Savannah River Site (SRS); namely, SDU 2A and SDU 6. SDU 2A is a cylindrical unit measuring 150 feet (ft) in diameter, 22 ft tall, and holds approximately three million gallons of grout. SDU 6 is 375 ft in diameter and 43 ft high with a capacity of over thirty million gallons. Prior to performing the thermal calculations for the SDU 6 facility, the benchmarking test for the smaller SDU 2A unit was performed to establish the solution method and to verify the computational results using existing thermocouple data. Based on the Lagrangian discrete method and boundary conditions established by the SDU 2A benchmarking test, the CFD calculations were performed to predict the transient temperatures at local positions of the poured grout and air spaces within the SDU 6 structure.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

New Formulation of Cast Stone for {sup 99}Tc Immobilization in Sulfate Rich Secondary Waste Stream - 16098

A low-temperature, cementitious waste form called Cast Stone (or grout) has been selected for solidification of the Effluent Treatment Facility (ETF)-treated wastes at the Hanford Site. Because the waste stream to be solidified may be relatively high in sulfate, the current Cast Stone dry blend formulation with ordinary Portland cement (OPC), fly ash (FA), and blast furnace slag (BFS) (47% BFS, 45% FA, and 8% OPC) may not be adequate. Thus a new formulation, called secondary waste grout, was proposed and tested. The secondary waste grout uses hydrated lime [Ca(OH){sub 2}] to tie up the sulfate initially such that ettringite [Ca{sub 6}Al{sub 2}(SO{sub 4}){sub 3}(OH){sub 12}.26(H{sub 2}O)] forms rapidly instead of forming as the cementitious waste form cures. Three different liquid waste simulants (242-A evaporator, Environmental Restoration Disposal Facility [ERDF] leachates, and Hanford Tank Waste Treatment and Immobilization Plant [WTP] off-gas condensates) were prepared and solidified using this new dry blend formulation. Baseline grout dry mixes were 20 wt% hydrated lime (HL), 35 wt% OPC, and 45 wt% BFS, and two different water-to-dry mix (w/dm) ratios (0.5 and 0.6) of free water mass to mass of dry blend were tested. After curing for a minimum of 28 days, the grout solidified waste forms were characterized and used for Tc leachability testing using the EPA 1315 Method. X-ray diffraction analysis confirmed that ∼12-15% of ettringite was formed in early stage of 28-day curing for the grouts prepared with the high sulfate WTP simulant and HL addition. In addition, the new formulation of secondary waste grout prepared with HL (20%), OPC (35%), and BFS (45%) at either 0.5 or 0.6 water to dry mix ratio yields higher average Tc interval leachability index (LI) values (12.5 to 13.9) after 28 to 90 days of leaching using deionized water, which is higher than the desired {sup 99}Tc LI value of 12 for grout destined for burial in the Integrated Disposal Facility at the Hanford Site. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Initial Progress on Tank Bottom Repair for the DOE EM Tank Waste R&D Program - 25089

Several years prior to the Lab23-EM001 Call Announcement, Washington River Protection Solutions (WRPS) had done a review in identifying tank repair feasibility. [1, 2] The most viable methods of repair identified for the Floor of a Primary Tank identified were Grout Stabilization and Polymer Grout. Grout Stabilization was described as a self-leveling grout which fills the entire bottom of the tank and creates a new or false bottom. These types of materials have been used at the Savannah River Site (SRS) to fill and close waste tanks as well as contaminated spaces within decommissioned reactors. No mention was made as to the chemical composition of these Stabilizing Grouts in the review, however, grouts used at SRS for the mentioned applications have always been a cementitious grout material. A thickness of approximately 12 inches was suggested in the review. It was also suggested that an additional polymeric coating could be applied to this fresh and clean grout surface.

BLUE, KAREEN↗
DOE OSTI2011

TANK 18 AND 19-F TIER 1A EQUIPMENT FILL MOCK UP TEST SUMMARY

The United States Department of Energy (US DOE) has determined that Tanks 18-F and 19-F have met the F-Tank Farm (FTF) General Closure Plan Requirements and are ready to be permanently closed. The high-level waste (HLW) tanks have been isolated from FTF facilities. To complete operational closure they will be filled with grout for the purpose of: (1) physically stabilizing the tanks, (2) limiting/eliminating vertical pathways to residual waste, (3) discouraging future intrusion, and (4) providing an alkaline, chemical reducing environment within the closure boundary to control speciation and solubility of select radionuclides. Bulk waste removal and heel removal equipment remain in Tanks 18-F and 19-F. This equipment includes the Advance Design Mixer Pump (ADMP), transfer pumps, transfer jets, standard slurry mixer pumps, equipment-support masts, sampling masts, dip tube assemblies and robotic crawlers. The present Tank 18 and 19-F closure strategy is to grout the equipment in place and eliminate vertical pathways by filling voids in the equipment to vertical fast pathways and water infiltration. The mock-up tests described in this report were intended to address placement issues identified for grouting the equipment that will be left in Tank 18-F and Tank 19-F. The Tank 18-F and 19-F closure strategy document states that one of the Performance Assessment (PA) requirements for a closed tank is that equipment remaining in the tank be filled to the extent practical and that vertical flow paths 1 inch and larger be grouted. The specific objectives of the Tier 1A equipment grout mock-up testing include: (1) Identifying the most limiting equipment configurations with respect to internal void space filling; (2) Specifying and constructing initial test geometries and forms that represent scaled boundary conditions; (3) Identifying a target grout rheology for evaluation in the scaled mock-up configurations; (4) Scaling-up production of a grout mix with the target rheology (16 second flow cone value) from 0.25 cubic feet to 4.3 cubic feet. (Ten 0.43 cubic batches were produced because full-scale equipment was not available for the Tier 1A test.); (5) Demonstrating continuous gravity filling of the ADMP mock up test form; (6) Demonstrating continuous gravity filling of 1 inch and 2 inch schedule 40 pipe; and (7) Demonstrating filling of 1 inch and 2 inch schedule 40 pipe from the bottom up by discharging through a tube inserted into the pipes. The Tier 1A mock-up test focused on the ADMP and pipes at least one inch in diameter. The ADMP which is located in center riser of Tank 18-F is a concern because the column for this long-shaft (55 ft) pump is unique and modification to the pump prior to placing it in service limited the flow path options for filling by creating a single flow path for filling and venting the ADMP support column. The large size, vertical orientation, and complicated flow path in the ADMP warrants a detailed description of this piece of ancillary equipment.

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

Mock-Up activities for the extraction of samples from a salt-stone disposal unit - 15502

Mock-up testing with respect to the core-drilling of simulant salt-stone grout was conducted to support the future retrieval of field-emplaced salt-stone samples from salt-stone Disposal Unit (SDU) Cell 2A. The primary objectives of extracting samples from SDU Cell 2A are to enable measurement of field-emplaced samples with respect to properties that influence long-term performance, such as saturated hydraulic conductivity, and to compare the measured properties for field-emplaced and comparable samples prepared in the laboratory. Initial mock-up activities (Phases 1 and 2) were conducted in Fiscal Years (FY) 2013 and 2014 in order to demonstrate the viability of standard core-drilling techniques that are typically employed for sampling concrete structures. The primary requirement for the core-drilling technique was that it should minimize the potential of physical or chemical sample changes that would artificially degrade key grout properties. Mock-up activities were aimed at optimizing the techniques for core-drilling, and subsequent sample extraction, using a set-up that mimicked, to the extent practical, both the physical characteristics, and operational complexities, of core-drilling salt-stone grout from the roof of the SDU. Samples extracted from the grout monolith were subsequently characterized with respect to saturated hydraulic conductivity and compressive strength, and compared to data for cast samples prepared using the same simulant salt-stone material. The comparison of these properties for the two sample types was expected to highlight potential flaws (e.g., micro-cracking) introduced by the core-drilling process. While the data for saturated hydraulic conductivity were virtually identical (approximately 2 E-09 cm/sec), the compressive strength of the core-drilled samples (approximately 3.5 MPa (500 psi)) was on average half that measured for the cast samples. It was suspected that increased water saturation and surface scoring of the core-drilled samples might account for the disparate compressive Strength data. During Phases 1 and 2 it was determined that cores could be successfully drilled and extracted to a depth of approximately 0.9 meters (3 feet) below the grout surface. Phase 3 (FY 2105) has been initiated and is primarily directed at demonstrating the ability to core-drill through approximately 1.8 meters (6 feet) of overlying grout to retrieve the desired sample from the SDU. The original drill depth of 0.6 - 0.9 meters (2-3 feet) was based on an SDU fill height of 5.6 meters (18.5 feet) and sample location of approximately 4.9 meters (16 feet); recently the allowable fill height in the SDUs has been increased to 6.5 meters (21.25 feet); hence the increased depth of overlying grout above the samples to be retrieved. (authors)

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

Development and Characterization of Cementitious Waste Forms for Immobilization of Granular Activated Carbon, Silver Mordenite, and HEPA Filter Media Solid Secondary Waste

Solid secondary waste materials expected to be generated during Hanford Waste Treatment and Immobilization Plant (WTP) operations were characterized (using representative materials) with respect to their ability to retain technetium-99 (Tc), iodine-129 (I), and mercury (Hg) as input to future updates to the Integrated Disposal Facility (IDF) performance assessments (PAs). The waste materials included granular activated carbon (GAC), silver mordenite (AgM), and high-efficiency particulate air (HEPA) filter media; all are used for removal of contaminants and radionuclides from the gaseous effluent treatment systems within the WTP. It is expected that the GAC and AgM will be mixed into a cementitious waste form in which the GAC and AgM particles will be blended/stabilized into the cementitious material. It is also expected that the HEPA filter media will be compacted and placed in a container that is then backfilled with a grout to macroencapsulate the medium. Here we report Kds for all waste materials of interest, examine the physical properties of grout specimens containing the waste materials, and provide solid-state characterization information to further understand the interaction of the waste materials with the encapsulating grout. The Kds are used in PA calculations that estimate contaminant release from the disposal site. Monolithic test specimens were prepared with the GAC and AgM mixed in either a Cast Stone grout formulation (8 weight percent [wt%] ordinary Portland cement [OPC], 45 wt% fly ash [FA], 47 wt% blast furnace slag [BFS]) or a Hanford grout mix 5 (HGM-5) formulation (25 wt% OPC, 75 wt% FA). As the specimens were being prepared, the fluid grout mixes were characterized for processing properties including flowability, set time, and the presence of free liquids during curing. After curing, compressive strengths of the waste forms were measured; the compressive strengths were above 2000 psi, easily exceeding the 500 psi minimum requirement. The cured waste forms were also characterized for their density, porosity, hydraulic conductivity, and water characteristic curve—all properties needed in PA calculations of radionuclide release from the waste forms in the IDF. Finally, EPA Method 1315 leach tests were conducted on the GAC and AgM waste materials encapsulated in the Cast Stone and HGM-5 grouts to determine the rate of release of contaminants from the waste forms. Effective diffusivities are provided, which can be used in future PA analyses of the disposal of these solid secondary waste materials.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Determining the Release of Radionuclides from Tank 18F Waste Residual Solids: FY2016 Report

Pore water leaching studies were conducted on actual Savannah River Site (SRS) Tank 18F residual waste solids to support Liquid Waste tank closure efforts. A test methodology was developed during previous simulant testing to produce slurries of tank residual solids and grout-representative solids in grout pore water solutions (based on SRS groundwater compositions) with pH and E h values expected during the aging of the closed waste tank. The target conditions are provided below where the initial pore water has a reducing potential and a relatively high pH (Reducing Region II). The pore water is expected to become increasingly oxidizing with time (Oxidizing Region II) and during the latter stages of aging (Oxidizing Region III) the pH is expected to decrease. For the reducing case, tests were conducted with both unwashed and washed Tank 18F residual solids. For the oxidizing cases (Oxidizing Regions II and III), all samples were washed with simulated grout pore water solutions prior to testing, since it is expected that these conditions will occur after considerable pore water solution has passed through the system. For the reducing case, separate tests were conducted with representative ground grout solids and with calcium carbonate reagent, which is the grout phase believed to be controlling the pH. Ferrous sulfide (FeS) solids were also added to the reducing samples to lower the slurry E h value. Calcium carbonate solids were used as the grout-representative solid phase for each of the oxidizing cases. Air purge-gas with and without CO 2 removed was transferred through the oxidizing test samples and nitrogen purge-gas was transferred through the reducing test samples during leach testing. The target pH values were achieved to within 0.5 pH units for all samples. Leaching studies were conducted over an E h range of approximately 0.7 V. However, the highest and lowest E h values achieved of ~+0.5 V and ~-0.2 V were significantly less positive and less negative, respectively, than the target values. Achievement of more positive and more negative E h values is believed to require the addition of non-representative oxidants and reductants, respectively.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗