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Langton, C. A.

Publications and source records attributed to Langton, C. A..

Mercury Speciation and Stabilization in Saltstone - 19103

Mercury is a contaminant of concern in Savannah River Site (SRS) high level waste (HLW). For five decades elemental mercury was used in the catalytic dissolution of aluminum cladding from the enriched-alloy uranium recovery process. Over 60,000 kg of mercury are now distributed in the SRS HLW tanks. The mercury speciation in the liquid waste streams resulting from conditioning HLW sludge for vitrification and in the decontaminated low activity sodium salt solution removed from the tanks was initially thought to be primarily ionic with a minor amount of elemental mercury. Recent sampling detected organic mercury, primarily methylmercury, HgCH{sub 3}{sup +} (MeHg{sup +}), and a trace amount of ethylmercury (EtHg) in these streams in addition to the ionic and elemental forms of mercury. The objective of this work was to identify the fate of the organic mercury in saltstone, a waste form containing portland cement, slag cement, and Class F fly ash. This information is needed to evaluate total mercury and organic mercury limits for the saltstone Waste Acceptance Criteria to assure regulatory compliance with mixed waste disposal requirements and to evaluate opportunities to enhance the waste form performance. Results to date indicate that the MeHg{sup +} reacts with sulfide in the cementitious reagents, slag in particular, to form nanoparticles of β-HgS, meta cinnabar, which is very insoluble and has a solubility product in water, pK{sub sp}, at 25 deg. C of 53. (authors)

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Review of Cementitious Materials Development and Applications That Have Supported DOE-EM Missions: Waste Treatment, Conditioning, Containment Structures, Tank Closures, Facility Decommissioning, Environmental Restoration, and Structural Assessments

The Department of Energy (DOE) is tasked with managing the legacy defense wastes that resulted from nuclear materials production and nuclear arms development. Nuclear-waste management encompasses generation, processing (treatment and packaging), storage, transport, and disposal. To date, there are over 100 million gallons of liquid radioactive and chemical mixed wastes within the Department of Energy complex as well as solid waste, debris, and environmental restoration media that require disposal. DOE has been able to meet the challenges involved in dispositioning this waste using unique technical approaches and application-specific data required due to the nature of the constituents to be managed (e.g., long-lived radionuclides and highly mobile radionuclides in the near surface environments). Cementitious materials have played a prominent role historically in the successful disposition of these wastes, in the reduction of risk to the public, and in the closure of decommissioned tanks and facilities across the DOE complex.

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Methylmercury Speciation and Retention Evaluation to Support Saltstone Waste Acceptance Criteria

Mercury is a contaminant of concern in Savannah River Site (SRS) high level waste (HLW). For five decades elemental mercury was used in the catalytic dissolution of aluminum cladding from the enrichedalloy uranium recovery process. Over 60,000 kg of mercury are now distributed in the SRS HLW tanks. The mercury speciation in the liquid waste streams resulting from conditioning HLW sludge for vitrification and in the decontaminated low activity sodium salt solution removed from the tanks was initially thought to be primarily ionic with a minor amount of elemental mercury. Recent sampling detected organic mercury, primarily methylmercury, HgCH 3 + (MeHg + ), and a trace amount of ethylmercury (EtHg) in these streams in addition to the ionic and elemental forms.

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Thermal Modeling Study for Geologic Borehole Conceptual Design - 17148

Instituto de Pesquisas Energeticas e Nucleares (IPEN-CNEN/SP) is developing a strategy for safe, permanent disposal of disused sealed radioactive sources (DSRS) from industrial and medical applications within Brazil. The Institute is proposing modifications to the International Atomic Energy Agency (IAEA) Borehole Disposal of Sealed Radioactive Sources (BOSS) concept originally developed by the Nuclear Energy Corporation of South Africa. The current Brazilian modified design differs from the IAEA design in that the disposal zone is below 300 m versus 30 m of the boss concept, and will be used to dispose of a much larger number of DSRS. These modifications result in a considerable departure from the generic safety case established by IAEA. Therefore, a new safety case is required to assess radiological and thermal impacts among other considerations. Predictive modeling and simulations were performed to address impacts of the proposed borehole concept at the early design stage in order to provide timely improvements to the concept and a traceable rationale for decisions made throughout the program as required by the safety case. Preliminary objectives of the modeling effort were focused on evaluating the mechanical and thermal loads anticipated within the current Brazilian borehole disposal concept in order to assess potential material and design issues. This paper presents the thermal modeling predictions and performance results for the proposed BOSS design. (authors)

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Test Methods for Cementitious Seal Materials for Borehole Disposal - 17352

The Nuclear and Energy Research Institute (IPEN-CNEN/SP) in Sao Paulo-Brazil, is considering borehole disposal of disused sealed radioactive sources (DSRS), which were used in smoke detectors, lightning arresters, radiotherapy, industrial gauges, irradiators, and other applications. The current IPEN concept of borehole is a modified BOSS system developed by the International Atomic Energy Agency (IAEA). It differs from the IAEA's design in that the disposal zone is below 300 m, and the DSRS are placed directly in the disposal packages constituted of stainless steel containers with 1.5 L capacity. A borehole drilled through sediment and granite, stabilized with stainless steel casing and cement grout is proposed for the conceptual model. Standard cement-material test methods and performance specific test methods, including accelerated aging methods, are needed for modeling the performance of the candidate cementitious grouts. A cross-disciplinary team from the USA Savannah River National laboratory is providing technical assistance to IPEN in this performance assessment. (authors)

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Characterization of Laboratory Prepared Concrete Pastes Exposed to High Alkaline and High Sodium Salt Solutions

The objective of this study was to identify potential chemical degradation mechanisms for the Saltstone Disposal Unit (SDU) concretes, which over the performance life of the structures may be exposed to highly alkaline sodium salt solutions containing sulfate, hydroxide, and other potentially corrosive chemicals in salt solution and saltstone flush water, drain water, leachate and / or pore solution. The samples analyzed in this study were cement pastes prepared in the SIMCO Technologies, Inc. concrete laboratory. They were based on the paste fractions of the concretes used to construct the Saltstone Disposal Units (SDUs). SDU 1 and 4 concrete pastes were represented by the PV1 test specimens. The paste in the SDU 2, 3, 5, and 6 concrete was represented by the PV2 test specimens. SIMCO Technologies, Inc. selected the chemicals and proportions in the aggressive solutions to approximate proportions in the saltstone pore solution [2, 3, 5, and 6]. These test specimens were cured for 56 days in curing chamber before being immersed in aggressive solutions. After exposure, the samples were frozen to prevent additional chemical transport and reaction. Selected archived (retrieved from the freezer) samples were sent to the Savannah River National Laboratory (SRNL) for additional characterization using x-ray diffraction (XRD), scanning electron microscopy (SEM), and energy dispersive x-ray (EDX) spectroscopy. Characterization results are summarized in this report. In addition, a correlation between the oxide composition of the pastes and their chemical durability in the alkaline salt solutions is provided.

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Cementitious Barriers Partnership - FY2015 End-Year Report

The DOE-EM Office of Tank Waste Management Cementitious Barriers Partnership (CBP) is chartered with providing the technical basis for implementing cement-based waste forms and radioactive waste containment structures for long-term disposal. Therefore, the CBP ultimate purpose is to support progress in final treatment and disposal of legacy waste and closure of High-Level Waste (HLW) tanks in the DOE complex. This status report highlights the CBP 2015 Software and Experimental Program efforts and accomplishments that support DOE needs in environmental cleanup and waste disposal. DOE needs in this area include: Long-term performance predictions to provide credibility (i.e., a defensible technical basis) for regulator and DOE review and approvals, Facility flow sheet development/enhancements, and Conceptual designs for new disposal facilities. In 2015, the CBP developed a beta release of the CBP Software Toolbox – “Version 3.0”, which includes new STADIUM carbonation and damage models, a new SRNL module for estimating hydraulic properties and flow in fractured and intact cementitious materials, and a new LeachXS/ORCHESTRA (LXO) oxidation module. In addition, the STADIUM sulfate attack and chloride models have been improved as well as the LXO modules for sulfate attack, carbonation, constituent leaching, and percolation with radial diffusion (for leaching and transport in cracked cementitious materials). These STADIUM and LXO models are applicable to and can be used by both DOE and the Nuclear Regulatory Commission (NRC) end-users for service life prediction and long-term leaching evaluations of radioactive waste containment structures across the DOE complex.

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X-Ray Diffraction of Slag-Based Sodium Salt Waste Forms - 15513

Cementitious materials are used to solidify and stabilize aqueous based radioactive waste containing sodium salts. The types and proportions of cementitious ingredients used to treat aqueous radioactive waste streams containing sodium salts depend on the performance objectives for the waste forms and the compositions of the waste streams. This paper documents sample preparation and x-ray diffraction results for a series of materials made with water or highly alkaline sodium salt simulated waste water and cementitious binders. The objective of this study was to: 1) generate a base line for the evolution of the waste form as a function of time and conditions, 2) design new binders based on mineralogy of the binder, 3) understand and predict anion and cation leaching behavior of contaminants of concern, and 4) predict performance of the waste forms for which phase solubility and thermodynamic data are available. Characterization of the mineralogy is also important for understanding the buffering effects that the waste form has on infiltrating water / leachates. In summary, mixtures of Type II portland cement, Grade 100 ground granulated blast furnace slag (GGBFS) and carbon burn-out (CBO) Class F Fly ash which were hydrated with water contained hydrated phase assemblages typical of those reported in the literature. The calcium silicate hydrate phase assemblage in samples hydrated with the alkaline 4.4 M sodium salt simulated waste solution was found to be a function of the (CaO + MgO) / (SiO{sub 2} + Al{sub 2}O{sub 3}) ratio of the samples characterized. No significant differences were detected in samples cured 2 months and 14 months in sealed containers at ambient indoor temperatures. Slag and a blend of slag and cement hydrated with caustic 4.4 M Na salt solution resulted in the most crystalline matrix. In addition to poorly ordered C-S-H, these samples contained fairly well ordered C-S-H I (a precursor of 14A tobermorite) and 11 A Al-substituted tobermorite. These crystalline C-S-H phases did not form or were present in only trace amounts in slag blends containing about 45 to 62 mass percent fly ash. These slag-Class F fly ash blends had a higher silica plus alumina content relative to lime and magnesia than the blends that produced C-S-H I and Al-substituted tobermorite. The calcium silicate binder in the 10:45:45 mixture of cement: slag: fly ash was made up of poorly ordered C-S-H. The sample cured for 14 months may contain a small amount of the more crystalline calcium silicate hydrate phases. Layered double hydroxides in the hydrotalcite (magnesium-aluminum carbonate hydroxide) and hydrocalumite / AFm phases (calcium aluminum hydroxide) were present in mixtures containing slag. The specific phase(s) were not identified because these phases form solid solutions and have a considerable amount of overlap in their x-ray patterns. Sodium nitrate was the only sodium salt phase identified in x-ray diffraction patterns of the samples hydrated with salt solution. Drying during x-ray diffraction sample preparation may have resulted in precipitation of the sodium nitrate or it may have been present in the samples prior to x-ray sample preparation. Sodium sulfate, aluminate, and carbonate may have been incorporated in the structures of the layered double hydroxide (AFm) type phases. These mixed metal layered double hydroxides make up an important fraction of the matrix in the slag containing blends hydrated with caustic salt solution. They are among the few oxide-based phases that exhibit substantial, permanent anion exchange capacity [Kirkpatrick, et al. 1999, Plamer, et al., 2009, and Zhang and Reardon, 2003]. They also contribute to the structural properties of cementitious matrices [Taylor, 1997]. (authors)

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Technetium oxidation in slag-based sodium salt waste forms exposed to water and moist Hanford soil - 15514

Several U.S. DOE sites use or plan to use waste forms and/or concrete containment structures for radioactive waste disposal that are designed to have a chemically reducing environment to immobilize selected contaminants such as Tc(VII)O{sub 4}{sup -} and Cr(VI)O{sub 4}{sup 2-}. These waste forms and containment structures are typically deployed in near surface unsaturated oxidizing environments. Consequently, the effect of exposure to air (oxygen) and water containing dissolved oxygen during production, during the period of institutional control, and over the long term period of performance is important for predicting the speciation and mobility of the redox sensitive radioactive and stable contaminants. Both the SRS and Hanford waste streams contain soluble technetium which may require stabilization to meet disposal requirements. Technetium stabilization is a difficult problem because: 1) Tc is soluble and very mobile in the oxidized form typical of near surface environments, and 2) Tc-99 is a long-lived isotope with a half-life of 2.1 E+05 years which places demanding requirements on the engineered barriers and environment to meet current regulatory disposal requirements. A depth-discrete sampling and leaching method approach for measuring contaminant oxidation rate (effective contaminant specific oxidation rate) was used in this study. The method was modified by coating all sides of a cylindrical sample with an impermeable epoxy and cutting a fresh surface 2 to 2.5 cm from the original top surface eliminates sample inhomogeneity as the result of settling as a reason from observed results and provides 1-D soluble ion transport and gas transport information. Soluble Tc was leached from all of the depth-discrete sub-samples from both Tc2-9 and Tc2-10 which strongly suggests that oxygen was present in the entire length of both samples. About 24 mass percent of the Tc in the original sample, was leached (soluble) from sub-samples between 0.8 and 46 mm below the exposed surface of Tc2-9 (exposed to Hanford sediment). The same percent (24%) was leached from the sub-samples between 0.8 and 11 mm below the exposed surface of Tc2-10 (exposed to DI water). This suggests that the rate of oxygen migration into the sample exposed to soil was faster than the rate of migration into the sample exposed to water which is consistent with the more rapid transport of ions through a gas phase as compared to a liquid phase. It is assumed that moisture in the Hanford sediment was not sufficient to completely block the surface pores with respect to gas transport across the soil-waste form boundary. Based on nitrate leaching results for the depth- discrete sub-samples, regions depleted in nitrates were identified from the top surfaces to 9.5 and 3 mm into samples Tc2-9 (exposed to moist Hanford sediment) and Tc2-10 (DI water). Low mass fractions of nitrate were leached from these depth-discrete samples compared to samples further from the exposed surface presumably because a significant portion of the nitrate had already migrated into the soil or water, respectively. Depth-discrete sub-sample leaching results for Na can be interpreted in the same way over the same regions in the two samples tested. In conclusion, leaching monolithic porous cementitious waste forms in water appears to be conservative for non-redox sensitive contaminants. However, leaching data obtained under saturated exposure conditions do not appear to be conservative for redox sensitive contaminants which are easily oxidized. Leaching crushed samples in water still seems to be a conservative approach to estimating the concentrations of soluble contaminants in a waste form. (authors)

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Cementitious Barriers Partnerships (FY2015 Mid-Year Status Report)

The DOE-EM Office of Tank Waste Management Cementitious Barriers Partnership (CBP) is chartered with providing the technical basis for implementing cement-based waste forms and radioactive waste containment structures for long-term disposal. Therefore, the CBP ultimate purpose is to support progress in final treatment and disposal of legacy waste and closure of High-Level Waste (HLW) tanks in the DOE complex. This status report highlights the CBP 2015 Software and Experimental Program efforts and accomplishments that support DOE needs in environmental cleanup and waste disposal. DOE needs in this area include: Long-term performance predictions to provide credibility (i.e., a defensible technical basis) for regulator and DOE review and approvals, Facility flow sheet development/enhancements, and Conceptual designs for new disposal facilities. In 2015, the CBP plans to release its newest version, the CBP Software Toolbox – “Version 3.0”, which will include new STADIUM carbonation and damage models, a new SRNL module for transport properties and flow in fractured and in-tact cementitious materials, and a new LeachXS/ORCHESTRA (LXO) oxidation module. In addition, improved STADIUM sulfate attack and chloride models will be included. This is in addition to the LXO modules for sulfate attack, carbonation, constituent leaching, and percolation with radial diffusion (for leaching and transport in cracked cementitious materials), of which will also be improved for Version 3.0. These STADIUM and LXO models are applicable and can be used by both DOE and the Nuclear Regulatory Commission (NRC) for service life and long-term performance evaluations and predictions of nuclear and radioactive waste containment structures across the DOE complex. In 2015, the Cementitious Barriers Partnership is providing tangible progress toward fulfilling the objective of developing a set of software tools and experimental programs to improve understanding and prediction of the long-term structural, hydraulic and chemical performance of cementitious barriers used in nuclear applications. To reflect this progress, CBP partners authored and are currently drafting many reports including six papers that were presented at WM2015.

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X-ray diffraction of slag-based sodium salt waste forms

The attached report documents sample preparation and x-ray diffraction results for a series of cement and blended cement matrices prepared with either water or a 4.4 M Na salt solution. The objective of the study was to provide initial phase characterization for the Cementitious Barriers Partnership reference case cementitious salt waste form. This information can be used to: 1) generate a base line for the evolution of the waste form as a function of time and conditions, 2) potentially to design new binders based on mineralogy of the binder, 3) understand and predict anion and cation leaching behavior of contaminants of concern, and 4) predict performance of the waste forms for which phase solubility and thermodynamic data are available.

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X-Ray Diffraction of Slag-Based Sodium Salt Waste Forms

Cementitious materials are used to solidify and stabilize aqueous based radioactive waste containing sodium salts. The types and proportions of cementitious ingredients used to treat aqueous radioactive waste streams containing sodium salts depend on the performance objectives for the waste forms and the compositions of the waste streams. Matrix phases can stabilize certain contaminants (co-precipitation, substitution, ion exchange, and / or sorption), influence processing properties, and are responsible for physical properties and durability of the cured waste forms. Consequently, characterization of the matrix (binder) mineralogy (chemical compositions and crystalline / non crystalline structures) is important for predicting contaminant leaching and evolution of the materials as a function of time and changing conditions This report documents sample preparation and x-ray diffraction results for a series of mixtures of sodium salt waste and cementitious binders. The objective of this study was to provide initial phase characterization for the CBP reference case cementitious salt waste form. This information can be used to: 1) generate a base line for the evolution of the waste form as a function of time and conditions, 2) potentially to design new binders based on mineralogy of the binder, 3) understand and predict anion and cation leaching behavior of contaminants of concern, and 4) predict performance of the waste forms for which phase solubility and thermodynamic data are available. Characterization of the mineralogy is also important for understanding the buffering effects that the waste form has on infiltrating water / leachates. More specifically, identification of hydrated phases capable of sequestering anions in the structures and crystallinity of the calcium silicate binder phases were of particular interest. The intent was to use this characterization data as a starting point for more detailed phase characterization using neutron diffraction techniques in addition to quasi-elastic neutron scattering techniques for characterization of water at the ORNL Spallation Neutron Source, Oak Ridge, TN. The initial characterization is complete. Due to extensive substitutions of cations and anions in the layered double hydroxide phases and the very fine intermixing of poorly crystalline hydrated phases in the reference case blend (10 : 45 : 45 cement : slag : fly ash), electron diffraction and transmission electron spectroscopy are recommended as the next step for characterization. In summary, the hydrated mixtures of Type II portland cement, Grade 100 ground granulated blast furnace slag (GGBFS) and carbon burn-out (CBO) Class F Fly ash contained hydrated phase assemblages which were typical of those reported in the literature. Based on x-ray diffraction results, no significant differences were detected in samples cured 2 months and 14 months in sealed containers at ambient indoor temperatures.

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Cast Stone Oxidation Front Evaluation: Preliminary Results For Samples Exposed To Moist Air

The rate of oxidation is important to the long-term performance of reducing salt waste forms because the solubility of some contaminants, e.g., technetium, is a function of oxidation state. TcO 4 - in the salt solution is reduced to Tc(IV) and has been shown to react with ingredients in the waste form to precipitate low solubility sulfide and/or oxide phases. Upon exposure to oxygen, the compounds containing Tc(IV) oxidize to the pertechnetate ion, Tc(VII)O 4 - , which is very soluble. Consequently the rate of technetium oxidation front advancement into a monolith and the technetium leaching profile as a function of depth from an exposed surface are important to waste form performance and ground water concentration predictions. An approach for measuring contaminant oxidation rate (effective contaminant specific oxidation rate) based on leaching of select contaminants of concern is described in this report. In addition, the relationship between reduction capacity and contaminant oxidation is addressed. Chromate (Cr(VI) was used as a non-radioactive surrogate for pertechnetate, Tc(VII), in Cast Stone samples prepared with 5 M Simulant. Cast Stone spiked with pertechnetate was also prepared and tested. Depth discrete subsamples spiked with Cr were cut from Cast Stone exposed to Savannah River Site (SRS) outdoor ambient temperature fluctuations and moist air. Depth discrete subsamples spiked with Tc-99 were cut from Cast Stone exposed to laboratory ambient temperature fluctuations and moist air. Similar conditions are expected to be encountered in the Cast Stone curing container. The leachability of Cr and Tc-99 and the reduction capacities, measured by the Angus-Glasser method, were determined for each subsample as a function of depth from the exposed surface. The results obtained to date were focused on continued method development and are preliminary and apply to the sample composition and curing / exposure conditions described in this report. The Cr oxidation front (depth to which soluble Cr was detected) for the Cast Stone sample exposed for 68 days to ambient outdoor temperatures and humid air (total age of sample was 131 days) was determined to be about 35 mm below the top sample surface exposed. The Tc oxidation front, depth at which Tc was insoluble, was not determined. Interpretation of the results indicates that the oxidation front is at least 38 mm below the exposed surface. The sample used for this measurement was exposed to ambient laboratory conditions and humid air for 50 days. The total age of the sample was 98 days. Technetium appears to be more easily oxidized than Cr in the Cast Stone matrix. The oxidized forms of Tc and Cr are soluble and therefore leachable. Longer exposure times are required for both the Cr and Tc spiked samples to better interpret the rate of oxidation. Tc spiked subsamples need to be taken further from the exposed surface to better define and interpret the leachable Tc profile. Finally Tc(VII) reduction to Tc(IV) appears to occur relatively fast. Results demonstrated that about 95 percent of the Tc(VII) was reduced to Tc(IV) during the setting and very early stage setting for a Cast Stone sample cured 10 days. Additional testing at longer curing times is required to determine whether additional time is required to reduce 100 % of the Tc(VII) in Cast Stone or whether the Tc loading exceeded the ability of the waste form to reduce 100 % of the Tc(VII). Additional testing is required for samples cured for longer times. Depth discrete subsampling in a nitrogen glove box is also required to determine whether the 5 percent Tc extracted from the subsamples was the result of the sampling process which took place in air. Reduction capacity measurements (per the Angus-Glasser method) performed on depth discrete samples could not be correlated with the amount of chromium or technetium leached from the depth discrete subsamples or with the oxidation front inferred from soluble chromium and technetium (i.e., effective Cr and Tc oxidation fronts). Residual reduction capacity in the oxidized region of the test samples indicates that the remaining reduction capacity is not effective in re-reducing Cr(VI) or Tc(VII) in the presence of oxygen. Depth discrete sampling and leaching is a useful for evaluating Cast Stone and other chemically reducing waste forms containing ground granulated blast furnace slag (GGBFS) or other reduction / sequestration reagents to control redox sensitive contaminant chemistry and leachability in the near surface disposal environment. Based on results presented in this report, reduction capacity measured by the Angus-Glasser Ce(IV) method is not an appropriate or meaningful parameter for determining or predicting Tc and Cr oxidation / retentions, speciation, or solubilities in cementitious materials such as Cast Stone. A model for predicting Tc(IV) oxidation to soluble Tc(VII) should consider the waste form porosity (pathway for oxygen ingress), oxygen source, and the contaminant specific oxidation rates and oxidation fronts. Depth discrete sampling of materials exposed to realistic conditions in combination with short term leaching of crushed samples has potential for advancing the understanding of factors influencing performance. This information can be used to support conceptual model development.

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Cementitious Barriers Partnership FY2013 End-Year Report

In FY2013, the Cementitious Barriers Partnership (CBP) demonstrated continued tangible progress toward fulfilling the objective of developing a set of software tools to improve understanding and prediction of the long-term structural, hydraulic and chemical performance of cementitious barriers used in nuclear applications. In November 2012, the CBP released “Version 1.0” of the CBP Software Toolbox, a suite of software for simulating reactive transport in cementitious materials and important degradation phenomena. In addition, the CBP completed development of new software for the “Version 2.0” Toolbox to be released in early FY2014 and demonstrated use of the Version 1.0 Toolbox on DOE applications. The current primary software components in both Versions 1.0 and 2.0 are LeachXS/ORCHESTRA, STADIUM, and a GoldSim interface for probabilistic analysis of selected degradation scenarios. The CBP Software Toolbox Version 1.0 supports analysis of external sulfate attack (including damage mechanics), carbonation, and primary constituent leaching. Version 2.0 includes the additional analysis of chloride attack and dual regime flow and contaminant migration in fractured and non-fractured cementitious material. The LeachXS component embodies an extensive material property measurements database along with chemical speciation and reactive mass transport simulation cases with emphasis on leaching of major, trace and radionuclide constituents from cementitious materials used in DOE facilities, such as Saltstone (Savannah River) and Cast Stone (Hanford), tank closure grouts, and barrier concretes. STADIUM focuses on the physical and structural service life of materials and components based on chemical speciation and reactive mass transport of major cement constituents and aggressive species (e.g., chloride, sulfate, etc.). THAMES is a planned future CBP Toolbox component focused on simulation of the microstructure of cementitious materials and calculation of resultant hydraulic and constituent mass transfer parameters needed in modeling. Two CBP software demonstrations were conducted in FY2013, one to support the Saltstone Disposal Facility (SDF) at SRS and the other on a representative Hanford high-level waste tank. The CBP Toolbox demonstration on the SDF provided analysis on the most probable degradation mechanisms to the cementitious vault enclosure caused by sulfate and carbonation ingress. This analysis was documented and resulted in the issuance of a SDF Performance Assessment Special Analysis by Liquid Waste Operations this fiscal year. The two new software tools supporting chloride attack and dual-regime flow will provide additional degradation tools to better evaluate performance of DOE and commercial cementitious barriers. The CBP SRNL experimental program produced two patent applications and field data that will be used in the development and calibration of CBP software tools being developed in FY2014. The CBP software and simulation tools varies from other efforts in that all the tools are based upon specific and relevant experimental research of cementitious materials utilized in DOE applications. The CBP FY2013 program involved continuing research to improve and enhance the simulation tools as well as developing new tools that model other key degradation phenomena not addressed in Version 1.0. Also efforts to continue to verify the various simulation tools through laboratory experiments and analysis of field specimens are ongoing and will continue into FY2014 to quantify and reduce the uncertainty associated with performance assessments. This end-year report summarizes FY2013 software development efforts and the various experimental programs that are providing data for calibration and validation of the CBP developed software.

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Grout Long Radius Flow Testing to Support Saltstone Disposal Unit 6 Design - 13352

The Saltstone Facility, located within the Savannah River Site (SRS) near Aiken, South Carolina, consists of two facility segments: The Saltstone Production Facility (SPF) and the Saltstone Disposal Facility (SDF). The SPF receives decontaminated legacy low level sodium salt waste solution that is a byproduct of prior nuclear material processing. The salt solution is mixed with cementitious materials to form a grout slurry known as 'Saltstone'. The grout is pumped to the SDF where it is placed in a Saltstone Disposal Unit (SDU) to solidify. SDU 6 is referred to as a 'mega vault' and is currently in the design stage. The conceptual design for SDU 6 is a single cell, cylindrical geometry approximately 114.3 meters in diameter by 13.1 meter high and is larger than previous cylindrical SDU designs, 45.7 meters in diameter by 7.01 meters high (30 million gallons versus 2.9 million gallons of capacity). Saltstone slurry will be pumped into the new waste disposal unit through roof openings at a projected flow rate of about 34.1 cubic meters per hour. Nine roof openings are included in the design to discharge material into the SDU with an estimated grout pour radius of 22.9 to 24.4 meters and initial drop height of 13.1 meters. The conceptual design for the new SDU does not include partitions to limit the pour radius of the grout slurry during placement other than introducing material from different pour points. This paper addresses two technical issues associated with the larger diameter of SDU 6; Saltstone flow distance in a tank 114.3 meters in diameter and quality of the grout. A long-radius flow test scaled to match the velocity of an advancing grout front was designed to address these technology gaps. The emphasis of the test was to quantify the flow distance and to collect samples to evaluate cured properties including compressive strength, porosity, density, and saturated hydraulic conductivity. Two clean cap surrogate mixes (Saltstone premix plus water) were designed to simulate slurry with the reference Saltstone rheology and a Saltstone with extra water from the process flushing operation. Long-radius flow tests were run using approximately 4.6 cubic meters of each of these mixes. In both tests the pump rate was 0.063 liters/second (1 gpm). A higher pump rate, 0.19 liters/second (3 gpm), was used in a third long-radius flow test. The angle of repose of the grout wedges increased as a function of time in all three tests. The final angles of repose were measured at 3.0 deg., 2.4 deg., and 0.72 deg.. The pump rate had the largest effect on the radial flow distance and slope of the grout surface. The slope on the pour placed at 0.19 liters/second (3 gpm) was most representative of the slope on the grout currently being pumped into SDU 2 which is estimated to be 0.7 deg. to 0.9 deg. The final grout heights at 1/3 of a meter from the discharge point were 115, 105, and 38 cm. Entrapped air (≥ 0.25 cm bubbles) was also observed in all of the mixes. The entrapped air appeared to be released from the flows within about 3.1 meters (10 feet) of the discharge point. The bleed water was clear but had a thin layer of floating particulates. The bleed water should be retrievable by a drain water collection system in SDU 6 assuming the system does not get clogged. Layering was observed and was attributed to intervals when the hopper was being cleaned. Heat from the hydration reactions was noticeable to the touch. (authors)

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Salt-stone Oxidation Study: Leaching Method - 13092

Cementitious waste forms can be designed to chemically stabilize selected contaminants, such as Tc{sup +7} and Cr{sup +6}, by chemically reduction to lower valance states, Tc{sup +4} and Cr{sup +3}, respectively, and precipitation of these species in alkaline media as low solubility solid phases. Data for oxidation of this type of cementitious waste form cured under field conditions as a function of time is required for predicting the performance of the waste form and disposal facility. The rate of oxidation (oxidation front advancement) is an important parameter for predicting performance because the solubilities of some radionuclide contaminants, e.g., technetium, are a function of the oxidation state. A non-radioactive experiment was designed for quantifying the oxidation front advancement using chromium, as an approximate redox-sensitive surrogate (Cr{sup +6} / Cr{sup +3}) for technetium (Tc{sup +7} / Tc{sup +4}). Nonradioactive cementitious waste forms were prepared in the laboratory and cured under both laboratory and 'field conditions'. Laboratory conditions were ambient temperature and sealed sample containers. Field conditions were approximated by curing samples in open containers which were placed inside a plastic container stored outdoors at SRS. The container had a lid and was instrumented with temperature and humidity probes. Sub-samples as thin as 0.2 mm were taken as a function of distance from the exposed surface of the as-cast sample. The sub-samples were leached and the leachates were analyzed for chromium, nitrate, nitrite and sodium. Nitrate, nitrite, and sodium concentrations were used to provide baseline data because these species are not chemically retained in the waste form matrix to any significant extent and are not redox sensitive. 'Effective' oxidation fronts for Cr were measured for samples containing 1000, 500 and 20 mg/kg Cr added as soluble sodium chromate, Na{sub 2}CrO{sub 4}. For a sample cured for 129 days under field conditions, leachable Cr (assumed to be the oxidized form, i.e., Cr{sup +6} was detected in the top 15 to 20 mm of the sample spiked with 1000 mg/kg Cr. Below about 20 mm, the Cr concentrations in leachates were below the detection limit (< 0.010 mg/L) which indicates that the oxidation as the result of exposure to air was limited to the top 20 mm of the sample after exposure for 129 days and that the bulk of the waste form was not affected, i.e., the Cr was stabilized and insoluble. For samples cured in the laboratory, leachable Cr was detected in the top 8 mm of the Cr 1000 sample cured in the laboratory for 37 days. Between 8 and 14 mm, the concentration Cr in the leachate dropped by a factor of about 20 to just above the detection limit. These depth of penetration results indicate that the rate of advancement of the oxidation front for samples spiked with 1000 mg/kg Cr cured under 'field conditions' for 129 days is less than that for the sample cured in the laboratory for 37 days, i.e., 0.156 and 0.216 mm/day, respectively. Additional data are presented for samples spiked with 500 and 20 mg/kg Cr. In summary, cementitious waste forms are porous solids with a network of interconnected pores ranging in diameter from 10 E-10 m to greater than a few mm. The oxidation process is assumed to occur as the result of oxygen transport through the interconnected porosity which may be filled with air, aqueous salt solution, or both. Upon oxidation, the Cr becomes soluble and can be transported in solution through aqueous pore fluid or leachate. (authors)

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