Effect of Temperature on Local Hydration of Zn in Hematite
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Mergelsberg, Sebastian T.↗
Engineering topics
Saslow, Sarah A.
Publications and source records attributed to Saslow, Sarah A..
Evaluation of Degradation Mechanisms for Solid Secondary Waste Grout Waste Forms
The overall objective of this work is to provide defensibility for the long-term performance of grouted Hanford SSW streams when disposed in a near surface disposal facility, IDF, on the Hanford Site. Providing defensibly for the long-term performance of the grouted waste forms is consistent with the research and development activities identified in the Performance Assessment Maintenance Plan, (Westcott et al. 2019), that are necessary to address the assumptions made in the PA. Specifically, this work addresses two areas identified for further research and development activities in the plan: (1) “Evaluate ongoing research on transport characteristics of cementitious materials using accelerated tests to approximate the effects of aging/alteration/weathering”; and (2) “Evaluate ongoing research on microbial effects on transport processes in cementitious materials.” The assembled subject matter expert team evaluated a list of degradation mechanisms and supporting processes and provided rankings of areas where further research and development (R&D) are needed. From this assessment, high priority R&D areas include: (1) the effects of carbonation, Ca leaching, and SSW dimensional change in grout waste forms; (2) updated model representations of grouted waste forms; and (3) scaled testing demonstrations. Moderate priority items including a paper study on possible microbial influence, reoxidation rates, radionuclide/contaminant dissolution from SSW in the grout and freeze thaw behavior. Other processes evaluated were either deemed unlikely to occur, to have little impact on the SSW waste forms, or to occur at time frames beyond those considered (>10,000 years). The assessments and proposed R&D approaches are expected to support an update to the WRPS SSW roadmap.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
An exploration of benchtop X–ray emission spectroscopy for precise characterization of the sulfur redox state in cementitious materials
The evolution of sulfur chemistry in cements is best known in the bailiwick of failure mechanisms via sulfate attack but is equally important for its contributions to the reduction capacity of cementitious materials often used for immobilizing nuclear waste streams destined for long-term storage, e.g., cementitious waste forms (CWF). The total reduction capacity of CWFs, encompassing contributions from both S and Fe reductants, and its implications toward radionuclide immobilization is most often studied by destructive wet chemistry methods requiring acid digestion in the presence of Ce(IV) and subsequent titration and colorimetric interpretation. Here, we investigate a similarly analytical but nondestructive alternative, benchtop high resolution wavelength-dispersive x-ray fluorescence spectroscopy, most commonly known as x-ray emission spectroscopy (XES), for probing the bulk sulfur oxidation state distribution. We present here an initial investigation of S XES, including an improved experimental protocol for lab XES of inhomogeneous samples, both as a complement to the Ce(IV) test and for new scientific opportunities that it enables for observing changes in sulfur chemistry. We discuss future improvements and opportunities, including: (1) the practical challenges associated with coordinating XES and Ce(IV) liquid extraction for a more comprehensive perspective on reduction capacity and for a high-precision evaluation of uncertainties in the Ce(IV) test; and (2) new opportunities, due to the nondestructive nature of XES, for controlled evolution studies aimed at elucidating specific chemical responses of CWF’s exposed to invasive gas or liquid species or to accelerated aging by radiative dose or thermal treatment.
36 MATERIALS SCIENCE↗
Vanadium Oxidation States and Structural Role in Aluminoborosilicate Glasses: An Integrated Experimental and Molecular Dynamics Simulation Study
Not Available
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Combined Technologies for In Situ Remediation of Tc-99 and U in Subsurface Sediments
In this study, combinations of chemical remedies were tested in bench-scale batch experiments to evaluate a two-step reduction-sequestration approach to effectively stabilize high concentrations of inorganic contaminant mixtures. Bench tests simulated contaminant and geochemical conditions of a perched aquifer located within the Central Plateau at the Hanford Site, located in southeastern Washington State (USA). Pairwise combinations of a reductant [e.g., zero valent iron, sulfur modified iron (SMI), or calcium polysulfide] and a sequestering agent [e.g., calcite, apatite, or dilute alkaline solution (e.g., NaOH)] were evaluated for immobilization and stabilization of technetium (Tc) (50,000 pCi/L), uranium (U) (150 mg/L), and nitrate (NO 3 ) (200 mg/L) in high ionic strength groundwater. The results of these batch studies demonstrated that reduction by SMI and sequestration in apatite or calcite are the most effective combination for these contaminant mixtures and conditions. Aqueous concentrations of Tc and U decreased by 95.6% ± 2.5% and 101.1% ± 5.2%, respectively, with SMI-apatite and 98.3% ± 0.0% and 101.2% ± 5.2%, respectively, with SMI-calcite. Sequential extractions showed that sequestered contaminants had limited capacity for re-oxidation; in fact, less than 10% of immobilized Tc and U was recovered by selective extraction of mineral phases most susceptible to oxidation. In addition, X-ray absorption near edge structure analysis of the sediment samples treated with SMI-calcite showed the presence of only U(IV), while both U(IV) and U(VI) were present in the SMI apatite combination [ratio of 0.43 U(IV):0.59 U(VI)].This study describes preliminary results that a two-step approach for stabilizing contaminant mixtures of long-lived radionuclides can be effective at reducing contaminant fluxes to groundwater from vadose and perched water zones.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Micrometer-sized Magnetite Synthesis using Fe(OH)2(s) as a Precursor for Technetium Sequestration from Liquid Nuclear Waste Streams
Systematic batch experiments under variable adjusted physicochemical conditions were conducted to explore optimization of micrometer-sized magnetite synthesis for Tc sequestration from radionuclide waste streams using Fe(OH)2(s) as the precursor. Extensive solid characterization using x-ray diffraction and spectroscopic methods was performed to assess changes in particle morphology and size distribution, as well as Tc speciation and incorporation, in the produced mineral phases. The results show that the solution pH, temperature, and oxidation kinetics play key roles in the final mineral products. Micrometer-sized magnetite crystals (0.62-0.96 µm on average) with well-defined dodecahedral or octahedral structures were synthesized under near neutral (~pH 8) or alkaline (~pH13) conditions at 75 °C, respectively; whereas goethite dominated the end products at room temperature. An increase in pH at 75 °C improved Tc removal from 27% (near neutral pH) to 42% (alkaline pH), but the removal process remained inhibited by redox competitive Cr(VI) present in the waste streams. By adding additional Fe(II) to the system, Tc sequestration was dramatically improved to up to 87% without observable changes in the solid product. The sequestrated Tc existed as TcO2·2H2O and/or Tc(IV) incorporated into magnetite, where extended X-ray absorption fine structure (EXAFS) spectroscopy showed that more Tc was incorporated into magnetite at elevated temperatures and pH conditions, with complete Tc(IV) incorporation into magnetite occurring under 75 °C-pH 13 conditions. Our results indicate that optimal micrometer-sized magnetite can be produced for Tc sequestration by reacting Fe(OH)2(s) with a waste stream simulant under elevated pH (~13) and temperature (75 °C) conditions. The incorporation of reduced Tc(IV) into stable micrometer-sized magnetite provides a viable supplemental immobilizing technology that may be used to improve nuclear waste treatment and disposal needs.
Wang, Guohui↗
Resolving Configurational Disorder for Impurities in a Low-Entropy Phase
Hematite (α-Fe 2 O 3 ) exerts a strong control over the transport of minor but critical metals in the environment and is used in multiple industrial applications; the photocatalysis community has explored the properties of hematite nanoparticles over a wide range of transition metal dopants. Nonetheless, simplistic assumptions are used to rationalize the local coordination environment of impurities in hematite. Here, we use ab initio molecular dynamics (AIMD)-guided structural analysis to model the extended X-ray absorption fine structure (EXAFS) of Cu 2+ - and Zn 2+ -doped hematite nanoparticles. Specific defect–impurity associations were identified, and the local coordination environments of Cu and Zn both displayed considerable configurational disorder that, in aggregate, approached Jahn–Teller-like distortion for Cu but, in contrast, maintained hematite-like symmetry for Zn. This study highlights the role of defects in accommodating impurities in a nominally low-entropy phase and the limits to traditional shell-by-shell fitting of EXAFS for dopants/impurities in unprecedented bonding environments.
36 MATERIALS SCIENCE↗
A Focused Ion Beam-Scanning Transmission Electron Microscopy with Energy-Dispersive X-ray Spectroscopy Study on Technetium Incorporation within Iron Oxides through Fe(OH) 2 (s) Mineral Transformation
Incorporation of Tc(IV) into iron oxide/hydroxide minerals has been explored and proposed as a promising pathway to preventing Tc(IV) reoxidation to environmentally mobile pertechnetate (TcO 4 - ) and improving long-term immobilization of radioactive technetium-99 (Tc). However, visual evidence evaluating the distribution of Tc(IV) incorporated within iron oxide/hydroxide phases has not been available, until now, despite potential implications on Tc(IV) stability within the host phase. For the purpose of this study Tc(IV) incorporation into iron oxide/hydroxide phases was facilitated via Fe(OH) 2 (s) oxidation and mineral transformation to magnetite (Fe 3 O 4 ). Focused ion beam - scanning transmission electron microscopy equipped with energy-dispersive X-ray spectroscopy (FIB/STEM-EDS) methods were then combined with X-ray diffraction and absorption spectroscopy techniques to characterize and visually demonstrate that, for the first time, Tc(IV) is heterogeneously incorporated into different iron oxide/hydroxide phases as Tc(IV)-incorporated magnetite and/or TcO 2 ·2H 2 O(s) via different incorporation mechanisms. Heterogeneous distribution of Tc(IV) in magnetite suggests either (i) TcO4- is reduced quickly at the magnetite surface and then encapsulated into magnetite during continued octahedral crystal growth, or (ii) Tc(IV) alternatively partitioned into multiple layers of a blocky, plate-like morphological magnetite structure showing stratified Tc. With limited Tc-hematite (Fe 2 O 3 ) incorporation, the results suggest that TcO 2 ·2H 2 O(s) is formed and mainly associated/embedded in fibrous nanometer-sized polycrystalline hematite. This work highlights the power of modern state-of-the-art FIB/STEM-EDS approach to provide essential visual insights of the Tc-iron oxide/hydroxide incorporation and generate reliable mechanism-informed designs for waste forms relying on Tc mineral incorporation.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Influences on Subsurface Plutonium and Americium Migration
Plutonium (Pu) has been released to the environment worldwide, including approximately 1.85 × 1015 Bq (200 kg) of Pu from process waste solutions to unconfined soil structures at the Hanford Site in Washington State. The subsurface mobility of Pu is influenced by complex interactions with sediments, groundwater, and any co-contaminants within the waste stream. Previous investigations at Hanford have shown that Pu exists as discrete PuO 2 particles forming before or after disposal, as secondary solid phases formed from waste interactions with sediments as adsorbed/incorporated species, and/or as dissolved species. In this research, new evidence is presented for the existence of PuO 2 , PuO 2 -Bi 2 O 3 composites, and particles from burnt Pu metal in near-surface sediments where Pu-laden acidic process waste was disposed to sediments. Pu and americium (Am) L3 X-ray absorption spectroscopy and density functional theory suggest that, in larger, more crystalline PuO 2 particles, Am formed from radioactive decay is retained in the Pu IV O 2 structure as Am IV . The Pu and Am that were disposed of in an acidic waste stream have since migrated deeper into the subsurface with detection to at least 37 meters below ground surface. In contrast, Pu deposited near the ground surface from neutral pH waste is found to be homogeneously distributed and relatively immobile. Groundwater extractions performed on contaminated sediments indicate that both Pu and Am are recalcitrant, with Am being fractionally less extractable than Pu on a molar basis. These results suggest that the more mobile fraction of Am has migrated from the near-surface and may be present in the deeper sediments as a different phase than Pu. From these results, it is suggested that Pu and Am deposited from acidic wastes were initially mobile and became significantly less mobile as wastes were neutralized within the soil profile.
38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
Behavior of iodate substituted ettringite during aqueous leaching
Not Available
Avalos, Nancy M. (ORCID:0000000180734642)↗
Competitive TcO4-, IO3-, and CrO42- Incorporation into Ettringite
Ettringite is a naturally occurring mineral found in cementitious matrices that is known for its ability to incorporate environmentally mobile oxyanion contaminants. To better assess this immobilization mechanism for contaminants within cementitious waste forms intended for nuclear waste storage, this work explores how mixed oxyanion contaminants compete for ettringite incorporation and influence the evolving mineralogy. Ettringite was precipitated in the presence of TcO4-, IO3-, and/or CrO42-, known contaminants of concern to nuclear waste treatment, over pre-determined precipitation periods. Solution analyses quantified contaminant removal and the collected solid was characterized using bulk and microprobe XRD coupled with PDF and microprobe XRF analyses. Results suggest that =96% IO3- is removed from solution, regardless of ettringite precipitation time or the presence of TcO4- or CrO42-. However, TcO4- removal remained <20%, was not significantly improved with longer ettringite precipitation times, and significantly decreased in the presence of IO3-. When IO3- is comingled with CrO42, gypsum is formed as a secondary mineral phase, which results in oxyanion partitioning among mineral phases, e.g., IO3- incorporation into ettringite and CrO42- incorporation into gypsum via SO42- substitution. Results from this work exemplify the importance of competitive immobilization when assessing waste form performance and environmental risk of contaminant release.
Gillispie, Elizabeth C.↗
Development and Characterization of Cementitious Waste Forms for Immobilization of Granular Activated Carbon, Silver Mordenite, and HEPA Filter Media Solid Secondary Waste
At the Department of Energy’s Hanford site, over 53 million gallons of chemically complex and radioactive wastes have been stored in 177 underground tanks. The Hanford Tank Waste Treatment and Immobilization Plant (WTP) is under construction and is designed to treat and immobilize these wastes. During operations of WTP, solid secondary wastes (SSWs) will be generated as a result of waste treatment, vitrification, off-gas management, and supporting process activities. SSW treatment processes and resulting disposal pathways for the final disposition form of the SSW are needed to support direct feed low activity waste (DFLAW) operations and facilitate continued operation of WTP. The SSWs produced through WTP operations are expected to include used process equipment, contaminated tools and instruments, decontamination wastes, high-efficiency particulate air (HEPA) filters, carbon absorption beds (granular activated carbon, GAC), silver mordenite (AgM) and spent ion-exchange resins. These waste streams are planned to be immobilized in a cementitious waste form and disposed of either as stabilized/blended (non-debris) or encapsulated (debris) in a cementitious waste form. Accordingly, cementitious waste forms from these streams were included in the 2017 Integrated Disposal Facility (IDF) Performance Assessment (PA). The input data used to represent these SSW forms in the 2017 IDF PA involved many assumptions and associated uncertainties. This data limitation was due to the lack of material- and site-specific data available for representative SSW materials in cementitious matrices. To verify the assumed values used in the IDF PA and fill this limitation in available data, Washington River Protection Solutions, LLC (WRPS), has initiated a program targeted toward gathering site specific data relevant to Hanford SSW disposal. The work within this report is a continuation of this ongoing program.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
Immobilizing Pertechnetate in Ettringite via Sulfate Substitution
Until recently, a nuclear waste form did not exist for the immobilization and long-term storage of the anionic form of radionuclide technetium-99 (99Tc), pertechnetate (TcO 4 - ). Across international nuclear waste sites, the inability to capture TcO 4 - poses a threat to the local environment due to the anion’s long half-life and environmental mobility under environmentally oxic conditions. To combat this challenge, most waste forms would capture 99Tc using materials that reduce TcO 4 - to Tc(IV) species, e.g. 99Tc oxides or 99Tc sulfides. However, this is a short-lived solution unless reducing capacities can be regenerated to last over the long life expectancy of some nuclear waste forms (~10,000 years). In light of recent experimental observations gained from the development of cementitious waste forms and unconfirmed hypotheses from the literature, this work explores how ettringite, a common mineral formed in cementitious materials with demonstrated success in incorporating oxyanions, may be used to immobilize TcO 4 - directly and over the life-time of the waste form. Using batch precipitation experiments, solid phase characterization techniques, and ab initio molecular dynamics simulations, we demonstrate herein successful incorporation of TcO 4 - into ettringite via substitution for SO 4 2- within the ettringite crystal structure. Here, these results are first of their kind and confirm the hypothesis that ettringite acts as an immobilizing mineral within cementitious waste forms for the highly mobile TcO 4 - oxyanion, enhancing the overall performance of these waste forms over time.
36 MATERIALS SCIENCE↗
Iodine Waste Form Corrosion: PNNL Summary Testing Report
A test method to correlate the laboratory corrosion behavior of iodine-containing waste forms (IWFs) to a conceptual long-term corrosion models is required. Several candidate methods have been evaluated previously, and each method presents unique challenges and limitations. Dynamic leach tests have emerged as the preferred candidate test method to evaluate IWFs and parameterize an eventual long-term corrosion model. This report was prepared in support of this effort to define the test suite to evaluate the corrosion of IWFs, with the goal of defining and parameterizing a conceptual long-term corrosion model. A review was presented highlighting the high degree of variability between the IWF corrosion data that is available in the literature and the need for a standardized test suite. The targeted test suite is composed of a single interval screening test, a dynamic leach test, and post-test solid characterization of the monolithic IWF samples. The data presented serves two purposes: to expand the range of IWFs evaluated with the test suite to assess method variability and to further understand the corrosion of IWFs to best inform conceptual long-term corrosion model development. A series of IWF types were included in the testing, including hot isostatically pressed Ag-mordenite, silver functionalized silica-based aerogels, iodosodalites (hot isostatic pressing, sintered, glass bonded ceramic), iodoapatite, tellurite glass and glass composite materials.
42 ENGINEERING↗
Hybrid Sorbents for 129 I Capture from Contaminated Groundwater
Radioiodine ( 129 I) poses a risk to the environment due to its long half-life, toxicity, and mobility. It is found at the U.S. Department of Energy Hanford Site due to legacy releases of nuclear wastes to the subsurface where 129 I is predominantly present as iodate (IO 3 – ). To date, a cost-effective and scalable cleanup technology for 129 I has not been identified, with hydraulic containment implemented as the remedial approach. Here, novel high-performing sorbents for 129 I remediation with the capacity to reduce 129 I concentrations to or below the US Environmental Protection Agency (EPA) drinking water standard and procedures to deploy them in an ex-situ pump and treat (P&T) system are introduced. Furthermore, this includes implementation of hybridized polyacrylonitrile (PAN) beads for ex-situ remediation of IO 3 – -contaminated groundwater for the first time. Iron (Fe) oxyhydroxide and bismuth (Bi) oxyhydroxide sorbents were deployed on silica substrates or encapsulated in porous PAN beads. In addition, Fe–, cerium (Ce)–, and Bi–oxyhydroxides were encapsulated with anion-exchange resins. The PAN–bismuth oxyhydroxide and PAN–ferrihydrite composites along with Fe- and Ce-based hybrid anion-exchange resins performed well in batch sorption experiments with distribution coefficients for IO 3 – of >1000 mL/g and rapid removal kinetics. Of the tested materials, the Ce-based hybrid anion-exchange resin was the most efficient for removal of IO 3 – from Hanford groundwater in a column system, with 50% breakthrough occurring at 324 pore volumes. The functional amine groups on the parent resin and amount of active sorbent in the resin can be customized to improve the iodine loading capacity. These results highlight the potential for IO 3 – remediation by hybrid sorbents and represent a benchmark for the implementation of commercially available materials to meet EPA standards for cleanup of 129 I in a large-scale P&T system.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Iodine Immobilization by Materials through Sorption and Redox-Driven Processes: A Literature Review
Radioiodine-129 (129I) in the subsurface is mobile and limited information is available on treatment technologies. Scientific literature was reviewed to compile information on materials that could potentially be used to immobilize 129I through sorption and redox-driven processes, with an emphasis on ex-situ processes. Candidate materials to immobilize 129I include iron minerals, sulfur-based materials, silver-based materials, bismuth-based materials, ion exchange resins, activated carbon, modified clays, and tailored materials (metal organic frameworks (MOFS), layered double hydroxides (LDHs) and aerogels). Where available, compiled information includes material performance in terms of (i) capacity for 129I uptake; (ii) long-term performance (i.e., solubility of a precipitated phase); (iii) technology maturity; (iv) cost; (v) available quantity; (vi) environmental impact; (vii) ability to emplace the technology for in situ use at the field-scale; and (viii) ex situ treatment (for media extracted from the subsurface or secondary waste streams). Because it can be difficult to compare materials due to differences in experimental conditions applied in the literature, Part II of this review describes results of laboratory studies for selected materials using a standardized batch loading test.
Moore, Robert C.↗
Impact of Cr and Co on 99Tc retention in magnetite: A combined study of ab initio molecular dynamics and experiments
This work explores the effect of co-mingled dopants, Co(II) and Cr(III), on Tc(IV) incorporation and retention in magnetite when heat treated to 625 or 700 °C. Key trends in Tc retention in the high temperature regime were identified using a combination of density-functional-theory based ab initio molecular dynamics (AIMD) simulations, and batch experiments including solid phase characterization techniques, e.g. X-ray absorption spectroscopy. A stabilizing effect on Tc(IV) was observed when the number of Tc and Cr atoms are equal or when the magnetite surface is oversaturated with Tc and Cr inclusions. Here, oversaturation is hypothesized to force Cr from the magnetite surface to form a Cr2O3 phase, which may act as a protective layer that prevents Tc release. With the addition of Co, Tc(IV) is stabilized via redox processes. The presence of Cr in low concentrations interferes with this redox stabilization and Cr is preferentially stabilized as opposed to Tc. As a result, using Co as a stabilizing dopant for Tc may be compromised in the presence of Cr. When the relative concentration of Tc, Cr and Co is the same, or more Co atoms are added to high Cr incorporated systems, the formation of the Cr2O3 phase may be suppressed. Although waste streams with co-mingled Tc and Cr potentially may benefit from a Co dopant, since the formation of a Cr2O3 passivation layer may protect incorporated Tc from being released, the relative concentration of the three elements will be a critical parameter for maximizing effectiveness of this strategy.
Lee, Mal Soon↗
Evaluation of the Change in Uranium Mobility in Sediments from the Hanford 300-FF-5 Stage B Polyphosphate Field Injection
The purpose of this study was to evaluate the change in uranium mobility in the periodically re-wetted zone (PRZ) and upper unconfined aquifer of the Hanford Site’s 300-FF-5 operable unit as a result of Stage B polyphosphate (PO 4 ) injections. These 300 Area sediments are beneath or near the former North Process Pond, which has previously been shown to contain metatorbernite [Cu(UO 2 ) 2 (PO 4 ) 2 •8H 2 O] and uranophane [Ca(UO 2 ) 2 (SiO 3 OH) 2 •5H 2 O], along with aqueous and adsorbed uranium (U), and small amounts of U in calcite as a result of acidic disposal with a significant number of co-contaminants. Previous laboratory-scale studies have identified multiple mechanisms that decrease uranium mobility with polyphosphate injection: (a) precipitation of a low-solubility uranium-phosphate mineral (autunite); (b) precipitation of a Ca-phosphate solid that incorporates U; (c) precipitation of Ca-phosphate mineral (apatite group minerals) that coats existing uranium phases (i.e., U in calcite, U in Fe-oxides), reducing uranium leaching; and (d) aqueous Ca-U-carbonate species adsorption onto apatite. Given the significant amount of apatite precipitation, other U phases such as carbonates could also coprecipitate with apatite. To quantify differences in solubility, leachability, and phases of uranium between pre- and post-PO 4 -treated sediments, different types of analyses were conducted, including analysis of uranium in (a) a carbonate solution extraction from sediment over 1000 h (41.67 days), (b) six sequential liquid extractions from sediment over approximately 1 week, (c) leaching of uranium from sediments in one dimensional (1-D) column experiments over 2 months, and (d) solid phase characterization of select sediments. An additional extraction and solid phase measurements were conducted to evaluate phosphate precipitate formation. Metals were also analyzed in sequential liquid extractions as indicators of (a) amendment injection delivery, (b) co-contaminant movement, and (c) changes in solid phases. Aqueous and solid phase carbonate measurements were also conducted to evaluate changes in carbonates.
12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗