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At least 19 records

Analysis of Technetium Ion Exchange Resin from the 200 West Pump-and-Treat Facility

The 200 West Area Pump-and-Treat (P&T) facility at the Hanford Site is a combined treatment train consisting of unit processes to remove radionuclides such as uranium (U) and technetium (Tc-99), other inorganic (nitrate and hexavalent chromium), and organic (carbon tetrachloride and trichloroethene) contaminants. The RAD building of the P&T facility removes Tc-99 and U using ion exchange chromatography, while the other inorganic and organic contaminants are removed in the facility’s BioPlant portion. The original design of the ion exchange resin for Tc-99 allowed for a 3-month Tc-99 breakthrough and subsequent resin canister change out. However, no Tc-99 breakthrough was noted for 3 years. The objective of the work was to analyze spent resin to determine if there are other compounds that may interfere with Tc-99 adsorption, and to determine whether the resin was removing any I-129.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Removal of Technetium-99 on Ion Exchange Resin - A Case Study at 200 West Pump and Treat - 17303

The 200 West Pump and Treat (P and T), on the U.S. Department of Energy's Hanford Site and operated by CH2M HILL Plateau Remediation Company, has a 9,464 liters per minute capacity designed to capture and treat an 8 km{sup 2} contaminated groundwater plume and reduce the mass of contaminants of concern (COCs) by 95 percent in 25 years. The plume is a complex mix of contaminants including technetium-99 (Tc-99), uranium, carbon tetrachloride, chromium, hexavalent chromium, nitrate, and iodine-129 (I-129). Ion exchange (IX), a common treatment approach for Tc-99 used by many nuclear remediation sites, is used to remove uranium and Tc-99 at 200 West P and T. The IX vessels are arranged in a sequence of three to provide a lead, lag and polish vessel. Tc-99 concentrations are monitored monthly to assure good performance of the system. Performance tracking revealed surprising results. On October 14, 2015, the resin in the lead vessels released Tc-99 at concentrations greater than what was being fed. Although Tc-99 was captured by the downstream lag and polish vessels, the facility staff grabbled with the sudden release of Tc-99 entertaining a variety of scenarios that might result in sudden failure of the IX processes. Subsequent sampling indicated Tc-99 removal began a steady return to normal. The incident raised many questions, chief among them whether the same events could recur and undermine Tc-99 treatment. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Speciation of technetium in carbonate media under helium ions and γ radiation

Technetium carbonates complexes produced by chemical, electrochemical and radiolytic methods have been studied by UV-Visible, X-ray Absorption Fine Structure (XAFS) and Density Functional Theory methods. The (NH 4 ) 2 TcCl 6 salt was dissolved in 2 M KHCO 3 . The resulting purple solution was analyzed by XAFS and UV-Visible spectroscopy. The UV-Visible spectra exhibits a band centered at 515 nm. The XAFS results were consistent with the presence of polymeric species containing the [Tc 2 (μ-O) 2 ] 4+ core coordinated to carbonate ligand. Concerning the electrochemical methods, the pertechnetate anion was electrochemically reduced in concentrated carbonate solution [(CO 3 2- )=5 M and (HCO 3 - )=0.5 M]. For the radiolytic reduction, the speciation of Tc under Helium ions particle beam and γ radiation was examined by UV-Visible and XAFS spectroscopy in high concentrated carbonate media. In concentrated carbonate solutions, pertechnetate as Tc(VII), was not reduced under irradiation due to the formation of carbonate radical which is a strong oxidant. Then, the solution proposed was the addition of formate to the solution which can scavenge hydroxyl radical 10 times faster than carbonate and prevent re-oxidation of reduced technetium. The XANES and EXAFS spectroscopies, approved by theoretical methods, revealed that the final product of the radiolytic reduction of pertechnetate is in the +IV oxidation state. The final structure of the reduced product by He 2+ radiolysis was the same as electrochemical reduction. From this complex determination and evolution vs. the dose, this study is reporting the solubility of the Tc(IV) complex.

Ghalei, Mohammad↗

Interim glycol flowsheet reduction/oxidation (redox) model for the Defense Waste Processing Facility (DWPF)

Control of the REDuction/OXidation (REDOX) state of glasses containing high concentrations of transition metals, such as High Level Waste (HLW) glasses, is critical in order to eliminate processing difficulties caused by overly reduced or overly oxidized melts. Operation of a HLW melter at Fe +2 /ΣFe ratios of between 0.09 and 0.33, a range which is not overly oxidizing or overly reducing, helps retain radionuclides in the melt, i.e. long-lived radioactive 99 Tc species in the less volatile reduced Tc 4+ state, 104 Ru in the melt as reduced Ru +4 state as insoluble RuO 2 , and hazardous volatile Cr 6+ in the less soluble and less volatile Cr +3 state in the glass. The melter REDOX control balances the oxidants and reductants from the feed and from processing additives such as antifoam. Currently, the Defense Waste Processing Facility (DWPF) is running a formic acid-nitric acid (FN) flowsheet where formic acid is the main reductant and nitric acid is the main oxidant. During decomposition formate and formic acid releases H 2 gas which requires close control of the melter vapor space flammability. A switch to a nitric acid-glycolic acid (GN) flowsheet is desired as the glycolic acid flowsheet releases considerably less H 2 gas upon decomposition. This would greatly simplify DWPF processing. Development of an EE term for glycolic acid in the GN flowsheet is documented in this study.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Ion Exchange Column Tests Supporting Technetium Removal Resin Maturation

The primary treatment of the tank waste at the DOE Hanford site will be done in the Waste Treatment and Immobilization Plant, currently under construction. The baseline plan for this facility is to treat the waste, splitting it into High Level Waste (HLW) and Low Activity Waste (LAW). Both waste streams are then separately vitrified as glass and sealed in canisters. The LAW glass will be disposed on site. There are currently no plans to treat the waste to remove technetium, so its disposition path is the LAW glass. Due to the soluble properties of pertechnetate and long half-life of 99 Tc, effective management of 99 Tc is important. Options are being explored to immobilize the supplemental LAW portion of the tank waste, as well as to examine the volatility of 99 Tc during the vitrification process. Removal of 99 Tc, followed by off-site disposal has potential to reduce treatment and disposal costs. A conceptual flow sheets for supplemental LAW treatment and disposal that could benefit from technetium removal will specifically examine removing 99 Tc from the LAW feed stream to supplemental immobilization. SuperLig® 639 is an elutable ion exchange resin. In the tank waste, 99 Tc is predominantly found in the tank supernate as pertechnetate (TcO 4 - ). Perrhenate (ReO 4 - ) has been shown to be a good non-radioactive surrogate for pertechnetate in laboratory testing for this ion exchange resin. This report contains results of experimental ion exchange distribution coefficient and column resin maturation kinetics testing using the resin SuperLig® 639a to selectively remove perrhenate from simulated LAW. This revision includes results from testing to determine effective resin operating temperature range. Loading tests were performed at 45°C, and the computer modeling was updated to include the temperature effects. Equilibrium contact testing indicated that this batch of SuperLig® 639 resin has good performance, with an average perrhenate distribution coefficient of 291 mL/g at a 100:1 phase ratio. This slightly exceeds the computer-modeled equilibrium distribution. The modeling agreed well with the experimental data for perrhenate removal with minor adjustments. Predicted breakthrough performance was on average within about 20% of measured values.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Selection and Validation of Alternate Slag Sources for Saltstone Production - 16145

To stabilize low activity salt solution produced at the Savannah River Site (SRS) the salt waste is mixed with a combination of fly ash (FA), ground granulated blast furnace slag (GGBFS), and ordinary Portland cement (OPC) to form a grout termed saltstone. Upon curing, the low activity waste is encapsulated within the hardened cementitious matrix. While the sources of the dry feed components have remained unchanged for several years, SRS was recently notified that its domestic source of GGBFS would no longer be available due to the shutdown of the steel making plant that produced the ferrous slag as a by-product. This shut-down follows a trend in the reduction of domestic ferrous slag sources. Alternate GGBFS vendors were sought and a program developed to validate the alternate sources for use in saltstone. GGBFS is primarily utilized in the construction industry as a replacement for OPC and the requirements of a GGBFS source, based on an American Society for Testing and Materials (ASTM) standard, are predominantly limited to demonstrating that the GGBFS replacement will provide equivalent strength in comparison to the baseline OPC-based concrete. This affords the construction industry significant flexibility with respect to the GGBFS source that can be used. In contrast, GGBFS has a role of significantly more importance when utilized in saltstone. In particular, the reducing blast furnace environment under which GGBFS is produced yields reducing species, such as sulfide (S{sup 2-}) and ferrous iron (Fe{sup 2+}), which are believed to facilitate the long-term immobilization of redox sensitive contaminants (e.g. technetium-99 ({sup 99}Tc)). In addition, a change in GGBFS source has the potential to impact the rheological properties and the reactive heat generation of the grout, which may adversely affect the ability to pump the grout to a Saltstone Disposal Unit (SDU) and the temperatures attained within an SDU, respectively. As such, alternate GGBFS sources for the processing of saltstone require significantly more scrutiny than is prescribed by the ASTM standard. Four alternate GGBFS sources were evaluated. All four sources met the ASTM requirements, only one source was considered viable for use in saltstone based on preliminary evaluation. The other three sources will require a more intensive assessment to determine their potential applicability. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Durable Tellurite Glasses for Vitrification of Technetium Wastes - 18270

Technetium-99 (Tc-99) can bring a significant environmental risk because it has a long half-life and high fission yield. The present work has developed alumino tellurite glass to immobilize Tc wastes generated by the pyrochemical processing technology. Rhenium (Re) was used as a non-radioactive surrogate for Tc. The Re{sub 2}O{sub 7} concentration in the tellurite glasses was as high as 9.11 mass% with retention of 86% on average. X-ray absorption spectroscopy analysis revealed that Re exists as Re{sup 7+} and is surrounded by 4 oxygen atoms. The 7-day PCT results were satisfied with the immobilized low-activity waste regulatory limit with Ca(ReO{sub 4}){sub 2} content less than 12 mass%. The long-term dissolution test was conducted for 256 days and a rate drop has occurred in which the rate of leaching gradually decreased. An alteration layer depleted soluble element was observed on the leached glass surface. These results suggest that tellurite glass can be a good candidate as a matrix for immobilizing Tc. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Precipitation of Epsilon Particles in Metal Doped Ceria Irradiated with Energetic Ions

Metallic particles precipitated from fission products in oxide fuel matrix (e.g., UO{sub 2}) have a great impact on the thermal and mechanical properties of the fuel. A burn-up of 40 MWd/kg U results in the conversion of 4% of the uranium to approximately 3% fission products and 1% transuranium elements. Epsilon phase is the major metallic phase of the precipitates with a hexagonal-closed packed (HCP) crystal structure. It can exist in a variety of metallic forms in UO{sub 2}, but typically, it consists of five metals: Mo, Pd, Rh, Ru and Tc. Epsilon particles can form over a wide range of stoichiometries in the five metal system. Simulated compositions with Re as a surrogate for Tc have been investigated as a waste form for {sup 99}Tc, an isotope with a long half-life of 2.13 10{sup 5} years and a high solubility under oxidizing conditions in addition to Mo in the corrosion process. There is a pressing need to understand the factors influencing the formation and growth of the metallic phase in fuel. Efforts are currently underway to perform careful neutron irradiation of nuclear fuel under controlled conditions in a test reactor, recover metallic phases that may be present, and characterize the resulting structure and chemistry. Due to the long duration, high cost and radiological concerns associated with neutron irradiation and sample characterizations, ion irradiation studies of a surrogate material with a full control of the processing parameters can emulate different stages of the particle precipitation, which can add a tremendous value to reactor-based studies. This presentation reports our recent ion irradiation results on the metallic particle precipitation under various irradiation and thermal annealing conditions.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Technetium Management Program Plan - 17376

Technetium management is a high-priority activity for the U.S. Department of Energy (DOE) Office of Environmental Management (EM) complex. Waste management and remediation issues involving technetium represent environmental risks and challenges that are unique to DOE. This plan lays out the technology development activities that are underway as well as future technology needs to address technetium issues across DOE EM sites and across programmatic areas of tank waste, groundwater and soils, and facility decommissioning and deactivation in order to be comprehensive and to allow integration of similar activities. The program was developed in close coordination with site representatives and program offices. Activities and needs that were identified share common themes and were grouped into areas of characterization, treatment, and disposition. Characterization includes understanding the inventory at particular locations, the chemical species, and chemical and physical behavior, whether in a treatment process flowsheet or a geological setting that displays periodic contaminant releases. The tools for characterization in these different environments might use the same sensors or protocols. Treatment options include methods to capture technetium such as ion-exchange or manipulation of oxidation states, which also may be applied across program areas. Disposition includes end-points of the processes and environmental risk, including waste form behavior, mobility of technetium once it is treated or remediated, and long-term monitoring. Disposition represents integration of all cleanup actions at a site. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Ion Exchange Distribution Coefficient Tests and Computer Modeling at High Ionic Strength Supporting Technetium Removal Resin Maturation

The primary treatment of the tank waste at the DOE Hanford site will be done in the Waste Treatment and Immobilization Plant (WTP) that is currently under construction. The baseline plan for this facility is to treat the waste, splitting it into High Level Waste (HLW) and Low Activity Waste (LAW). Both waste streams are then separately vitrified as glass and poured into canisters for disposition. The LAW glass will be disposed onsite in the Integrated Disposal Facility (IDF). There are currently no plans to treat the waste to remove technetium, so its disposition path is the LAW glass. Due to the water solubility properties of pertechnetate and long half-life of 99 Tc, effective management of 99 Tc is important to the overall success of the Hanford River Protection Project mission. To achieve the full target WTP throughput, additional LAW immobilization capacity is needed, and options are being explored to immobilize the supplemental LAW portion of the tank waste. Removal of 99 Tc, followed by off-site disposal, would eliminate a key risk contributor for the IDF Performance Assessment (PA) for supplemental waste forms, and has potential to reduce treatment and disposal costs. Washington River Protection Solutions (WRPS) is developing some conceptual flow sheets for supplemental LAW treatment and disposal that could benefit from technetium removal. One of these flowsheets will specifically examine removing 99 Tc from the LAW feed stream to supplemental immobilization. To enable an informed decision regarding the viability of technetium removal, further maturation of available technologies is being performed. This report contains results of experimental ion exchange distribution coefficient testing and computer modeling using the resin SuperLig ® 639 a to selectively remove perrhenate from high ionic strength simulated LAW. It is advantageous to operate at higher concentration in order to treat the waste stream without dilution and to minimize the volume of the final wasteform. This work examined the impact of high ionic strength, high density, and high viscosity if higher concentration LAW feed solution is used. Perrhenate (ReO 4 - ) has been shown to be a good nonradioactive surrogate for pertechnetate in laboratory testing for this ion exchange resin, and the performance bias is well established. Equilibrium contact testing with 7.8 M [Na + ] average simulant concentrations indicated that the SuperLig ® 639 resin average perrhenate distribution coefficient was 368 mL/g at a 100:1 phase ratio. Although this indicates good performance at high ionic strength, an equilibrium test cannot examine the impact of liquid viscosity, which impacts the diffusivity of ions and therefore the loading kinetics. To get an understanding of the effect of diffusivity, modeling was performed, which will be followed up with column tests in the future.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Removal of TcO 4 - ions from solution: materials and future outlook

Technetium mainly forms during artificial nuclear fission; it exists primarily as TcO 4- in the nuclear waste, and is among the most hazardous radiation-derived contaminants because of its long half-life (t1/2 = 2.13 × 105 yrs) and environmental mobility. The high water solubility of TcO 4- (11.3 mol L -1 at 20°C) and its ability to readily migrate within the upper layer of Earth’s crust make it particularly hazardous. Several types of materials, namely resins, molecular complexes, layered double hydroxides, and pure inorganic and metal-organic materials, have been shown to be capable of capturing TcO 4- (or other oxoanions) from solution. In this review, we give a brief description about the types of materials that have been used to capture TcO 4- and closely related oxyanions so far and discuss the possibility of using metal-organic frameworks (MOFs) as next-generation ion-exchange materials for the stated application. In particular, with the advent of ultra-stable MOF materials, in conjunction with their chemical tunability, MOFs can be applied to capture these oxyanions under real-life conditions.

36 MATERIALS SCIENCE↗

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

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

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Characterization of SuperLig® 639 rhenium and technetium resin with batch contact and column tests

Two new (2013) lots of SuperLig® 639 ion exchange resin (IBC Advanced Technologies, American Forks, UT) were tested for the first time above typical sodium concentrations (7.8 M sodium, along with typical 5 M concentration) in highly alkaline solutions. Batch contact and ion exchange column tests characterized rhenium (perrhenate) adsorption as a surrogate for pertechnetate. The work supports technetium removal options for Supplemental Low Activity Waste processing at the Hanford River Protection Project Waste Treatment Plant (WTP). The current work found that the resin performs well in the 7.8 M sodium simulant despite complete floating of the beads. A notable difference in performance between the two new resin lots was found. As a result, resin loading overall versus temperature, potassium concentration, and rhenium/nitrate ratios is consistent with previous data and expectations despite the high sodium concentration and floating of the resin beads.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

The simultaneous removal of technetium and iodine from Hanford tank waste

The simultaneous removal of radionuclides technetium-99 and iodine-129 from an actual decontaminated Hanford tank waste sample (a mixture of decontaminated waste from tanks 241-AP-105 and 241-AP-107) was demonstrated for the first time in this work. A series of commercially available ion exchange resins were evaluated in batch contact tests in the tank waste, and all showed removal of both Tc and I. The highest Tc removal was observed for Purolite A530e while the highest iodine removal was observed for ResinTech SIR-110-MP. Batch tests in simulated tank waste with these two resins showed that the SIR-110-HP-MP had consistently higher K d for both pertechnetate and iodide and much higher K d than previous works on Tc removal from Hanford waste. As such, the SIR-110-MP was evaluated in a dual -column (lead/lag) test processing 5.2L of the tank waste mixture showing 60% breakthrough of Tc on the lead column and no significant breakthrough on the lag after 625 bed volumes (BV, 6 mL size) while significant iodine breakthrough (>50%) occurred after 28 BV. The limited iodine uptake was attributed to the column conditions generating mass transfer limitations. A fraction of the Tc and I was not captured by the resin (<10%) in either the batch tests or column tests. The iodine fraction was identified to be an iodide, likely organo-iodide. The fraction of the Tc was identified as a non-pertechnetate species, which is the first time non-pertechnetate has been identified in AP-105 and AP-107 tanks, although the exact species is still unknown.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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↗