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At least 325 records · Page 18

Development of Tc(IV)-Incorporated Fe Minerals to Enhance 99Tc Retention in Glass Waste Form

Iron minerals have been considered to be good hosts for Tc immobilization because the Tc(IV) ion substitutes for Fe(III) in the crystal structure of the Fe oxide due to similarities in (1) cation size [Tc(IV) = 78.5 pm ; Fe(III) = 69 or 78.5 pm], (2) metal-oxygen interatomic distance (Tc—O = 0.199 nm, Fe—O = 0.203 nm), (3) number of coordinating oxygen atoms (both 6-fold coordinated), and (4) the redox potential (Eh=ca. +20 mV at pH = 7) for a redox couple between Tc(VII)/Tc(IV) and Fe(III)/Fe(II). Magnetite, maghemite, and trevorite are iron oxide minerals and all belong to spinel mineral group. Laboratory testing shows that Tc can be removed from aqueous waste solutions by a process of Tc reduction from Tc(VII) to Tc(IV) followed by co-precipitation with iron oxide minerals during recrystallization of Fe(OH)2(s) used as an initial solid precursor. X-ray absorption near edge structure (XANES) spectroscopy confirmed that Tc was in the +4 oxidation state in final Tc-Fe minerals. The Tc-incorporated Fe minerals were also tested for Tc retention in glass melts at different temperatures between 600 – 1,000 oC in a furnace. After being cooled in air, the solid glass specimens collected at different temperatures were analyzed for Tc oxidation state using XANES and Tc retention using liquid scintillation counting (LSC). Even though Tc(IV) started to reoxidize at 600 oC, Tc retention in the final glass specimen prepared with Tc-incorporated Fe mineral even at high temperatures was at least two times higher than glass prepared with KTcO4 salt. Higher Tc retention in glass is considered to result from limited and delayed Tc volatilization process due to Fe mineral encapsulation for Tc. Therefore, the results showing the presence of Tc(IV) in the Fe mineral structure indicate strong possibility to enhance Tc retention in borosilicate glass as well as to reduce the remediation costs at the Hanford Site.

Environmental Molecular Sciences Laboratory↗

Glass–water interaction: Effect of high-valence cations on glass structure and chemical durability

Borosilicate glass is a durable solid, but it dissolves when in contact with aqueous fluids. The dissolution mechanism, which involves a variety of sequential reactions that occur at the solid-fluid interface, has important implications for the corrosion resistance of industrial and nuclear waste glasses. In this study, spectroscopic measurements, dissolution experiments, and Monte Carlo simulations were performed to investigate the effect of high–valence cations (HVC) on the mechanisms of glass dissolution under dilute and near-saturated conditions. Raman and NMR spectroscopy were used to determine the structural changes that occur in glass, specifically network formers (e.g., Al, Si, and B), with the addition of the HVC element hafnium in the Na2O–Al2O3–B2O3–HfO2–SiO2 system (e.g., Na/[Al+B] = 1.0 and HfO2/SiO2 from 0.0 to 0.42). Spectroscopic measurements revealed that increasing hafnium content decreases N4 (tetrahedral boron/total boron) and increases the amount of Si—O—Hf moieties in the glass. Results from flow–through experiments conducted under dilute and near–saturated conditions show a decrease of approximately 100× or more in the dissolution rate over the series from 0 to 20 mol% HfO2. Comparing the average steady-state rates obtained under dilute conditions to the rates obtained for near-saturated conditions reveals a divergence in the magnitude between the average steady state rates measured in these different conditions. The reason for this divergence was investigated more thoroughly using Monte Carlo simulations. Simulations indicate that the divergence in glass dissolution behavior under dilute and near-saturated conditions result from the stronger binding of Si sites that deposit on the surface from the influent when Hf is present in the glass. As a result, the residence time at the glass surface of these newly-formed Si sites is longer in the presence of Hf, which increases the density of anchor sites from which altered layers with higher Si densities can form. These results illustrate the importance of understanding solid–water/solid-fluid interactions by linking macroscopic reaction kinetics to nanometer scale interfacial processes.

Environmental Molecular Sciences Laboratory↗

Statistical generic design of glass and optimization: Selective review on oxide glasses

Designing a single glass composition for a multidimensional property space is challenging, and the difficulty increases with the number of design criteria. Traditionally, the task is accomplished using multiple statistical models that describe the relationships between composition (C) and property (P) values, i.e., C-P models. Recently, the structure (S)-property (P) statistical modeling has emerged as a complementary approach. The S-P modeling approach has also been shown to be a preferred method for modeling glass properties, particularly when a small data set is available, such as in single-component studies, or when strong nonlinearities exist between composition and properties. The combined model package, C-S-P, implements the concept of generic glass design, i.e., designing glass for performance by first selecting a specific or optimized set of glass network structural groups using S-P models and then transferring the designed structures (genes) to a particular composition using C-S models. This article reviews a set of supporting cases from the previous C-S-P modeling studies of phosphate, silicate, and borosilicate glasses, which are relevant for many critical commercial applications. The methodology for developing the statistical C-S-P database is presented, enabling the application of P?S?C to achieve a generic glass design and optimization, targeting multiple design criteria for both performance and processing properties simultaneously.

Network structure↗

New interaction potentials for borate glasses with mixed network formers

Here, we adapt and apply a recently developed optimization scheme used to obtain effective potentials for aluminosilicate glasses to include the network former boron into the interaction parameter set. As input data for the optimization, we used the radial distribution functions of the liquid at high temperature generated by ab initio molecular dynamics simulations, and density, coordination, and elastic modulus of glass at room temperature from experiments. The new interaction potentials are shown to reliably reproduce the structure, coordination, and mechanical properties over a wide range of compositions for binary alkali borates. Furthermore, the transferability of these new interaction parameters allows mixing to reliably reproduce the properties of various boroaluminate and borosilicate glasses.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

The effects of glass doping, temperature and time on the morphology, composition, and iron redox of spinel crystals

Precipitation of large crystals/agglomerates of spinel and their accumulation in the pour spout riser of a Joule-heated ceramic melter during idling can plug the melter and prevent pouring of molten glass into canisters. Thus, there is a need to understand the effects of spinel-forming components, temperature, and time on the growth of crystals in connection with an accumulation rate. In our study, crystals of spinel [Fe, Ni, Mn, Zn, Sn][Fe, Cr]₂O₄ were precipitated from simulated high-level waste borosilicate glasses containing different concentrations of Ni, Fe, and Cr by heat treating at 850 and 900°C for different times. These crystals were extracted from the glasses and analyzed with scanning electron microscopy and image analysis for size and shape, with inductively coupled plasma-atomic emission spectroscopy and atom probe tomography for concentration of spinel-forming components, and with wet colorimetry and Mössbauer spectroscopy for Fe²⁺/Fe total ratio. High concentrations of Ni, Fe, and Cr in glasses resulted in the precipitation of crystals larger than 100 µm in just two days. Crystals were a solid solution of NiFe₂O₄, NiCr₂O₄, and -Fe₂O₃ (identified only in the high-Ni-Fe glass) and also contained small concentrations of less than 1 at% of Li, Mg, Mn, and Al.

chemical analysis↗

The effectiveness of TRIS and ammonium buffers in glass dissolution studies: a comparative analysis

Abstract Selecting appropriate buffers is crucial for evaluating the chemical durability of glass under controlled conditions such as in the EPA 1313 test designed to measure elemental release as a function of pH. The efficacy of two alkali-metal free buffers, TRIS (NH 2 C(CH 2 OH) 3 ) and ammonium chloride—ammonia (NH 3 /NH 4 Cl), was investigated during EPA 1313 testing of a simulated Hanford low-activity waste borosilicate glass in the alkaline regime (pH 8.5–10.5) at varying temperatures (RT, 40 °C, and 60 °C). While both buffers maintained the desired pH at room temperature, and up to 40 °C, the effectiveness of TRIS decreased at elevated temperatures, particularly at pH 10.5. Although 11 B NMR showed evidence of TRIS-B complexation, its effect on the rate of elemental release was found to be negligible under the test conditions. With ammonium buffer, the release of alkali cations was slightly elevated when compared to the same conditions with TRIS at early time points.

36 MATERIALS SCIENCE↗

Environmental Testing of Tritium-Phosphor Glass Vials for Use in Long-Life Radioisotope Power Conversion Units

Power generation in extreme environments, such as the outer solar system, the night side of planets, or other low-illumination environments, currently presents a technology gap that challenges NASA's ambitious scientific goals. We are developing a radioisotope power cell (RPC) that utilizes commercially available tritium light sources and standard 1.85 eV InGaP2 photovoltaic cells to convert beta particle energy to electric energy. In the test program described here, we perform environmental tests on commercially available borosilicate glass vials internally coated with a ZnS luminescent phosphor that are designed to contain gaseous tritium in our proposed power source. Such testing is necessary to ensure that the glass containing the radioactive tritium is capable of withstanding the extreme environments of launch and space for extended periods of time.

Zemcov, Michael↗

Product Quality Assessment of Glass Formulations for High Sodium Nuclear Waste Streams - 18198

Sodium carbonate is currently being considered as a wash-out reagent for the removal of the settled solids in the unagitated Highly Active Liquor (HAL) storage tanks at Sellafield. As the settled solids are expected to comprise mainly zirconium molybdate (ZM), this will result in a feed to the Waste Vitrification Plant (WVP) containing high concentrations of both molybdenum and sodium. This feed is expected to be challenging for WVP due to solubility limitations in existing base glass compositions and the operating temperature. In particular, depending on the wash-out strategy employed, there is the potential to produce high volumes of sodium-containing waste, which will result in large quantities of vitrified HLW containers. Hence, new glass compositions are being investigated as part of a 3-year Innovate UK-funded collaborative project in order to maximise the sodium content of the vitrified product and minimise the number of containers produced. This paper describes the product quality assessment of several sodium titanosilicate (NaTiSi) compositions that can potentially contain up to ∼15 wt% waste Na{sub 2}O, more than double what is possible using the current UK HLW glass borosilicate composition. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Linear and Non-linear Optical Characterization of Glass and Sapphire for Optical Instrumentation of Advanced Fission Reactors

The linear and nonlinear optical properties of glass and sapphire are investigated to determine the material’s suitability to support optical instrumentation for advanced fission reactors. A post-irradiation examination experiment consisting of a Z-scan, measuring nonlinear optical absorption and refraction, and a spectrometer, measuring linear optical absorption was developed and used. Radiation-induced negative nonlinear optical absorption was observed for the first time in fused silica, sapphire, and borosilicate glass under both types of thermal annealing conditions and the respective effects of thermal annealing are reported.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Structural Characterization of Ternary Salt Melts for Low Activity Waste Applications

Reactions of alkali salts (nitrates, sulfates, carbonates, halides, borates) play a key role in the low temperature feed conversion occurring at the cold cap during processing of Hanford Low Activity Waste (LAW) glass melters. An alkali salt phase can sometimes form, and preferentially incorporate radionuclides of Cs, Cl, I, and Tc. During melting of the slurry feed, some of the feed components sequentially break down with increasing temperature to form gases (i.e., nitrates → NO x , carbonates → CO 2 , and boric acid → H 2 O) or partially volatilize (halides). Sulfate, however, tends not to volatilize but has limited solubility in the final borosilicate glass waste form. To improve understanding of these low temperature processes and their composition dependencies, a scoping study was undertaken to synthesize salt systems that remain amorphous at room temperature, thus facilitating structural study. Melts of equimolar ratios of K2SO4-ZnSO4 (a known ionic glass-forming system) with added nitrates, halides, or carbonates, were melted and quenched. Some of the materials formed single phase glasses and some underwent crystallization upon quenching. Characterization of these quenched materials by thermal analysis, infrared absorption, and diffraction was performed. Addition of other anions to the sulfate base glass resulted in a distortion of the sulfate tetrahedron, as evidenced by infrared absorption. Carbonates strongly promoted crystallization, mostly of carbonate phases. Nitrates promoted crystallization of ZnO, and the nitrate volatilized with some incorporating into the glass. Here, halides tended to incorporate into the glass, but the small (F) and large (I) halogens promoted crystallization of sulfate-containing crystals, while moderate sized (Cl) halogens produced single-phase ionic glasses.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Diagnostics: Chapter 8 of the special issue: on the path to tokamak burning plasma operation

This chapter presents the activity conducted by the ITPA topical group (TG) on Diagnostics over about the last 15 years. Following a general introduction of the ITER Diagnostics led by their measurement roles, the document is organized in several subchapters detailing the design support, research and development activity conducted by each of the specialist working groups (WGs) of the TG. Please note that the magnetic diagnostics were supported at the TG without a specific WG. Their status is included in the general introduction. In the following some highlights of the subchapter’s contents are provided. Recent advances in ITER first wall (FW) diagnostics for the measurements of plasma-metallic wall interaction in support of the ITER research plan are reported. An InfraRed imaging Video Bolometer for ITER has been developed and tested on several tokamaks to measure the radiated power loss. A laser-induced breakdown spectroscopy (LIBS) technique which utilizes a pulsed laser beam to ablate locally by forming a crater, will measure local tritium inventory in the FW material. Real-time Residual Gas Analyzers will measure the neutral gas composition in a divertor port and an equatorial port during plasma operation. Due to the full metallic FW environment, the plasma-wall interaction in ITER will face several challenges such as the compromised radiated power and divertor heat flux measurements by reflection. Ray tracing and analysis codes have been developed to eliminate and correct the effects of reflection in the measurements. The characteristics of the reflecting surfaces depending on the roughness and angle of the incidence have been measured by dedicated experiments, and the results were applied to the reflection elimination. For the measurement of the metallic impurity radiation induced by eroded metallic atoms, a vacuum ultraviolet spectrometer has been developed and tested. An extensive thermonuclear diagnostic suite will be required to support the operation of ITER and the planned experimental program for future burning plasma experiments. Due to the harsh environmental conditions, the implementation of diagnostic systems in ITER is a major challenge. These conditions include high levels of neutron and gamma fluxes, neutron heating, particle bombardment. Therefore, the selection and design of diagnostic systems must take into account a number of phenomena previously unseen in diagnostic design. For this reason, the measurement of neutrons and confined or lost fast ions, with particular emphasis on alpha particles, is critical to ITER. The diagnostics associated with these measurements will be important for future plasma-burning experiments at ITER. The high neutron emission and very large plasma size in ITER make neutron diagnostics the main diagnostic method used to measure plasma parameters such as fusion power, fusion power density, ion temperature, energy of fast ions and their spatial distributions in the plasma core. Active spectroscopy techniques are methods where a neutral particle beam is injected into the plasma and information on plasma parameters is extracted from the measurement of line emission resulting from the beam-plasma interaction, either by plasma ions or by beam atoms. Spatial localization is achieved by crossing the beamline and multiple observation lines. The ITER plasma will be a high temperature, moderately dense, fully ionized collisional plasma. The plasma facing surfaces are principally metallic being fashioned from beryllium or tungsten but many other elements, arising from either structural or from operational needs, may enter this plasma. The energy range of the emitted photons range from meV (infra-red) to multi keV (x-rays) and originate from all areas of the plasma volume. The primary role of passive emission diagnostics is to identify what is in the plasma from spectral signatures. Extracting quantitative information from these measurements such as impurity content, ion temperature, rotation, degree of detachment and radiated power depends on calibrated instruments, a physics model of the atomic and molecular processes and plasma transport and an analysis workflow that takes into account environmental effects such as reflections. The particular needs for ITER have prompted a multi-machine, many-year effort to address all these aspects and this chapter reviews the work on diagnostic design, experiments and new analysis techniques. An overview of the laser diagnostics to be implemented on ITER is also provided in this paper. This includes descriptions of the Thomson scattering in the core, edge and divertor regions, polarimetry and interferometry diagnostics used for measuring plasma density and also measurements of helium density in the divertor using Laser Induced Flourescence. Techniques which can allow improvements on current measurements are also addressed in particular expanding poloidal polarimetry measurements to measure field fluctuations and proposed use of dispersion interferometery which has a number of advantages over existing methods. This paper identifies particular areas where further research and testing on existing tokamaks is useful even at this advanced stage to inform the design of diagnostics for ITER. Outstanding areas of concern for the implementation of laser diagnostics, in particular with a view to reliable operation are identified. An overview of the latest developments of microwave diagnostic systems and techniques is given. The primary focus is the contributions for ITER—the next step burning plasma experiment—which is supplemented by describing recent progress of techniques applicable for fusion experiments beyond ITER. The contributions are intentionally kept concise, and are being supplemented by a rich list of references for further studies. Radiation induced effects are receiving continuous and well-deserved attention of the ITER diagnostic community and they are in many cases one of the primary design drivers of the ITER diagnostic systems. The paper summarizes recent progress in this area focusing primarily on the ITER diagnostics but in some cases provides also outlook for the possible solutions for even more demanding radiation environment of fusion reactors beyond ITER. Despite advancements in the area of modeling and simulation of various radiation induced effects, experimental testing in a nuclear environment as close as possible to the target one is still seen as unavoidable for proper qualification of particular diagnostic functional elements. Recent advancement within three diagnostic areas: optical diagnostics, magnetics and bolometers is covered. Encouraging results on qualification of silica glass vacuum window assemblies are presented. In the area of magnetic sensors, progress of irradiation tests performed on ITER in-vessel LTCC inductive sensors is presented with outlook for novel technological approaches to inductive sensors utilizing thick printing and photolithography technologies being highlighted. Summary of advancements in the area of steady state magnetic field sensors based on Hall effect is given. New results of neutron irradiation test of the ITER borosilicate glass inserts for vacuum electrical feedthroughs are summarized finding negligible swelling at target level of neutron fluence. Off-line irradiation tests of fiber optic current sensors for plasma current measurement demonstrated that both for gamma doses up to 5 MGy and a total neutron fluence up to 10 15 cm −2 , radiation induced changes are still compatible with required measurement accuracy on ITER. The ITER bolometers are given as an example how considering radiation effects may influence the diagnostic design. Finally, outlook for future main R&D directions is outlined. All optical and laser-based diagnostics in ITER will be using mirrors to guide plasma radiation toward detectors, cameras and sensors. In the hostile plasma, radiation and particle environment the optical characteristics of diagnostic mirrors will degrade directly affecting the entire performance of involved diagnostic systems. An assessment of factors affecting mirror performance is provided. Among the prime adverse factors are deposition of plasma impurities, sputtering of mirror surface and steam ingress in the vicinity of mirrors. Within the International Tokamak Physics Activity with active support by ITER central team and domestic agencies, the structured research and development (R&D) program on mitigation of risks for diagnostic mirrors is underway. Within this program the mirror material development, the passive mitigation of mirror degradation by using diagnostic ducts and shutters along with an active mirror recovery program comprising the in-situ mirror cleaning and calibration is underway. Recent developments in diagnostic mirror R&D are described in this Chapter along with an example of their implementation of R&D solutions in ITER Infrared Thermography diagnostic. An assessment of still open engineering and physics questions, considerations on mirror risks during an early phase of ITER operation are given along with an overview of diagnostic mirror evolution in the late ITER operation stage toward the demonstration fusion power plant. Several crucial areas of diagnostic R&D outlined in ITER Research Plan are addressed. The basic control groups in a fusion reactor can be broken-down in five categories: (1) plasma position, magnetic configuration, and plasma current control, (2) profile control and confinement optimization, (3) MHD control and suppression, (4) edge dissipation control, radiation and plasma exhaust control and (5) break-down optimization. These categories are coupled via the physics (a control action in one domain will affect the other domains) and via shared actuators (e.g. ECRH for impurity accumulation avoidance, current density distribution control and MHD suppression). Consequently, a supervisory control system should determine the priority of the various control tasks, their couplings, and the interfaces with the safety and interlock system. For the systematic development of the various controllers taking the complexity of the plasma and the control system into account, a model-based approach is required. A short historical overview is given of the developments in systems and control theory and control engineering with special emphasis on those developments that are most relevant for Nuclear Fusion research and operation. An overview is given of the state of the field of fusion plasma control for the control categories. It will be shown how synthetic diagnostics are being developed in ITER and how they are used in diagnostic design and design validation and how they can be in model-based controller synthesis using relatively simple models. In modern control methods, multiple diagnostics are used to constrain relatively simple models. The constrained models provide an estimate for the state. This opens the route to state controllers, such as model predictive control. A major challenge in nuclear fusion research is the coherent combination of data from heterogeneous diagnostics and modeling codes for machine control and safety as well as physics studies. Measured data from different diagnostics often provide information about the same subset of physical parameters. Additionally, information provided by some diagnostics might be needed for the analysis of other diagnostics. A joint analysis of complementary and redundant data allows, e.g. to improve the reliability of parameter estimation, to increase the spatial and temporal resolution of profiles, to obtain synergistic effects, to consider diagnostics interdependencies and to find and resolve data inconsistencies. Physics-based modeling and parameter relationships provide additional information improving the treatment of ill-posed inversion problems. A coherent combination of all kind of available information within a probabilistic framework allows for improved data analysis results. The concept of integrated data analysis (IDA) in the framework of Bayesian probability theory is outlined and contrasted with conventional data analysis. Components of the probabilistic approach are summarized and specific ingredients beneficial for data analysis at fusion devices are discussed.

ITER↗

Dynamics of self-reorganization explains passivation of silicate glasses

Understanding the dissolution of silicate glasses and minerals from atomic to macroscopic levels is a challenge with major implications in geoscience and industry. One of the main uncertainties limiting the development of predictive models lies in the formation of an amorphous surface layer––called gel––that can in some circumstances control the reactivity of the buried interface. Here, we report experimental and simulation results deciphering the mechanisms by which the gel becomes passivating. The study conducted on a six-oxide borosilicate glass shows that gel reorganization involving high exchange rate of oxygen and low exchange rate of silicon is the key mechanism accounting for extremely low apparent water diffusivity (~10 –21 m 2 s –1 ), which could be rate-limiting for the overall reaction. Furthermore, these findings could be used to improve kinetic models, and inspire the development of new molecular sieve materials with tailored properties as well as highly durable glass for application in extreme environments.

36 MATERIALS SCIENCE↗

Potential-Induced Degradation of Cu(In,Ga)Se 2 Solar Cells: Alkali Metal Drift and Diffusion Effects

Potential-induced degradation (PID) of photovoltaic modules is due to transport of alkali metal ions (Na + ) from the soda-lime glass (SLG) into the semiconductors. For the most efficient polycrystalline absorbers, Na and K in the Cu(In,Ga)(Se,S) 2 (CIGS) absorber often benefit performance, so a more detailed mechanism for PID is needed. To that end, CIGS solar cells have been encapsulated, stressed with high voltage, and cored to extract the active regions for characterization. SLG substrates led to 14.9% efficiency on average, which reduced to 0% after 25 h of -1000 V bias. This was accompanied by increased Na in the CIGS layer, particularly at the buffer interface, as well as decreased carrier concentrations. On the other hand, borosilicate glass substrates with low Na and high K content led to 13.6% efficiency on average, which only reduced to 12.1% after 25 h of stress. This was accompanied by slightly increased K content in the CIGS layer. As K has led to recent world record efficiency CIGS devices, understanding Na and K similarities and differences may help to enhance initial efficiency and reduce PID.

14 SOLAR ENERGY↗

Corrosion Behavior of Developmental Iron Phosphate Waste Forms: FY20 Status Report

Corrosion tests were performed to assess the dissolution behaviors of developmental iron phosphate materials that are being evaluated as an alternative to the glass-bonded sodalite ceramic waste form to immobilize salt wastes from electrochemical separation operations. Production of the iron phosphate waste form results in dehalogenation of the waste salt that increases potential waste loading. Ferric oxide is added to the waste form to increase the chemical durability. Tests conducted to optimize the amount of ferric oxide used to make the waste form are summarized in this report. Specimens prepared from materials made with between 17 and 34 mole % ferric oxide were subjected to two test methods to assess the effects of the iron content on the relative durability and retention of immobilized salt cations including cesium, strontium, and neodymium. Modified ASTM C1308 test results show the intrinsic durability was significantly higher for materials made with 27 mol % ferric oxide. Further additions generated iron-rich inclusion phases and did not improve durability. Modified ASTM C1285 test results show that solution feedback attenuates the dissolution rate similar to what is observed for borosilicate glasses within seven days. Analyses of test specimens after 42 days show no evidence that surface layers formed. Combined with previous studies addressing the salt loading, a composition region of the ammonium (di)hydrogen phosphate-waste salt-ferric oxide ternary has been defined for durable waste form compositions. Materials with that composition can be used to determine optimal processing conditions, assess long-term performance, and parameterize a degradation model.

Stariha, S. A.↗

Preliminary assessment of stable nitrogen and oxygen isotopic composition of USGS51 and USGS52 nitrous oxide reference gases and perspectives on calibration needs

Rationale: Despite a long history and growing interest in isotopic analyses of N 2 O, there is a lack of isotopically characterized N 2 O isotopic reference materials (standards) to enable normalization and reporting of isotope-delta values. Here, in this paper we report the isotopic characterization of two pure N 2 O gas reference materials, USGS51 and USGS52, which are now available for laboratory calibration (https://isotopes.usgs.gov/lab/referencematerials.html). Methods: A total of 400 sealed borosilicate glass tubes of each N 2 O reference gas were prepared from a single gas filling of a high vacuum line. We demonstrated isotopic homogeneity via dual-inlet isotope-ratio mass spectrometry. Isotopic analyses of these reference materials were obtained from eight laboratories to evaluate interlaboratory variation and provide preliminary isotopic characterization of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and site preference (S P ) values. Results: The isotopic homogeneity of both USGS51 and USGS52 was demonstrated by one-sigma standard deviations associated with the determinations of their δ 15 N, δ 18 O, δ 15 N α , δ 15 N β and S P values of 0.12 mUr or better. The one-sigma standard deviations of SP measurements of USGS51 and USGS52 reported by eight laboratories participating in the interlaboratory comparison were 1.27 and 1.78 mUr, respectively. Conclusions: The agreement of isotope-delta values obtained in the interlaboratory comparison was not sufficient to provide reliable accurate isotope measurement values for USGS51 and USGS52. Lastly, we propose that provisional values for the isotopic composition of USGS51 and USGS52 determined at the Tokyo Institute of Technology can be adopted for normalizing and reporting sample data until further refinements are achieved through additional calibration efforts.

54 ENVIRONMENTAL SCIENCES↗

Iodosodalite synthesis with hot isostatic pressing of precursors produced from aqueous and hydrothermal processes

Iodosodalite powders were synthesized using aqueous and hydrothermal methods, with or without sodium borosilicate glass binders, and then hot isostatically pressed (HIP) at 900 ? and 175 MPa for 3 h to convert into waste forms. After HIPing, the structures, compositions, morphologies, porosities, and leach rates of the aqueous and hydrothermally produced iodosodalite samples were compared. X-ray diffraction patterns of HIPed samples showed that iodosodalite remained as the dominant phase. However, the fraction of the iodosodalite phase decreased after HIPing, indicating decomposition of the iodosodalite structure during the HIP process. Scanning electron microscopy and chemical imaging on the cross sections of HIPed samples showed homogeneous elemental distribution for aqueous-grown iodosodalite, whereas hydrothermally grown iodosodalite samples had more heterogeneity and porosity. The densities of HIPed samples with more glass binder were generally higher than sampled HIPed without binder. The leach tests on samples containing 20 mass% glass binder showed that the iodine dissolution rate of HIPed hydrothermally grown iodosodalite was about 4 times higher than iodosodalite by aqueous method. This study provides alternative techniques for immobilizing iodine-streams in iodosodalite waste forms.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Pilot production & commercialization of LAPPD ™

We present a progress update on plans to establish pilot production and commercialization of Large Area (400 cm2) Picosecond Photodetector (LAPPD™). Steps being taken to commercialize this MCP and LAPPD™ technology and begin tile pilot production are presented including (1) the manufacture of 203 mm×203 mm borosilicate glass capillary arrays (GCAs), (2) optimization of MCP performance and creation of an ALD coating facility to manufacture MCPs and (3) design, construction and commissioning of UHV tile integration and sealing facility to produce LAPPDs. Taken together these plans provide a “pathway toward commercialization”.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗