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At least 487 records · Page 27

Branching ratios for the three most intense gamma rays in the decay of 47 Ca

A sample of 47 Ca produced through isotope harvesting at the National Superconducting Cyclotron Laboratory was used to measure branching ratios of 7.17(5)%, 7.11(5)%, and 75.0(5)% for the 489.2, 807.9, and 1297.1 keV characteristic gamma rays, respectively. Based on these updated branching ratios, the ground state to ground state 47 Ca to 47 Sc beta decay branching ratio has been indirectly measured as 17.7(5)% and the ground state to 1297.1 keV excited state as 82.2(5)%. Here these values represent a greatly increased precision for all five branching ratios compared to the currently accepted values. The measurements presented here were made relative to the ingrown 47Sc daughter in a 47 Ca sample and the well-established 159.4 keV gamma-ray branching ratio and the half-life for the decay of 47 Sc. These measurements were supported by verifying that the half-lives measured from characteristic gamma-ray peaks over multiple spectra for both 47 Ca and 47 Sc were consistent with previously reported values. Additionally, the half-lives of both 47 Ca and 47 Sc were independently measured with Liquid Scintillation Counting to reverify the previously reported values used in this study to find updated gamma-ray branching ratio values.

07 ISOTOPE AND RADIATION SOURCES↗

Proton radiation damage in optical filter glass

Samples of Schott BG-39 and Hoya CM-500 blue-green filter glass were subjected to proton radiation to determine their acceptability for spaceflight. Initial testing done with 2.7 MeV protons showed negligible change in optical transmittance with doses as high as 5.2 x 10 to the 14th protons per sq cm. Irradiation with protons of energy up to 63 MeV caused a significant reduction in transmittance in the Schott samples at doses of 5.3 x 10 to the 12th protons per sq cm, while negligible change occurred in the Hoya samples.

Grillot, Patrick N.↗

Results for the Third Quarter Calendar Year 2018 Tank 50 Salt Solution Sample

In this Technical Report, the chemical and radionuclide contaminant results from the Third Quarter Calendar Year 2018 (CY18) sample of Tank 50 salt solution are presented in tabulated form. The information from this characterization will be used by Savannah River Remediation (SRR) for the transfer of aqueous waste from Tank 50 to the Saltstone Production Facility, where the waste will be treated and disposed in the Saltstone Disposal Facility. This Technical Report compares results, where applicable, to Saltstone Production Facility (SPF) Waste Acceptance Criteria (WAC) limits and targets. The chemical and radionuclide contaminant results from the characterization of the Third Quarter CY18 sampling of Tank 50 were requested by SRR personnel via a Task Technical Request (TTR) and details of the testing are presented in the Savannah River National Laboratory (SRNL) Task Technical and Quality Assurance Plan (TTQAP). This Technical Report is part of Deliverable 2 relating to Task 1 from the SRR request. Data pertaining to the regulatory limits for Resource Conservation and Recovery Act (RCRA) metals will be documented at a later time per the TTQAP for the Tank 50 Saltstone task.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Microbiological Contamination of Spacecraft

The International Space Station (ISS) Phase1 Program resulted in seven US astronauts residing aboard the Russian Space Station Mir between March 1995 and May 1998. Collaboration between U.S. and Russian scientists consisted of collection and analyses of samples from the crewmembers and the Mir and Shuttle environments before, during, and after missions that lasted from 75 to 209 days in duration. The effects of long-duration space flight on the microbial characteristics of closed life support systems and the interactions of microbes with the spacecraft environment and crewmembers were investigated. Air samples were collected using a Russian or U.S.-supplied sampler (SAS, RCS, or Burkard,) while surface samples were collected using contact slides (Hycon) or swabs. Mir recycled condensate and stored potable water sources were analyzed using the U.S.-supplied Water Experiment Kit. In-flight analysis consisted of enumeration of levels of bacteria and fungi. Amounts of microorganisms seen in the air and on surfaces were mostly within acceptability lin1its; observed temporal fluctuations in levels of microbes probably reflect changes in environmental conditions (e.g., humidity). All Mir galley hot water samples were within the standards set for Mir and the ISS. Microbial isolates were returned to Earth for identification of bacterial and fungal isolates. Crew samples (nose, throat, skin, urine, and feces) were analyzed using methods approved for the medical evaluations of Shuttle flight crews. No significant changes in crew microbiota were found during space flight or upon return relative to preflight results. Dissemination of microbes between the crew and environment was demonstrated by D A fingerprinting. Some biodegradation of spacecraft materials was observed. Accumulation of condensate allowed for the recovery of a wide range of bacteria and fungi as well as some protozoa and dust mites.

Pierson, D. L.↗

Application for a Permit to Operate a Class III Solid Waste Disposal Site at the Nevada National Security Site Area 5 Asbestiform Low-Level Solid Waste Disposal Site

The Nevada National Security Site (NNSS) is located approximately 105 km (65 mi) northwest of Las Vegas, Nevada. The U.S. Department of Energy National Nuclear Security Administration Nevada Site Office (NNSA/NSO) is the federal lands management authority for the NNSS and National Security Technologies, LLC (NSTec) is the Management and Operations contractor. Access on and off the NNSS is tightly controlled, restricted, and guarded on a 24-hour basis. The NNSS is posted with signs along its entire perimeter. NSTec is the operator of all solid waste disposal sites on the NNSS. The Area 5 Radioactive Waste Management Site (RWMS) is the location of the permitted facility for the Solid Waste Disposal Site (SWDS). The Area 5 RWMS is located near the eastern edge of the NNSS (Figure 1), approximately 26 km (16 mi) north of Mercury, Nevada. The Area 5 RWMS is used for the disposal of low-level waste (LLW) and mixed low-level waste. Many areas surrounding the RWMS have been used in conducting nuclear tests. The site will be used for the disposal of regulated Asbestiform Low-Level Waste (ALLW), small quantities of low-level radioactive hydrocarbon-burdened (LLHB) media and debris, LLW, LLW that contains Polychlorinated Biphenyl (PCB) Bulk Product Waste greater than 50 ppm that leaches at a rate of less than 10 micrograms of PCB per liter of water, and small quantities of LLHB demolition and construction waste (hereafter called permissible waste). Waste containing free liquids, or waste that is regulated as hazardous waste under the Resource Conservation and Recovery Act (RCRA) or state-of-generation hazardous waste regulations, will not be accepted for disposal at the site. Waste regulated under the Toxic Substances Control Act (TSCA) that will be accepted at the disposal site is regulated asbestos-containing materials (RACM) and PCB Bulk Product Waste greater than 50 ppm that leaches at a rate of less than 10 micrograms of PCB per liter of water. The term asbestiform is used throughout this document to describe RACM. The disposal site will be used as a depository of permissible waste generated both on site and off site. All generators designated by NNSA/NSO will be eligible to dispose regulated ALLW at the Asbestiform Low-Level Waste Disposal Site in accordance with the DOE/NV-325, Nevada National Security Site Waste Acceptance Criteria (NNSSWAC, current revision). Approval will be given by NNSA/NSO to generators that have successfully demonstrated through process knowledge (PK) and/or sampling and analysis that the waste is low-level, contains asbestiform material, or contains PCB Bulk Product Waste greater than 50 ppm that leaches at a rate of less than 10 micrograms of PCB per liter of water, or small quantities of LLHB demolition and construction waste and does not contain prohibited waste materials. Each waste stream will be approved through the Radioactive Waste Acceptance Program (RWAP), which ensures that the waste meets acceptance requirements outlined in the NNSSWAC.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Assessment of Air Quality in the International Space Station (ISS) and Space Shuttle Based on Samples Returned Aboard STS-ll1 (UF2) in June 2002

The toxicological assessments of grab sample canisters (GSCs) and 2 solid sorbent air samplers (SSASs) returned aboard STS-111 are reported. Analytical methods have not changed from earlier reports. Surrogate standard recoveries from the GSCs were 86-106% and 62% to 136 % from the SSASs; 2 tubes with low surrogate recoveries were not reported. Pressure tracking indicated no leaks in the canisters during analysis. Recoveries from lab and trip controls for formaldehyde analyses ranged from 87 to 96%. The two general criteria used to assess air quality are the total-non-methane-volatile organic hydrocarbons (NMVOCs) and the total T-value (minus the CO2 and formaldehyde contributions). Because of the inertness of Freon 218 (octafluoropropane, OFP), Its contribution to the NMVOC is subtracted and tabulated separately. Control of atmospheric alcohols is important to the water recovery system engineers, hence total alcohols (including acetone) are also shown for each sample. Because formaldehyde is quantified from sorbent badges, its concentration is listed separately. The table shows that the air quality in general was acceptable for crew respiration; however, certain values shown in bold require further explanation. The 1.05 T value on 2/28/02 was caused by an unusually high measurement ofhexamethylcyc1otrisiloxane (T value = 0.50), which is not a concern. The MPLM T value of 1.42 and the alcohol level of 7.5 mg/cu m were due to an overall polluted atmosphere, which was expected at first entry. The major T-value component was carbon monoxide at a contribution of 0.44 units. Since the crew was only exposed momentarily to the polluted atmosphere, no health effects are expected. The formaldehyde value of 0.060 mg/cu m found in the Lab sample from 3/27/02 is cause for concern because the Lab consistently shows higher concentrations of formaldehyde than the SM and occasionally the concentrations are above the acceptable guideline. Levels of OFP have remained low, suggesting that no further leaks of the SM air conditioner have occurred.

James, John T.↗

Space‐Time Causal Discovery in Earth System Science: A Local Stencil Learning Approach

Causal discovery tools enable scientists to infer meaningful relationships from observational data, spurring advances in fields as diverse as biology, economics, and climate science. Despite these successes, the application of causal discovery to space-time systems remains immensely challenging due to the high-dimensional nature of the data. For example, in climate sciences, modern observational temperature records over the past few decades regularly measure thousands of locations around the globe. To address these challenges, we introduce Causal Space-Time Stencil Learning (CaStLe), a novel meta-algorithm for discovering causal structures in complex space-time systems. CaStLe leverages regularities in local space-time dependencies to learn governing global dynamics. This local perspective eliminates spurious confounding and drastically reduces sample complexity, making space-time causal discovery practical and effective. For causal discovery, CaStLe flexibly accepts any appropriately adapted time series causal discovery algorithm to recover local causal structures. These advances enable causal discovery of geophysical phenomena that were previously unapproachable, including non-periodic, transient phenomena such as volcanic eruption plumes. Regularities in local space-time dependencies are transformed into informative spatial replicates, which actually improve CaStLe's performance when applied to ever-larger spatial grids. We successfully apply CaStLe to discover the atmospheric dynamics governing the climate response to the 1991 Mount Pinatubo volcanic eruption. We provide validation experiments to demonstrate the effectiveness of CaStLe over existing causal-discovery frameworks on a range of geophysics-inspired benchmarks while identifying the method's limitations and domains where its assumptions may not hold.

Nichol, J. Jake [Univ. of New Mexico, Albuquerque,↗

Measurement of valence-band offsets of InAlN/GaN heterostructures grown by metal-organic vapor phase epitaxy

The valence band offsets, {Delta}E{sub V}, of In{sub 0.17}Al{sub 0.83}N/GaN, In{sub 0.25}Al{sub 0.75}N/GaN, and In{sub 0.30}Al{sub 0.70}N/GaN heterostructures grown by metal-organic vapor phase epitaxy were evaluated by using x-ray photoelectron spectroscopy (XPS). The dependence of the energy position and the full width at half maximum of the Al 2p spectrum on the exit angle indicated that there was sharp band bending caused by the polarization-induced electric field combined with surface Fermi-level pinning in each ultrathin InAlN layer. The {Delta}E{sub V} values evaluated without taking into account band bending indicated large discrepancies from the theoretical estimates for all samples. Erroneous results due to band bending were corrected by applying numerical calculations, which led to acceptable results. The evaluated {Delta}E{sub V} values were 0.2{+-}0.2 eV for In{sub 0.17}Al{sub 0.83}N/GaN, 0.1{+-}0.2 eV for In{sub 0.25}Al{sub 0.75}N/GaN, and 0.0{+-}0.2 eV for In{sub 0.30}Al{sub 0.70}N/GaN. Despite the large decrease of around 1.0 eV in the band gap of InAlN layers according to the increase in the In molar fraction, the decrease in {Delta}E{sub V} was as small as 0.2 eV. Therefore, the change in band-gap discontinuity was mainly distributed to that in conduction band offset.

36 MATERIALS SCIENCE↗

On the mid-infrared variability of candidate eruptive variables (exors): A comparison between Spitzer and WISE data

Aiming to statistically study the variability in the mid-IR of young stellar objects, we have compared the 3.6, 4.5, and 24 μm Spitzer fluxes of 1478 sources belonging to the C2D (Cores to Disks) legacy program with the WISE fluxes at 3.4, 4.6, and 22 μm. From this comparison, we have selected a robust sample of 34 variable sources. Their variations were classified per spectral Class (according to the widely accepted scheme of Class I/flat/II/III protostars), and per star forming region. On average, the number of variable sources decreases with increasing Class and is definitely higher in Perseus and Ophiuchus than in Chamaeleon and Lupus. According to the paradigm Class ≡ Evolution, the photometric variability can be considered to be a feature more pronounced in less evolved protostars, and, as such, related to accretion processes. Moreover, our statistical findings agree with the current knowledge of star formation activity in different regions. The 34 selected variables were further investigated for similarities with known young eruptive variables, namely the EXors. In particular, we analyzed (1) the shape of the spectral energy distribution, (2) the IR excess over the stellar photosphere, (3) magnitude versus color variations, and (4) output parameters of model fitting. This first systematic search for EXors ends up with 11 bona fide candidates that can be considered as suitable targets for monitoring or future investigations.

79 ASTRONOMY AND ASTROPHYSICS↗

Analysis of Harrell Monosodium Titanate Lot #46000619120

Monosodium titanate (MST) for use in the Actinide Removal Process (ARP) must be qualified and verified in advance. A single qualification sample for each batch of material is sent to SRNL for analysis, as well as a statistical sampling of verification samples. The Harrell Industries Lot #46000619120 qualification and the 13 verification samples met each of the selected specification requirements that were tested and, consequently, the material is acceptable for use in the ARP process.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Impact of Standing Bleed Water on Saltstone Placement

The amount of water present during placement and subsequent curing of saltstone has the potential to impact several properties important for grout quality. An active drain water system can remove residual standing water and expose the surface of the placed saltstone to air. Oxidation of the saltstone may result in an increase in the leachability of redox sensitive elements. A dry surface can lead to cracking, causing an increase in hydraulic conductivity. An inactive drain water system can allow standing water that generates unnecessary hydrostatic head on the vault walls. Standing water that cannot be removed via the drain system will be available for potential incorporation into subsequent grout placements. The objective of this work is to study the impact of standing water on grout quality pertaining to disposal units. A series of saltstone mixes were prepared, and cured at ambient temperature to evaluate the impact of standing water on saltstone placement. The samples were managed to control drying effects on leachability by either exposing or capping the samples. The water to premix ratio was varied to represent a range of processing conditions. Samples were analyzed for density, leachability, and hydraulic conductivity. A monolith of each composition was cut into four sections to analyze the homogeneity of the sample with respect to vertical position within the sample. The density of each section was measured by two methods, helium pycnometry and by ASTM 642-06. The results show a trend of increasing density with increasing depth in the samples. This effect is more pronounced with the inclusion of excess bleed water and indicative of increased settling. The leachability of the eight different samples was analyzed by ANS/ANSI 16.1 method. These results indicate that drying of the saltstone during curing leads to decreased Leachability Indices (indicative of more release) for potassium, sodium, rhenium, nitrite, and nitrate. This may be caused by shrinkage cracking in the samples creating additional pathways for contaminant release. There was no noticeable effect on leachability by changing the water to premix ratio or by including excess bleed water. There was no detectable chromium release in any of the samples. Chromium and rhenium were added in equal amounts to determine whether rhenium might be an acceptable surrogate for chromium, a hazardous material. This testing shows no correlation between the behavior of the two elements, as chromium is not released at detectable levels and rhenium is released at a comparable rate to nitrate, the most prevalent and mobile species in saltstone.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Product consistency test results for the LAW Phase 4 gases

In this report, the Savannah River National Laboratory provides chemical analysis of Product Consistency Test (PCT) leachates from a series of simulated nuclear waste glasses fabricated at the Pacific Northwest National Laboratory (PNNL). The series included quenched and canister-centerline cooled (CCC) versions of the glasses. The resulting data will be used in the development of enhanced property/composition models for waste vitrification at Hanford. For some of the glass leachates, minor scatter among the triplicate values of some analytes were observed. For other leachates, there were more significant differences among the triplicate values. A review of the PCT data noted that there was little difference between the normalized values based on targeted or measured glass composition. Several of the study glasses have normalized concentration of element “i” (NCi) values that are greater than the Hanford Tank Waste Treatment and Immobilization Plant immobilized low-activity waste constraint of 4 g/L for boron (B), sodium (Na), and silicon (Si). The results of these glasses will help ensure the ability of advanced glass performance models to appropriately predict acceptable compositions. For the study glasses with NCi values exceeding 4 g/L, the CCC heat treatment samples had generally lower NCi values than quenched samples. The samples of the Environmental Assessment (EA) reference glass included with each PCT set had generally consistent NCi values. The release rates for boron (B), potassium (K), lithium (Li), sodium (Na), and silicon (Si) were highly correlated for the study glasses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NASTRAN Benefits Analysis. Volume 1: Executive Summary

The acceptance of NASTRAN, the NASA structural analysis computer program, is explored, based on data from a sample set of users. Baseline data are generated for future comparison of costs and benefits of the program. The impact on, and benefits to, segments of government and industry from current use of NASTRAN are considered. Ways in which potential users may benefit from application of the program to their individual needs are also discussed.

Source record↗

Rapid Analysis of Carbohydrates in Bioprocess Samples: An Evaluation of the CarboPac SA10 for HPAE-PAD Analysis by Interlaboratory Comparison

A technique for carbohydrate analysis for bioprocess samples has been developed, providing reduced analysis time compared to current practice in the biofuels R&D community. The Thermofisher CarboPac SA10 anion-exchange column enables isocratic separation of monosaccharides, sucrose and cellobiose in approximately 7 minutes. Additionally, use of a low-volume (0.2 mL) injection valve in combination with a high-volume detection cell minimizes the extent of sample dilution required to bring sugar concentrations into the linear range of the pulsed amperometric detector (PAD). Three laboratories, representing academia, industry, and government, participated in an interlaboratory study which analyzed twenty-one opportunistic samples representing biomass pretreatment, enzymatic saccharification, and fermentation samples. The technique's robustness, linearity, and interlaboratory reproducibility were evaluated and showed excellent-to-acceptable characteristics. Additionally, quantitation by the CarboPac SA10/PAD was compared with the current practice method utilizing a HPX-87P/RID. While these two methods showed good agreement a statistical comparison found significant quantitation difference between them, highlighting the difference between selective and universal detection modes.

09 BIOMASS FUELS↗

Ranking of Chemicals Measured in Emissions from R&D Facilities

The Pacific Northwest National Laboratory (PNNL) operates a number of multidisciplinary laboratory research facilities for the U. S. Department of Energy and has sampled air chemical emissions from some of these facilities since 1998. The primary purpose of this sampling is to obtain data to compare estimated release fractions to those used for emissions estimates, verifying that methods used to determine compliance with air regulations and permits conservatively predict actual emissions. Sampling also identifies and quantifies emissions of air toxics to compare with compliance limits established by regulatory agencies. Hundreds of samples have been taken from four different buildings (325, 329, 331, and EMSL) over a 10-year time period. Results from initial sampling campaigns were evaluated and reported by Woodruff, Benar, and McCarthy (2000) who summarized the compliance approach used by PNNL and described sampling and analytical measurements for the first sampling campaigns. Conclusions reported in this paper were that none of the measurements of the target compounds exceeded an acceptable source impact level (ASIL) (Washington Administrative Code, Chapter 173-460) even using significant overestimation factors, and that an average release fraction calculated from the data provided reasonable validation of the factor used in compliance assessments. Subsequent analysis compared chemical signatures from the buildings (Ballinger, Duchsherer, and Metoyer 2008). Results from this analysis showed that stack emissions from three of the four buildings had relatively similar chemical signatures but the fourth building differed from the other three significantly using the developed metric. This paper presents additional analyses of the measured air chemical emissions to 1) rank the chemical compounds that present the greatest risk to a potential downstream receptor and 2) determine whether the sampling parameters and detection limits provided sufficient resolution to verify compliance at potential receptor locations. The ranking method includes chemical-specific parameters such as measured concentrations, detection limits, and regulatory limits plus building-specific parameters such as location, stack flow-rate, and distance to receptors.

54 ENVIRONMENTAL SCIENCES↗

Sampling Size Optimization for Bioburden Density Estimation in Planetary Protection

Planetary protection (PP) is a discipline that focuses on minimizing the biological contamination of spacecraft to ensure compliance with international policy. Precise estimation of bioburden - the total number of microbes in or on spacecraft hardware – and the bioburden density are of utmost importance for PP. Such estimation is the way concordance with requirements is demonstrated, and it is critical for quantifying the potential risk of inadvertently contaminating other planetary bodies. Although a suite of molecular techniques have been used to thoroughly characterize and profile the microbiome of various cleanroom environments and spacecraft, the gold standard remains the physical enumeration of microbes via culturing of samples directly taken from spacecraft and associated surfaces. However, due to technical, budgetary, and programmatic constraints, only a manageable portion (around 10%) of the entire spacecraft surface is directly sampled with cotton swabs or wipes. To generate the bioburden current best estimate (CBE) for components not directly verifiable, the accepted approach is to apply a NASA-defined bioburden estimate based on the components’ manufacturing or assembly environment. This approach utilizes a prespecified bioburden density estimation that applies a maximum value across the total surface area of the specified component. For hardware components that underwent similar assembly processes, an implied bioburden is adopted for all components, based on a direct verification of a representative component within the same lot. Once all components have a CBE, the bioburden estimates are generated. In previous publication [ 1], we have shown that statistical risks quantifying the accuracy of the estimates for sampled, prespecified, and implied components can be derived and ranked. For mean squared error (MSE) function, the risks are available analytically and hence a cost function can be obtained to optimize the risks with respect to the sampling area and sampling cost. Since the sampling area and sampling cost are two complimentary variables, their sum will have a well-defined minimum. This paper presents the multivariate optimization of the integrated risk of an empirical Bayes estimator to determine the optimal sampling schedule for a given number of components. It is assumed that given a number of components, N, the bioburden density for each component can either be sampled, implied, or prespecified. The multivariate optimization searches through different options to sample, imply or prespecify the bioburden density for a component, and account for the component’s surface area and cost of sampling. The idea of the optimization is based on the observation that the statistical risk of using an estimator is a monotonically decreasing function of the sampled area. The larger the sampled area, the lower the risk of using the estimator as the estimator becomes more and more accurate as the sampling area increases. On the other hand, the cost of sampling is monotonically increasing as the sampled surface grows. This makes the risk and total cost of sampling complimentary variables which can be counterbalanced to achieve an optimal overall value with respect to the sampled surface. In this paper, the integrated risk has been used to quantify the accuracy of the estimator. This risk has been selected because it depends on neither the true value of the parameter nor on the collected data. The cost of each sample was also available to obtain the total cost of sampling of N components. The paper will present the results based on computer-simulated data as well as the data collected during the InSight mission. The computer-simulated data have N components with randomly generated total areas and each component assigned to one of the three categories according to the method of estimating of bioburden density: sampled, implied, or prespecified. The cost of sampling is also available. The cost of sampling is estimated based on a cost model provided by the planetary protection group at JPL. For this paper, the overall cost was assumed to be a linear function of exposure. The optimization process finds the allocation of the components to the three categories that minimizes the tradeoff between integrated risk and total cost. For the InSight data, a set of components is selected representing all three categories, and optimization is performed to determine if the performed allocation was optimal or if a better allocation could have been obtained. To the best of our knowledge, this work is the first attempt not only perform an accurate estimation of bioburden density but also do it in an optimal way.

97 - MATHEMATICS AND COMPUTING↗

Destructive Analysis of TRISO Particles: Crush/Burn/Leach Followed by Davies-Gray Titration and IDMS

The accurate accounting of nuclear materials is a cornerstone of international nuclear safeguards. One emerging challenge in this domain is the fabrication of TRIstructural ISOtropic (TRISO) particle fuels. Although these innovative fuel forms are critical for advanced reactor applications, their robust refractory ceramics and coating compositions present significant obstacles to destructive analysis (DA) methods. Ensuring full and quantitative recovery from these particles is essential for accurate mass accountancy. The current study was initiated to address these challenges, first by validating a previously established destructive method developed by Oak Ridge National Laboratory (ORNL) for the quantitative recovery of uranium from TRISO particles and then following that process with uranium content determination through isotope dilution mass spectrometry (IDMS) and Davies-Gray titration. This study expands on the scope of a digestive method that was developed under the Advanced Gas Reactor Fuel Development and Qualification program and is currently implemented in both the Coated Particle Fuel Development Laboratory and Irradiated Fuels Examination Laboratory at ORNL. The success of the previous Advanced Gas Reactor work relied on developing a DA method to evaluate the fabrication process and reactor experiments. The methodology described in this report was designed to rigorously investigate the efficacy of the crush/burn/leach sample preparation of TRISO particles; it aims to quantify uranium recovery while also assessing the effects of TRISO constituents (e.g., silicon and zirconium) on analytical precision and accuracy. By comparing the results from the titration method and IDMS, we sought to determine whether existing analytical procedures accepted by the International Atomic Energy Agency (IAEA) could be effectively translated to TRISO fuel forms. The team employed an approach that involved processing replicate TRISO samples, optimizing the milling (i.e., crushing) step and performing serial leaches. The elemental composition of the analytical samples was examined to prepare for interference studies in the second year of this project. The integration of gamma spectrometry to verify residual uranium activity further strengthened the validation. Statistical methods were applied to the collected data to evaluate the uncertainties arising from sampling, sample preparation and uranium quantification. These uncertainties were then compared to the IAEA’s international target values (ITVs). Additional data collected in upcoming project work will strengthen the uncertainty estimates. Ultimately, it is hoped that this project will contribute materially to the body of work related to characterization of TRISO based fuels for the purpose of material accountancy and its applications to international safeguards.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Potential Challenges in Near-Field Scanning Optical Microscopy for Space Applications

Near-field scanning optical microscopy (NSOM) also called scanning near-field optical microscopy (SNOM) is now well accepted as a powerful tool for sub-wavelength (nanoscale in the optical region) spatial resolution microscopy and a large number of related tasks. The importance lies in the fact of strategic advantages of standard microscopy but with significantly enhanced resolution. Since many modern optical diagnostic techniques have found useful applications in space, it is logical to consider the future role of NSOM in such situations. For example, protein crystal growth study under microgravity conditions is a valid candidate. If applied successfully, processes at molecular level can be studied during the growth. NSOM has already been demonstrated to be useful for the study of such crystals here on earth. The basic principle of NSOM can be illustrated. The illumination-collection mode is shown although several other possible approaches exist. In this, the sample is illuminated and the light from the sample is collected through the same tiny aperture opening. A tapered optical fiber is scanned near the sample surface. The tip is coated generally with a metal with a sub-wavelength aperture opening. The tip-sample distance is maintained constant while scanning. Thus, the optical signal available for collection is generally a function of the optical properties of the sample surface. Since the aperture is sub-wavelength in diameter and the tip is held very close (again in the sub-wavelength domain) to the surface, the lateral resolution in the sub-wavelength domain is obtained. Thus, the typical wavelength- order resolution of ordinary microscopy can be significantly enhanced while maintaining the strategic advantages (no need of sample in vacuum chamber, electron beams, etc). Commercial NSOM systems play a key role in the success and widespread acceptance of the tool. These commercial systems work fairly well in laboratory conditions on earth. However, they may not be deployed on a space mission as such with comparable outcome. In this communication we discuss several potential problems and some possible solutions.

Vikram, Chandra S.↗