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At least 163 records · Page 9

Analysis of Tank 38H (HTF-38-20-62, -63) and Tank 43H (HTF-43-20-60, -61) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The results indicate the concentrations of most species in the Tank 38H surface sample increased from the previous surface sample. The Tank 38H sub-surface sample shows only small changes in concentration for most major species in the solution from the previous sample. The large differences in the concentrations of major components between the Tank 38H surface and sub-surface samples indicate significant stratification of solution species within the tank. The Tank 38H surface and sub-surface samples both contained a small amount of sludge solids (<1 wt%). The Tank 43H surface and sub-surface samples are slightly more dilute than the previous samples. The Tank 43H sub-surface sample exhibits a composition more concentrated than the surface sample indicating some stratification within the tank. The Tank 38H surface and sub-surface sample both show large increases in the concentrations of uranium and plutonium likely due to the presence of sludge solids in both samples. (Note: the samples were digested and analyzed without filtration.) The total uranium concentrations of the two Tank 43H samples are similar to the previous sample results. The plutonium concentration in both Tank 43H samples appear to have decreased from the previous samples; however, the surface sample concentrations are close to the detection limit.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Solvent hold tank sample results for MCU-17-150-152 (July 2017) and MCU-17-153-155 (August 2017): Quarterly report

A trend summary that includes the last two Solvent Hold Tank (SHT) monthly samples is shown; MCU- 17-150-152 (July SHT) and MCU-17-153-155 (August SHT). Since the last SHT sample sent for analysis was the August sample the chemical state of the solvent is best approximated by the chemical analysis of the August SHT sample (MCU-17-153-155). This report mainly focused on the chemical analysis of the August SHT sample. The analysis data from the July SHT sample are presented in the “trend” plots of this report. Analysis of the August SHT sample (MCU-17-153-155) indicated that the modifier (CS-7SB) was 2% below but the extractant (MaxCalix) concentration was at its nominal recommended level (169,000 mg/L and 46,400 mg/L respectively). The suppressor (TiDG) level has decreased since the last measurement taken while the Modular Caustic-Side Solvent Extraction unit (MCU) was operating in January 2017, but has remained steady in the range of 666 (observed in April) to 715 mg/L (observed in the August 2017 sample) since February 2017, well above the minimum recommended level (479 mg/L), but below the nominal level. The “flat” trends observed in the TiDG, MaxCalix, modifier, and Gamma measurement are consistent with the solvent being idle since January 10, 2017. A strong correlation between density and modifier concentration in the solvent continues to be observed in the SHT samples. This analysis confirms the Isopar™L addition to the solvent in January 2017. This analysis also indicates the solvent did not require further additions. Based on the current monthly sample, the levels of TiDG, Isopar™L, MaxCalix, and modifier are sufficient for continuing operation but are expected to decrease with time if the Modular Caustic-Side Solvent Extraction Unit (MCU) returns to processing radioactive liquid waste. Otherwise, the levels of these components will remain steady. A future Isopar™L trimming addition to the solvent is recommended when MCU resumes processing waste. Two unknown impurities related to the modifier (but not sec-butyl phenol: a modifier degradation product observed before) at the 290 and 110 mg/L levels were observed in the August SHT sample by the Gas - Chromatography-Mass Spectrometry (GC-MS) method. They were observed in a second GC-MS re-run with a new column. Their identification can’t be ascertained at this time. No impurities were observed in the Hydrogen Nuclear Magnetic Resonance (HNMR). Another impurity observed in the samples was mercury. Based on the August SHT sample, up to 23 ± 5 micrograms of mercury per mL of solvent was detected (the average of the Cold Vapor-Atomic Adsorption [CV-AA] and X-Ray Fluorescence [XRF] methods). The higher mercury concentration in the solvent (as determined in the last three-monthly samples) is possibly due to either a higher mercury concentration in Salt Batches 8 and 9 (Tank 49H) . The gamma level (~ 2.0E4 dpm/mL) measured in the August SHT samples was one order of magnitude lower than the gamma levels observed in the December 2016 and January 2017 SHT samples. A similar level was observed in the July SHT sample (MCU-SHT-150-152). The gamma level has remained consistently steady since January 10, 2017 when MCU stopped processing radioactive liquid waste. The laboratory will continue to monitor the quality of the solvent in particularly for any new impurities or degradation of the solvent components.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

First Annual Progress Report on the Procurement and Post-Irradiation Examination of the Selected Samples of Alloy 800H and Grade 92 and 91 Steels

Ferritic-martensitic steel Grade 92, with Grade 91 as a reference, together with austenitic stainless steel (or Incoloy Alloy) 800H and its grain-boundary-engineered version 800H-TMP (Thermo-Mechanical Processing), is investigated in this project. A total of fifteen Grade 92 samples from two or three heats, four T91 samples from two heats, and six 800H and six 800H-TMP samples from one heat were selected, which were primarily irradiated in the Advanced Test Reactor (ATR) of Idaho National Laboratory (INL), with the rest in the High Flux Isotope Reactor (HFIR) of Oak Ridge National Laboratory (ORNL), BOR-60 of Russia, and Phénix reactor of France. The samples were irradiated in the temperature range of 241 to 720°C and a dose range of 1.28 to ~70 displacements per atom. All the INL and ORNL samples and part of the LANL (Los Alamos National Laboratory) samples have been received at the Irradiated Materials Examination and Testing (IMET) hot cell facility. The selected ORNL samples include six Grade 92 and two 800H samples, which were irradiated in the HFIR to 0.46–14.66 dpa at 400 to ~720°C. The Grade 92 is an optimized heat and named as G92-2b. The two 800H samples have one sample as the standard solution-annealed condition and the other sample as a TMP condition with a maximized fraction of low-Σ coincidence site lattice (CSL) boundaries. Tensile test of the G92-2b samples were conducted at room temperature in the IMET hot cell. The lower temperature irradiation at 400–496.7°C to 0.52–14.66 dpa resulted in minimal changes in tensile properties. However, the higher temperature irradiation at ~683.3–720°C to 0.46–14.63 dpa tended to reduce yield and tensile strength by about –136 to –311 MPa and plastic elongation by –1 to –3% with the increasing dose. The 800H and 800H-TMP samples were tensile-tested at their irradiation temperature 580°C in the IMET hot cell, which showed >40% increase in yield and tensile strength with nearly 9% reduction in elongation for 800H-TMP compared with 800H. Three of the G92-2b samples, i.e., GB04 (7.44 dpa at ~490°C), GB05 (14.66 dpa at 496.7°C), and GB12 (14.63 dpa at ~720°C), were examined at the LAMDA for Vickers hardness measurements and microstructural characterization by SEM and TEM. Vickers hardness was successfully measured on GB12, which was reduced by is – (112.4 ± 12.3) HV1 from the control sample. However, the Vickers hardness measurements were failed on GB04 and GB05 because the samples were polished too thin to prevent the interference from the substrate (epoxy). The other half of the GB04 and GB05 will be polished for the hardness measurements, as well as nanoindentation studies. Fractography by SEM indicated increased numbers of ductile dimples (or voids) with the increasing irradiation dose, while significantly increased numbers and sizes of dimples with the increasing irradiation temperature. TEM characterization exhibited the presence of Cr 23 C 6 , VN, and Laves precipitates at boundaries and matrix, which showed pronounced precipitate-dislocation interactions (pinning effect). Dense dislocations but limited dislocation loops were observed in the samples, which noticeably reduced in GB12. Additionally, some tiny partially amorphized spherical domains were observed in GB12, which had a normal body-centered cubic lattice parameter of 9Cr steels at the surround regions but ~11% smaller than the lattice parameter of the matrix away from the amorphized spherical domains. Further characterization will be pursued to clarify the new findings.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Nevada Higher Education Benefits from US Department of Energy (DOE) Environmental Management (EM) Nevada Program's Transfer of Geologic Samples - 20442

The Nevada National Security Site (NNSS), formerly the Nevada Test Site, was the location of 100 historic atmospheric and 828 historic underground nuclear tests from 1951 to 1992. Related to this historic nuclear testing, geologic and hydrologic studies of the site were conducted utilizing the skills and the expertise of the U.S. Geological Survey (USGS) and national laboratories (Los Alamos National Laboratory, Lawrence Livermore National Laboratory), who were principal in leading the development of weapons and were responsible for specific underground testing programs. The subsurface samples and technical/scientific data associated with NNSS geologic studies (past and present) are preserved and stored at the USGS Mercury Core Library and Data Center located at the NNSS. Currently, the facility stores over 2,000,000 linear feet of cores and cuttings from more than 2,600 drill holes that can be accessed for study. Most of the samples and historic geologic work was focused directly on subsurface geologic settings that relate directly to historic underground nuclear testing. Since 1992, the United States has observed a unilateral moratorium on full-scale nuclear testing, and the U.S. Department of Energy (DOE) Environmental Management (EM) Nevada Program is now responsible for hydrogeologic characterization of the potential impacts to the natural groundwater systems that may have resulted from historic underground nuclear tests. As part of this effort, the EM Nevada Program Underground Test Area (UGTA) Activity has drilled and completed over 58 deep (2,000 - 7,000 ft.) characterization wells, totaling in excess of 170,000 linear feet of cuttings and core samples. Cutting samples were collected as triplicate samples for each respective depth interval, to account for potential later nondestructive/destructive analysis and to preserve samples for regulatory purposes. Recently, it was recognized by the EM Nevada Program that opportunities may exist to reduce the cost and floor space required for the storage of geologic samples at the Mercury Core Library without impacting the integrity and representative nature of the samples necessary for project execution. An initiative was sponsored by EM Nevada Program to evaluate several options: 1) disposal of a portion of cuttings and cores in a land fill setting; 2) reduction in sample volume through skeletonizing core and cuttings from wells to a representative but much smaller number of samples; and 3) solicit potential interest in the academic community where other geoscientists could freely access the samples for studies. The Nevada state university system through the Nevada Bureau of Mines and Geology responded positively to the opportunity to receive these NNSS samples from the EM Nevada Program. In June 2019, approximately 17,000 geologic samples, representing greater than 170,000 linear feet of drilling and weighing over 20,000 pounds, were shipped from the NNSS to the Great Basin Science Sample and Records Library located in Reno, Nevada. The benefits resulting from this transfer were realized by the EM Nevada Program in terms of cost and space savings for geologic sample storage at the NNSS. The transfer did not impact the EM Nevada Program mission as access to representative geologic samples for regulatory and scientific purposes was preserved. Moreover, the Nevada Bureau of Mines and Geology acquired a significant resource of subsurface geologic samples and supporting technical data to support academic and scientific studies in a complex volcanic setting in southwest Nevada. (authors)

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Analysis of Tank 38H (HTF-38-17-52, -53) and Tank 43H (HTF-43-17-54, -55) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 41.3 mg/L while the sub-surface sample was 43.5 mg/L. The Tank 43H samples contained total uranium concentrations of 28.5 mg/L in the surface sample and 28.1 mg/L in the sub-surface sample. The U-235 percentage ranged from 0.62% to 0.63% for the Tank 38H samples and Tank 43H samples. The total uranium and percent U-235 results in the table appear slightly lower than recent Tank 38H and Tank 43H uranium measurements. The plutonium results in the table show a large difference between the surface and sub-surface sample concentrations for Tank 38H. The Tank 43H plutonium results closely match the range of values measured on previous samples. The Cs-137 results for the Tank 38H surface and sub-surface samples show similar concentrations slightly higher than the concentrations measured in recent samples. The Cs-137 results for the two Tank 43H samples also show similar concentrations within the range of values measured on previous samples. The four samples show silicon concentrations somewhat lower than the previous samples with values ranging from 124 to 168 mg/L.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Tank 38H (HTF-38-18-43, -44) and Tank 43H (HTF-43-18-41, -42) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 38.8 mg/L while the sub-surface sample was 35.7 mg/L. The Tank 43H samples contained total uranium concentrations of 27.5 mg/L in the surface sample and 23.4 mg/L in the sub-surface sample. The U-235 weight fraction ranged from 0.62% to 0.63% for the Tank 38H samples and Tank 43H samples. The total uranium concentrations in the table are reasonably consistent with recent Tank 38H/43H sample uranium measurements. The plutonium results in the table are consistent with the range of concentrations measured in recent samples from these tanks with the exception of the Pu-238 value measured in the Tank 43H sub-surface sample. The Pu-238 in the Tank 43H sub-surface sample is higher than any recent measurement by a factor of two. The Cs-137 results show slightly lower concentrations in the surface samples versus the sub-surface samples from each tank. The non-radioactive components of the samples show some differences between the surface and sub-surface samples for each tank.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Tank 38H (HTF-38-18-43,-44) and Tank 43H (HTF-43-18-41, -42) Samples for Support of the Enrichment Control and Corrosion Control Programs

SRNL analyzed samples from Tank 38H and Tank 43H to support ECP and CCP. The total uranium in the Tank 38H surface sample was 38.8 mg/L while the sub-surface sample was 35.7 mg/L. The Tank 43H samples contained total uranium concentrations of 27.5 mg/L in the surface sample and 23.4 mg/L in the sub-surface sample. The U-235 weight fraction ranged from 0.62% to 0.63% for the Tank 38H samples and Tank 43H samples. The total uranium concentrations in the table are reasonably consistent with recent Tank 38H/43H sample uranium measurements. The plutonium results in t he table are consistent with the range of concentrations measured in recent samples from these tanks with the exception of the Pu-238 value measured in the Tank 43H sub-surface sample. The Pu-238 in the Tank 43H sub-surface sample is higher than any recent measurement by a factor of two. The Cs-137 reslts show slightly lower concentrations in the surface samples versus the sub-surface samples from each tank. The non-radioactive components of the samples show some differences between the surface and sub-surface samples for each tank.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Additional Analysis of the 2H-Evaporator Wall Scale Sample HTF-17-57

Savannah River National Laboratory previously analyzed scale samples from both the wall and cone sections of the 242-16H Evaporator prior to chemical cleaning. The samples were analyzed for uranium and plutonium isotopes required for a Nuclear Criticality Safety Assessment of the scale removal process. The analysis of the scale samples found the material to contain crystalline nitrated cancrinite and clarkeite and significant amounts of mercury. Savannah River Remediation subsequently requested additional analyses on the samples. Inspection of the sample bottles revealed that no sample remained of the cone scale (HTF-17-56) while approximately 4 g of the wall scale sample (HTF-17-57) remained. The wall sample was subsequently ground with a mortar and pestle, at which time it was discovered that the sample contained a significant amount of liquid, metallic mercury. The portion of the sample that was not mercury was approximately 3 g. This portion of the sample was analyzed to determine the concentrations of selected radionuclides. The following radionuclide concentrations were measured: <9.6E+02 dpm/g H-3, 2.9E+02 dpm/g C-14, 5.6E+03 dpm/g Tc-99, and 1.6E+02 dpm/g I-129. Blank samples were also analyzed to evaluate sample contamination from the Shielded Cells environment. All blank sample results were below detectable limits. Due to the limited sample size and the anticipated low levels of the target radionuclides, no replicate sample analysis was conducted.

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Focused‐beam X‐ray fluorescence and diffraction microtomographies for mineralogical and chemical characterization of unsectioned extraterrestrial samples

Abstract This study describes the application of new synchrotron X‐ray fluorescence (XRF) and diffraction (XRD) microtomographies for the 3‐D visualization of chemical and mineralogical variations in unsectioned extraterrestrial samples. These improved methods have been applied to three compositionally diverse chondritic meteorite samples that were between 300 and 400 μm in diameter, including samples prepared from fragments of the CR2 chondrite LaPaz Icefield (LAP) 02342, H5 chondrite MacAlpine Hills (MAC) 88203, and the CM2 chondrite Murchison. The synchrotron‐based XRF and XRD tomographies used are focused‐beam techniques that measure the intensities of fluorescent and diffracted X‐rays in a sample simultaneously during irradiation by a high‐energy microfocused incident X‐ray beam. Measured sinograms of the emitted and diffracted intensities were then tomographically reconstructed to generate 2‐D slices of XRF and XRD intensity through the sample, with reconstructed pixel resolution of 1–2 μm, defined by the resolution of the focused incident X‐ray beam. For sample LAP 02342, primary mineral phases that were visualized in reconstructed slices using these techniques included isolated grains of α‐Fe, orthopyroxene, and olivine. For our sample of MAC 88203, XRF/XRD tomography allowed visualization of forsteritic olivine as a primary mineral phase, a vitrified fusion crust at the sample surface, identification of localized Cr‐rich spinels at spatial resolutions of several micrometers, and imaging of a plagioclase‐rich glassy matrix. In the sample of Murchison, major identifiable phases include clinoenstatite‐ and olivine‐rich chondrules, variable serpentine matrix minerals and small Cr‐rich spinels. Most notable in the tomographic analysis of Murchison is the ability to quantitatively distinguish and visualize the complex mixture of serpentine‐group minerals and associated tochilinite–cronstedtite intergrowths. These methods provide new opportunities for spatially resolved characterization of sample texture, mineralogy, crystal structure, and chemical state in unsectioned samples. This provides researchers an ability to characterize such samples internally with minimal disruption of sample micro‐structures and chemistry, possibly without the need for sample extraction from some types of sampling and capture media.

Geochemistry & Geophysics↗

Report on partially complete post-irradiation-examination of the INL samples

Ferritic-martensitic steels (NF616 and T91), and austenitic stainless steel 800H and its Grain Boundary Engineering (GBE)-treated version 800H-TMP (ThermoMechanical Processing) were irradiated in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) and their microstructures and mechanical properties were characterized. Ferritic-martensitic steels were irradiated up to 8.16 dpa in the irradiation temperatures ranging from 241 °C to 447.5 °C. Selected 800H and 800H-TMP samples were also irradiated up to 9.12 dpa at 359°C to 431°C. Vickers hardness measurement, fractography, and microstructural characterization were performed on the selected samples in the LAMDA lab. Radiation-induced hardening of NF616 and T91 was observed in the hardness measurements which show ~37% to ~65% increases, depending on irradiation dose and irradiation temperature. Within the irradiation conditions studied in this work, samples with a higher dose had a higher hardness. All the tested alloy 800H and 800H-TMP in this work showed irradiation-hardening by ~96±7% to ~152±10%. Alloy 800HTMP tended to have slightly smaller irradiation-hardening than alloy 800H. The fractography of NF616 samples D2 (2.96 dpa at 291.5°C), D4 (5.91 dpa at 359°C), and D6 (8.16 dpa at 431°C) indicated loss of ductility with negligible necking for the sample D2, yet obvious ductile failure for samples D4 and D6. Fractography of alloy 800H samples N4 (7.27 dpa at 359°C), N5 (3.9 dpa at 451.5°C), and N6 (9.01 dpa at 431°C), and alloy 800H-TMP samples P4 (7.36 dpa at 359°C), P5 (3.95 dpa at 451.5°C), and P6 (9.12 dpa at 431°C) indicated that all samples failed in a ductile mode, with obvious necking. Dimples were observed where large Ti-containing particles were observed for the samples. TEM characterization was performed on alloy 800H (N4, N5, N6) and 800H-TMP (P4, P5 and P6). Accumulation of M23C6 precipitates at grain boundaries was observed in all samples, and the presence of Ti(C,N) precipitates at grain boundaries and in the matrix was observed in alloy 800H-TMP. M23C6 precipitates were found to have the cube-on-cube orientation relationship with the matrix. In addition, nanoscale Si-rich clusters were observed in the matrix of all samples. Atom probe tomography was conducted on the same samples, and their results are being analyzed to be integrated with the TEM results for a confident description of the clustering behavior. Due to the low irradiation temperature (up to 451.5°C), dislocation loops formed in all samples, with the density and the average size of dislocation loops in the order of 1022 – 1023 m-3 and 11.7 – 15.9 nm, respectively. The loop densities in alloy 800H were higher than that in alloy 800H-TMP under the same irradiation conditions. Further systematic data analyses, together with some complementary experiments, will be pursued for these samples to foster peer-reviewed journal article publications.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Surface Sampling Techniques for the Canister Deposition Field Demonstration

This report describes plans for dust sampling and analysis for the multi-year Canister Deposition Field Demonstration. The demonstration will use three commercial 32PTH2 NUHOMS welded stainless steel storage canisters, which will be stored at an ISFSI site in Advanced Horizontal Storage Modules. One canister will be unheated; the other two will have heaters to achieve canister surface temperatures that match, to the degree possible, spent nuclear fuel (SNF) loaded canisters with heat loads of 10 kW and 40 kW. Surface sampling campaigns will take place on a yearly or bi-yearly basis. The goal of the planned dust sampling and analysis is to determine important environmental parameters that impact the potential occurrence of stress corrosion cracking on SNF dry storage canisters. Specifically, the size, morphology, and composition of the deposited dust and salt particles will be quantified, as well as the soluble salt load per unit area and the rate of deposition, as a function of canister surface temperature, location, time, and orientation. Sampling locations on the canister surface will nominally include 25 locations, corresponding to 5 circumferential locations at each of the 5 longitudinal locations. At each sampling location, a 2x2 sampling grid (containing 4 sample cells) will be painted onto the metal surface. During each sampling campaign, two samples at each sampling location will be collected, in a specific routine to measure both periodic (yearly or bi-yearly) and cumulative deposition rates. For each sample, a wet and a dry sample will be collected. Wet samples will be analyzed to determine the composition of the soluble salt fraction and to estimate salt loading per unit area. Dry samples will be analyzed to assess particle size, morphology, mineralogy, and identity (e.g. for floral/faunal fragments). The data generated by this proposed sampling plan will provide detailed information on dust and salt aerosol deposits on spent nuclear fuel canister surfaces. The anticipated results include information regarding particle compositions, size distributions, and morphologies, in addition to particle deposition rates as a function of canister surface location, orientation, time, and temperature. The information gathered during the Canister Deposition Field Demonstration is critical for ongoing efforts to develop a detailed understanding of the potential for stress corrosion cracking on SNF dry storage canisters

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of Tank 38H (HTF-38-25-36, -32) and Tank 43H (HTF-43-25-33, -35) Samples for Support of the Enrichment Control and Corrosion Control Programs

Savannah River National Laboratory (SRNL) analyzed samples from Tank 38H and Tank 43H to support the Enrichment Control Program (ECP) and Corrosion Control Program (CCP). The results indicate the concentrations of most soluble species in the Tank 38H surface sample are similar to the previous Tank 38H surface sample. The current Tank 38H subsurface sample shows similar Na, free hydroxide, and anions in comparison to the previous subsurface sample. The current Tank 38H subsurface sample appears brown in color. Measurement of the wt.% insoluble solids in the Tank 38H subsurface sample and associated uncertainty analysis indicates that the calculated average wt.% insoluble solids is 5.5 ± 3.6 wt.%. Significant differences in the concentrations of major components between the Tank 38H surface and subsurface samples indicate stratification of solution species between these two locations within the Tank 38H. The current Tank 43H surface sample is ~ 10% diluted versus the previous Tank 43H surface sample and the Tank 43H subsurface sample is similar in composition to the previous Tank 43H subsurface sample. Information provided by SRMC on tank additions since the last ECP sampling indicates that a total of about 4,062 gallons of water was added to Tank 43H. This addition could account for the observed relatively small dilution of ~ 10% in the Tank 43H surface sample. Similar solution compositions measured in the current Tank 43H surface and subsurface samples indicate a minimal stratification within the tank.

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Nonparametric Multiparticle Set Methods for Interpreting Environmental Samples

Collection and analysis of environmental samples is commonly used by a range of stakeholders in nuclear safeguards and security contexts. While the ubiquity of samples and their transport in the environment allow regular collection, developing and demonstrating methods for analyzing these samples is difficult. In this work, an environmental sample consists of a set of one or more individual particles. Recent advances in reactor simulation have allowed us to generate data that are more representative of real-world environmental samples, enabling statistically defensible method development and testing. The most notable of these advances is a drastic increase in the number of material depletion regions, which allows our simulations to capture the variation in isotopic composition seen at length scales consistent with environmental samples. Traditional approaches for handling multiparticle samples treat each particle in the sample individually, estimating the quantity of interest (e.g., core-average burnup) resulting from measurement and analysis of signatures (e.g., nuclide assays) from each individual particle. Individual estimates are then averaged to generate a single estimate of the quantity of interest over the entire sample. In this presentation, we introduce two novel approaches for interpreting environmental samples that comprise of multiple particles: (1) the Quantile-Quantile Comparator, which uses a multivariate generalization of quantile-quantile plots for comparing unknown statistical distributions, and (2) the Set Transformer, an attention-based neural network module designed to model interactions among elements (particles) in the input set (sample). Statistically representative sampling cannot be guaranteed as samples are passively collected and are beholden to what particles are available in the environment. These new analysis methods for set-input problems are expected to be more robust than traditional approaches to issues of sampling bias where particles are not uniformly distributed throughout regions of interest, as well as generally outperform traditional approaches by jointly considering all elements in the set. We will present results comparing the performance of traditional single particle approaches and the novel Quantile-Quantile Comparator and Set Transformer for interpretation of simulated environmental samples.

Phathanapirom, Birdy↗

Sampling Density in Regional Exploration and Environmental Geochemical Studies: A Review

A variety of factors contribute to the proper and efficient evaluation of geochemical programs including sampling medium, sample size and sample fraction, sampling density, digestion procedure, and analytical techniques. Among the aforementioned factors, sampling density is of great importance, affecting project ability to detect anomalous sites, which are either economically viable or environmentally hazardous. It is quite critical to have a sufficient number of samples to delineate geochemical anomalies or baselines and to reveal the relative variations in elemental concentrations in a study area. The resolution of the subsequent maps obtained by sampling greatly depends on sampling density. While a large number of samples may generate redundant data, a small number of samples smooth out the patterns and may completely miss anomalies. This review provides a platform for applied geochemists who desire to design a sampling scheme for a regional geochemical program and do not have the financial resources to perform an orientation survey, which will give them the necessary information for designing, according to project objectives, a cost-effective regional geochemical survey for their study area. It is advisable to integrate during the desktop study all available information, such as geological, structural, geophysical, remote sensing data and topographical data by using different data fusion algorithms to arrive at a sampling density fit-for-purpose of the target area. This in turn facilitates an effective spatial positioning of sample locations. Quantitative analyses of the efficiency of different sampling densities for delineating geochemical patterns have not been well documented, warranting more attention and research.

58 GEOSCIENCES↗

Sensing and Sampling of Trace Contaminations by a Dexterous Hexrotor UAV at Nuclear Facilities - 18600

Safe and efficient cleanups are a priority for decontamination and decommissioning of nuclear facilities. The contaminations of byproducts and wastes in such nuclear facilities pose a serious problems while decommissioning, to both the operators and public. Sensing these contaminations and cleaning them is an essential part of the safety procedures. The contaminations might range from low-energy to high-energy byproducts. Sensing these byproducts would require contact based or non-contact based sensing, based on its energy levels. Byproducts such as americium, are low-energy which makes it difficult to sense and sample without contact. Therefore, the workers need to physically swab the surfaces to collect the samples of these contaminations. These tasks pose a great danger for the safety of the human workers which includes the risk to reach greater heights, exposure to the radiation and sampling the entire building. A robotic solution is much more desirable in these cases, where the worker can safely handle the contaminations from a safe area. Use of robotic technologies inside these hazardous environments ensures the safety and enhances the performance. The more suitable robotic solution for reaching great heights and covering large areas of nuclear facilities, are aerial vehicles. Multi-rotor unmanned aerial vehicle (UAV) are chosen for their ability to hover at a position and also fly around in confined spaces. Quadrotors are a common choice of multi-rotor UAVs both research and industry because of its ease to fly and commercial availability. For the applications during the cleanups we need the UAV to not only hover and fly in confined spaces, but also interact with the physical world. Despite of quadrotor's advantages, they are not a best suit as they can't interact with the physical world. The tasks involving physical interactions would require the UAV to apply arbitrary forces and torques in all six degrees of freedom (DOF). As quadrotors are under-actuated and non-holonomic in motion, they cannot exert all the required forces. At Collaborative Robotics Lab, Purdue University, we developed a novel multi-rotor UAV solution, Dexterous Hexrotor, which can exert arbitrary forces and torques in all six DOF, independently and instantaneously. This enables the UAV platform to quickly respond to the external disturbances and precisely hold its position during the mission. The Dexterous Hexrotor serves as a robotic tool for the workers to perform sensing and sampling during the cleanups. Workers can operate Dexterous Hexrotor manually and/or semi-autonomously with human intervention. Manual control requires the worker to fly the Dexterous Hexrotor using a remote control. So the workers should possess knowledge on flying the UAV and to perform physical interaction. A semiautonomous Dexterous Hexrotor requires human input to some extent and requires very less knowledge of flying. The autonomy is designed to operate in flight mode and sampling mode. In flight mode, Dexterous Hexrotor takes off from a 'safe' area, reaches the desired altitude, and fly autonomously towards a sampling point. This sampling point is the target position specified on the 2D reference map. This mode also includes navigation towards the sampling point, avoiding the obstacles in the constrained environment. After reaching a stopping point, Dexterous Hexrotor waits for the human input for a target location to swab and collect samples. The Dexterous Hexrotor is now in sampling mode and waits for the human input. The human operator selects the swabbing location through the live streaming video from onboard camera. Through visual servoing, aided by the map, the UAV will move closer towards the target position. It then transitions to the impact control scheme to perform physical interaction with the wall and collects samples. Once the sample is collected, it autonomously returns back to the takeoff position in 'safe' area for the analysis by mass spectrometry. In this paper, we majorly focus on the physical interaction strategy and the required components which enables the autonomy. Decommissioning of nuclear facilities requires decontamination inside the entire buildings. Decontamination of nuclear facilities involves sensing and sampling the huge buildings, long shafts, etc. Sampling the entire facility is not possible due to the limitation in Dexterous Hexrotor's flight time. But this can be achieved by using a swarm of Dexterous Hexrotors to cover larger areas. The onboard robotic arm can be designed based on the applications such as cleaning, applying sealants, etc. The modularity of the design allows us to switch components as per the requirements of the task. These kind of robotic solutions functioning as tools for the workers, aims to make the work environment safer and playful. (authors)

42 ENGINEERING↗

Sampling and Analysis Plan for Investigation of Undeclared Nuclear Activities - 20104

The nuclear-centered energy policy in South Korea is moving towards a nuclear-free era. It also facilitates an action or progress on the denuclearization of the Korean peninsula. The Nuclear Safety and Security Commission (NSSC) launched a new R and D project which attempts to verify nuclear activities via analyzing environmental samples. Environmental samples possibly contain significant radiological information relevant to past undeclared activities. In order to precisely verify them, it is essential to provide 1) the concrete information of target facilities, 2) appropriate methodologies and procedures, and 3) well-suited instrumentation and equipment corresponding to sample signatures. It is also important to provide scientific reliability or validity in any process such as sample collection, handling, transportation and laboratory analysis. Therefore, the information of nuclear facilities (fuel fabrication plant, graphite moderated reactor, reprocessing plant) in North Korea are reviewed in order to determine parameters for appropriate sampling methods representing a facility's characteristics. Secondly, a sampling procedure for radioactive elements is being developed based on international and domestic standards such as ASTM (American Society for Testing and Materials), KS (Korean industrial Standards), and International Atomic Energy Agency (IAEA) manuals. The procedure contains some specific information including sampling process, sampling tools, amount of sample, sample identification, and other related information. Developing the qualified national guidelines is most important since sampling and analyzing results can be used as evidences of nuclear activities. The guideline developed through this work will clearly define various methodologies such as document verification, sampling procedures, collection methods, sample storage criteria, chain of custody, and transportation conditions. The final objective of this work is to establish the infrastructure and regulatory framework for assessment of nuclear activities, and provide a national guideline for sampling and analysis. This will bring confidence in the results and play a critical role in complete denuclearization progress in South Korea. (authors)

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Applications of Hyporheic Zone Sampling for Assessing VOC Plume Engineered Remediation and Natural Attenuation Effectiveness - 20414

Determining the efficacy of engineered remedial actions and/or natural attenuation as an acceptable EPA Record of Decision (ROD) must address long-term temporal and spatial variability. Since final plume downslope destinations are aquifers and related surface streams and rivers, hyporheic zone sampling is essential. Comprehensive hyporheic sampling documents plume groundwater remediation prior to upwelling into stream benthic strata and natural attenuation within this dynamic zone itself. Our intensive sampling of the Savannah River Site (SRS) Chemical, Metals, and Pesticides (CMP) Pits VOC plume-fringe from 2005 to 2018 documented PCE natural attenuation and effectiveness of In Situ Thermal Treatment (ISTT). Most plume hyporheic upwelling was delimited to a 20 m inflow reach along Pen Branch. Our study utilized corroborative sampling methodologies: ambient hole-water grab samples: passive diffusion bags (PDB); and hole-core sediment samples to confirm station to station spatial and temporal trends. VOC hot spot detections were confirmed from both groundwater and soil core samples. VOC pathways through the Pen Branch hyporheic zone were assessed at hole-installation using sequential soil samples from augered cores and grab-samples of hole-bottom water. Longer term, composite water samples were collected from PDBs deployed for a minimum two-week equilibration period. Soil samples were collected from the 15 and 65 cm core levels in December 2017 and June 2018 at six stations. Additional core depths of 40 and 85 cm were sampled in June 2018 at the highest VOC station (5DB80). All samples were analyzed in an EPA certified lab by purge and trap GC-MS. Effectiveness of previous ISTT and soil vapor extraction (SVE) for this CMP Pits PCE plume, was clearly documented by significant downward trends in VOC at hyporheic zone stations prior to December 2015. Achieving final stage conversions of PCE daughter products to ethene and CO{sub 2} may be limited depending upon suitable interactions between hyporheic zone sediment morphology, hydrology, and redox conditions. Because declines in VOC daughter products at our hyporheic stations may also be caused by physical actions of dilution and dispersion rather than true biochemical dechlorination, full quantification of natural attenuation requires the use of compound-specific isotope ratio analysis (CSIA) and microbial 16S rRNA with qPCR. To assist these next-phase efforts, a natural attenuation index (NAI) was used to help produce quicker, more cost-effective decision making for locating CSIA and microbial sampling efforts. The NAI used natural logarithm transformed GC-MS results for station VOC degradation compounds versus VOC parent compounds. Wide differences were observed between stations. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Analysis of the 2H-evaporator scale samples (HTF-17-56, -57)

Savannah River National Laboratory analyzed scale samples from both the wall and cone sections of the 242-16H Evaporator prior to chemical cleaning. The samples were analyzed for uranium and plutonium isotopes required for a Nuclear Criticality Safety Assessment of the scale removal process. The analysis of the scale samples found the material to contain crystalline nitrated cancrinite and clarkeite. Samples from both the wall and cone contain depleted uranium. Uranium concentrations of 16.8 wt% 4.76 wt% were measured in the wall and cone samples, respectively. The ratio of plutonium isotopes in both samples is ~85% Pu-239 and ~15% Pu-238 by mass and shows approximately the same 3.5 times higher concentration in the wall sample versus the cone sample as observed in the uranium concentrations. The mercury concentrations measured in the scale samples were higher than previously reported values. The wall sample contains 19.4 wt% mercury and the cone scale sample 11.4 wt% mercury. The results from the current scales samples show reasonable agreement with previous 242-16H Evaporator scale sample analysis; however, the uranium concentration in the current wall sample is substantially higher than previous measurements.

2H evaporator system↗