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DOE OSTI2021

X-ray diffraction and scanning electron microscope characterizations of the salt waste processing facility tank 101 and tank 104 solid samples

The “as-received” Salt Waste Processing Facility (SWPF) Tank 101 and two Tank 104 samples (pre-wash and washed solids) have been characterized using x-ray diffraction (XRD) and scanning electron microscope/energy dispersive x-ray (SEM/EDX) techniques to address the concerns for the existence of solids, which may interfere with the operational performance of the SWPF crossflow filtration process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Tank Waste Characterization: History, Challenges, and Success Stories

The preparation and chemical and radiochemical analysis of Hanford tank waste samples can be performed with standard laboratory equipment and instruments as relatively routine processes that are not particularly challenging. Rather, the main challenges of tank waste characterization are associated with radiological dose and sampling limitations. Accurate, representative and effective sampling techniques are difficult with the waste tanks because they were not designed for routine sampling. There are a finite number of sampling locations for each tank based on riser positioning, depth and the operational functionality of the sampling riser. For example, in one recently emptied SST, there was one riser that was found to have had concrete dumped down it, thereby eliminating that sampling port. Additionally, the waste within the tank; especially true for the saltcake and sludge, is not homogenous. The ability to adequately mix a million-gallon double shell tank (DST) is a concern for data reproducibility. Another real challenge that must be addressed for sampling single shell tanks, is how to dissolve the salt cake waste in a compromised (leaking) SST. These physical constraints mean that uncertainty in the representativeness of samples must be considered when applying analytical results to the bulk contents of the tank. The tank waste is highly radioactive and thus can only be handled initially by facilities that can receive samples into concrete-shielded hot cells with remote operation with an example provided in Figure 1. The shielding protects the worker from the radiological dose while mineral oil windows and remotely operated manipulators enables the samples to be handled. At Hanford, analytical laboratories with these hot cell capabilities are limited to the Pacific Northwest National Laboratory and the main Hanford operations support laboratory, 222-S Laboratory. Because of their highly radioactive nature, samples must be sufficiently diluted to facilitate their analysis outside of a shielded cell. In some cases, this means some accuracy must be compromised to complete the analysis beyond that normally encountered for non-radioactive material.

Waste Characterization, BBI, PHOENIX: Tank Farms: ↗

DOE OSTI2019

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↗

DOE OSTI2017

Chemical, biological, and DNA markers for tracing slaughterhouse effluent

Agricultural practices, if not managed correctly, can have a negative impact on receiving environments via waste disposal and discharge. In this study, a chicken slaughter facility on the rural outskirts of Sydney, Australia, has been identified as a possible source of persistent effluent discharge into a peri-urban catchment. Questions surrounding the facility's environmental management practices go back more than four decades. Despite there having never been a definitive determination of the facility's impact on local stream water quality, the New South Wales Environment Protection Authority (NSW EPA) has implemented numerous pollution reduction requirements to manage noise and water pollution at the slaughter facility. However, assessment of compliance remains complicated by potential additional sources of pollution in the catchment. To unravel this long-standing conundrum related to water pollution we apply a forensic, multiple lines of evidence approach to delineate the origin of the likely pollution source(s). Water samples collected between 2014 and 2016 from irrigation pipes and a watercourse exiting the slaughter facility had elevated concentrations of ammonia (max: 63,000 µg/L), nitrogen (max: 67,000 µg/L) and phosphorus (max: 39,000 µg/L), which were significantly higher than samples from adjacent streams that did not receive direct runoff from the facility. Arsenic, sometimes utilised in growth promoting compounds, was detected in water discharging from the facility up to ~4 times (max 3.84 µg/L) local background values (<0.5 µg/L), with inorganic As{sup (∑V+III)} being the dominant species. The spatial association of elevated water pollution to the facility could not unequivocally distinguish a source and consequently DNA analysis of a suspected pollution discharge event was undertaken. Analysis of catchment runoff from several local streams showed that only water sampled at the downstream boundary of the facility tested positive for chicken DNA, with traces of duck DNA being absent, which was a potential confounder given that wild ducks are present in the area. Further, PCR analysis showed that only the discharge water emanating from the slaughter facility tested positive for a generalized marker of anthropogenic pollution, the clinical class 1 integron-integrase gene. The environmental data collected over a three-year period demonstrates that the slaughter facility is indisputably the primary source of water-borne pollution in the catchment. Moreover, application of DNA and PCR for confirming pollution sources demonstrates its potential for application by regulators in fingerprinting pollution sources. - Highlights: • Multiple lines of evidence approach to delineate the origin of water pollution. • Arsenic speciation and clinical class 1 integron-integrase gene used as indicators. • Multidisciplinary approach for addressing global concerns about agricultural waste.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2018

LLNL Evaluation of 44th OPCW Environmental Proficiency Test

The goal of the test was to analyze all samples for the presence of any Scheduled Chemicals and/or their precursors/degradation/reaction products and chemicals listed in the list of “Additional Non-Scheduled Reportable Chemicals”. According to the test scenario, the samples were collected from a facility described as an industrial research laboratory for developing new chemical compounds. Each participating laboratory received a set of three aqueous samples (described as “Decon Waste”) and a set of three soil samples (described as collected in an area of suspected chemical contamination, near a chemical storage facility). Each set of samples contained one “test sample”, one “control sample”, and one “blank sample” without indication of their identities. The test sample contained an unknown number of spiking chemicals, each present at a concentration of 1 ppm or greater. The control sample contained an unknown number of spiking chemicals, each present at a concentration of 5 ppm or greater. The blank sample contained no chemicals relevant to the aim of the test. However, for this test, the blank samples did contain irrelevant chemicals in addition to the sample matrix.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Soil Sample Workplan in Support of the Site 300 Explosives Waste Treatment Facility Ecological Risk Assessment Pursuant to the Hazardous Waste Facility Permit (Part V, Special Condition #14 a-f)

The Department of Toxic Substances Control issued the Final Hazardous Waste Facility Permit to Lawrence Livermore National Laboratory, Site 300 in 2017. As part of the continual process to ensure waste treatment emissions are not impacting ecological receptors, LLNL analyzed soil samples in the vicinity of the Explosive Waste Treatment Facility (EWTF) Burn Units (i.e., Burn Cage and Burn Pan) and the Detonation Pad. Soil samples were analyzed by EPA Solid Waste 846 Methods for furans, explosives, metals, and semi-volatile compounds. In all samples, furans, explosives, and semi-volatile organic compounds were not detected. Metals were detected at concentrations below background levels. This soil sample plan will sample the same four downwind areas of the Burn Units and the same downwind areas of the Detonation, as well as including four new sample locations. The four new locations will be located to the northeast and southwest of the Burn Units and Detonation (as shown in Figure 3). The constituents to be analyzed are in Tables 7 and 8. Perchlorate was not identified as a constituent of concern in the 2007 Soil Sampling Plan. However, for this plan, all soil samples will be analyzed for perchlorate. Nitrate and all CAM17 metals have been added to the sampling plan to comply with DTSC comments received in correspondence dated June 4, 2021. After completion of the sampling event, a soil sample report will be submitted to DTSC in accordance with requirements specified in the Hazardous Waste Facility Permit, Part V, Special Conditions 16 a-f. This proposed soil sampling plan will be fully implemented no later than one year after receiving DTSC approval, in accordance with the Hazardous Waste Facility Permit, Part V, Special Condition 15.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2024

Analytical Results of the Tank 51H Sludge Batch 11 As-Received Qualification Sample

Savannah River National Laboratory (SRNL) has been requested by Savannah River Mission Completion (SRMC) to qualify the next sludge batch, Sludge Batch 11 (SB11), for processing at the Defense Waste Processing Facility (DWPF). This report documents the first steps of the qualification process, characterization of the Tank 51H as-received qualification material. SRMC sent SRNL two 200 mL samples received from Tank 51H on the 12th of August 2024. The combined sample, HTF-51-24-85/86, was analyzed for the following: supernate and slurry density, weight percent solids, settling, chemical composition, and radionuclides.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Determination of Reportable Radionuclides for Defense Waste Processing Facility (DWPF) Sludge Batch 9 (Macrobatch 11)

This report documents analyses and calculations performed by the Savannah River National Laboratory (SRNL) of Tank 40 sludge as part of the Waste Acceptance Product Specifications (WAPS) requirements for Sludge Batch 9 (SB9) for the Defense Waste Processing Facility (DWPF). Tank Farm sample HTF-40-17-5 was received by SRNL Shielded Cells Operations (SCO) and was prepared for radionuclide analyses in addition to various other physical and chemical characterizations. Radionuclide analyses were performed by SRNL Analytical Development (AD). Based on criteria set forth in the Department of Energy (DOE) WAPS and DWPF’s Waste Form Compliance Plan (WCP), as well as, historical lessons from previous sludge batch analyses, a list of radionuclides was developed for which the sample was analyzed. The results of these analyses were then used as input into commercially available software, RadDecay version (v) 5.01. The software was used to calculate the activity of the measured analytes in index years 2017 through 3115 in 100-year increments. Radionuclides with half-lives greater than 10 years and activities that comprised more than 0.01% of the total sludge batch activity are reportable.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Identification and Shipment Progress of the INL and LANL Samples to Be Received at ORNL

Ferritic-martensitic steel Grade 92, with T91 as a reference, together with austenitic stainless steel (or Incoloy Alloy) 800H and its grain-boundary-engineered version 800H-TMP (ThermoMechanical 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 of Idaho National Laboratory (INL), with the rest in the High Flux Isotope Reactor 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 samples, most of the ORNL samples, and part of the LANL (Los Alamos National Laboratory) samples from the ATR, BOR-60 and Phénix reactors have been received at the Irradiated Materials Examination and Testing (IMET) hot cell facility and Low Activation Materials Design and Analysis (LAMDA) laboratory of ORNL. Post-irradiation examination of the received samples is in progress at ORNL. The effects of irradiation temperature, dose, reactor (e.g., dose rate, neutron-spectrum-induced difference in transmutation), TMP, and heats variation on the microstructures and mechanical properties of the samples will be evaluated.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Soil Sample Plan in Support of the Site 300 Explosives Waste Treatment Facility Ecological Risk Assessment Pursuant to the Hazardous Waste Facility Permit, Part V, Special Condition #14 a-f. August 2020

The Department of Toxic Substances Control issued the Final Hazardous Waste Facility Permit to Lawrence Livermore National Laboratory, Site 300 in 2017. As part of the continual process to ensure waste treatment emissions are not impacting ecological receptors, LLNL analyzed soil samples in the vicinity of the Explosive Waste Treatment Facility (EWTF) Burn Units (i.e., Burn Cage and Burn Pan) and the Detonation Pad. Soil samples were analyzed by EPA Solid Waste 846 Methods for furans, explosives, metals, and semivolatile compounds. In all samples, furans, explosives, and semi-volatile organic compounds were not detected. Metals were detected at concentrations below background levels. This soil sample plan will sample the same four downwind areas of the Burn Units and the same downwind areas of the Detonation, as well as including four new sample locations. The four new locations will be located to the northeast and southwest of the Burn Units and Detonation (as shown in Figure 3). The constituents to be analyzed are in Tables 2 and 3. Perchlorate was not identified as a constituent of concern in the 2007 Soil Sampling Plan. However, for this plan, all soil samples will be analyzed for perchlorate. After completion of the sampling event, a soil sample report will be submitted to DTSC in accordance with requirements specified in the Hazardous Waste Facility Permit, Part V, Special Conditions 16 a-f. This proposed soil sampling plan will be fully implemented no later than one year after receiving DTSC approval, in accordance with the Hazardous Waste Facility Permit, Part V, Special Condition 15.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2021

Optimizing a magnitude-limited spectroscopic training sample for photometric classification of supernovae

ABSTRACT In preparation for photometric classification of transients from the Legacy Survey of Space and Time (LSST) we run tests with different training data sets. Using estimates of the depth to which the 4-m Multi-Object Spectroscopic Telescope (4MOST) Time Domain Extragalactic Survey (TiDES) can classify transients, we simulate a magnitude-limited sample reaching rAB ≈ 22.5 mag. We run our simulations with the software snmachine, a photometric classification pipeline using machine learning. The machine-learning algorithms struggle to classify supernovae when the training sample is magnitude limited, in contrast to representative training samples. Classification performance noticeably improves when we combine the magnitude-limited training sample with a simulated realistic sample of faint high-redshift supernovae observed from larger spectroscopic facilities; the algorithms’ range of average area under receiver operator characteristic curve (AUC) scores over 10 runs increases from 0.547–0.628 to 0.946–0.969 and purity of the classified sample reaches 95 per cent in all runs for two of the four algorithms. By creating new, artificial light curves using the augmentation software avocado, we achieve a purity in our classified sample of 95 per cent in all 10 runs performed for all machine-learning algorithms considered. We also reach a highest average AUC score of 0.986 with the artificial neural network algorithm. Having ‘true’ faint supernovae to complement our magnitude-limited sample is a crucial requirement in optimization of a 4MOST spectroscopic sample. However, our results are a proof of concept that augmentation is also necessary to achieve the best classification results.

79 ASTRONOMY AND ASTROPHYSICS↗

DOE OSTI2021

Analysis of Defense Waste Processing Facility Sample: Recycle Collection Tank Sample Batch 4945

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (now Savannah River Mission Completion (SRMC)), through a Technical Task Request, to characterization the “as-received” Recycle Collection Tank (RCT) Sample identified as sample batch 4945 [Sludge Receipt and Adjustment Tank (SRAT) batch 796)], which was delivered to SRNL Shielded Cells on January 28, 2021. The RCT characterization data will be used as input to the Defense Waste Processing Facility (DWPF) Recycle Diversion Project. This RCT report is the first of three sample characterization reports that will be used for this DWPF Project. The other DWPF reports will involve the characterization of the Off-Gas Condensate Tank (OGCT) and the Slurry Mix Evaporator Condensate Tank (SMECT) samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Recycle Collection Tank Sample Batch 4945

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

A new capability facilitating nuclear materials research: the Activated Materials Laboratory at the Advanced Photon Source

The Activated Materials Laboratory (AML), located in the Long Beamline Building (LBB) of the Advanced Photon Source (APS) of Argonne National Laboratory (ANL), serves as a centralized radiological facility for preparing radioactive samples for APS beamline experiments. The AML is equipped to receive shipments, handle open-form radioactive materials, encapsulate samples, and transport samples to-and-from beamline end-stations. The AML works closely with users and the APS radiological safety committee to make sure the safe conduct of experiments.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Slurry Mix Evaporator Condensate Tank Sample Batch 4638

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR, now Savannah River Mission Completion (SRMC)), through a Technical Task Request, to characterization the “as-received” Slurry Mix Evaporator Condensate Tank (SMECT) sample identified as sample batch 4638, which was delivered to SRNL Shielded Cells on March 19, 2021. The SMECT characterization data will be used as input to the Defense Waste Processing Facility (DWPF) Recycle Diversion Project. This SMECT report is the second of three sample characterization reports that will be used for this DWPF Project. The other two DWPF characterization reports involve the characterization of the Recycle Collection Tank (RCT) sample and the future Off-Gas Condensate Tank (OGCT) characterization report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Analysis of Defense Waste Processing Facility Sample: Off-Gas Condensate Tank Sample Batch 27862

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (now Savannah River Mission Completion (SRMC)), through a Technical Task Request (X-TTR-H-00107), to characterize the “as-received” Off-Gas Condensate Tank (OGCT) Sample identified as sample batch 27862, which was delivered to SRNL Shielded Cells on April 30, 2021. This OGCT report is the third of three sample characterization reports dealing with this Defense Waste Processing Facility (DWPF) Recycle Diversion Project. The other two recycling stream characterization reports are the Recycle Collection Tank (RCT) and the Slurry Mix Evaporator Condensate Tank (SMECT) sample report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Micro to nanostructural observations in neutron irradiated nuclear graphites PCEA and PCIB

Here, the neutron irradiation induced structural changes in nuclear grade graphites PCEA and PCIB were investigated using scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectroscopy, transmission electron microscopy (TEM), selected area electron diffraction (SAED) and electron energy loss spectroscopy (EELS). The graphite samples were irradiated at the Advanced Test Reactor National User Facility at the Idaho National Laboratory. Received doses ranged from 1.5 dpa - 6.8 dpa and irradiation temperatures varied between 350°C - 670°C. XRD data showed crystallite sizes to reduce by 35% (for both La and Lc) for low dose, low temperature specimens and by 50% (for both La and Lc) for high dose, high temperature specimens (compared to unirradiated specimens of the same grade). Analysis of the G peak in Raman spectra of irradiated specimens provided evidence for the fragmentation of crystallites following neutron irradiation. Conventional TEM and SAED were used to observe the structure of lattice fringes and measure the spacing of planes. Image analysis software was applied to TEM images to quantify fringe length, tortuosity, and relative orientation of planes. Neutron irradiation appeared to induce basal plane fragmentation and curvature. EELS was performed to study the proportion of sp2 bonding and specimen density. The high dose high temperature specimens showed evidence of structural recovery where sp2 values are slightly higher than values associated with low dose low temperature specimens. Data from XRD, Raman, TEM, SAED and EELS showed that low dose low temperature specimens tended to exhibit higher structural damage (such as lower sp2 content, higher d-spacing, and reduced crystallite size) than high dose high temperature specimens.

36 MATERIALS SCIENCE↗

DOE OSTI2024

MODELING AND METHOD FOR OPTICAL PERFORMANCE OF A RECEIVER COATING AND ITS DEGRADATION DUE TO OPERATION

The optical properties of the coating used on a concentrated solar power (CSP)’s receiver directly impact the performance of the power plant. Receiver coatings are designed to absorb as much heat as possible and transfer it to the circulating fluid. Over time, the absorptivity of the receiver coating degrades due to environmental and operational conditions. This project aims to (1) create a test apparatus that allows coatings to undergo accelerated lifetime testing under conditions that mimic what the coating will experience on-tower; and (2) develop a mathematical model that based on the test data predicts absorptivity over time. To create the mathematical model, samples of BrightSource Energy’s Gen1 and Gen2 coatings were tested first looking at individual failure modes (such as high temperature cycling) and then for combined failure modes in the newly developed apparatus. In addition to taking optical measurements, the samples were destroyed to allow for metalogical evaluation to understand what was happening on a microscopic level. Pre-existing models from the literature that describe accelerated testing as well as individual phenomena observed in the coating were then combined to create the model. Additionally, the Gen2 and Gen3 coatings are being testing at the Plataforma Solar de Almería (PSA) facility in Almeria, Spain to confirm that the apparatus test results are similar to those received on-sun. (PSA’s facility closely mimics on-tower conditions). The goal is to enable industry players to test coatings using the new apparatus, gather absorptivity measurements (without needing to destroy samples), and input the information into the model to determine how the coating will perform over time, thus allowing the optical performance of coatings to be compared even before they are used on-tower. The model will be publicly available by the end of the project (currently projected as December 2024).

14 SOLAR ENERGY↗