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At least 235 records · Page 13

Data Compilation for AGC-2 Matrix-only Compact Lot A3-H08

This document is a compilation of fabrication and characterization data for the compact lot A3-H08, which was produced for possible insertion into the second ATR Graphite Creep irradiation test capsule (AGC-2). The compacts were produced by Oak Ridge National Laboratory (ORNL) for the Advanced Gas Reactor Fuel Development and Qualification (AGR) program. This compact lot was fabricated using a graphite/resin blend formulated by INL as a candidate matrix precursor for scale-up of overcoating and compacting processes. The matrix precursor powder for compact lot A3-H08 was a jet milled blend of 64 wt% natural graphite (Asbury 3482), 16 wt% synthetic graphite (Graftech GTI-D), and 20 wt% high purity novolac resin (Hexion D_SD-1708 with 7.5% hexamethylenetetramine added). The “Matrix Compacts for AGC-2 Irradiation” Specification (INL SPC-1285, Rev. 1) provides the requirements necessary for acceptance of the compacts. Sections 2.03 and 2.04 of SPC-1285 provide the property requirements for the heat-treated compacts. There are requirements on the length, diameter, and matrix density. Section 2.02.01.01 further requests impurity analysis on representative samples from the final compact lot, but there are no specified acceptance criteria. The impurity information will be evaluated by INL as part of a final decision on whether to insert the compacts into the AGC-2 experiment. The procedures for characterizing and qualifying the compacts are outlined in ORNL product inspection plan AGR-CHAR-PIP-16. The measurement of compact length, diameter, and matrix density was performed according to data acquisition method AGR-CHAR-DAM-39. The data report forms generated by this procedure document the product acceptance for the property requirements listed in sections 2.03 and 2.04 of SPC-1285. All compacts selected for irradiation conformed to the specified requirements for length, diameter, and density. In addition to the characterization data, this report also contains other records relevant to the product acceptance. A history of the material flow and sample naming is included and the compacting process is summarized. In addition to results of the impurity analysis on representative samples from the final compact lot, impurity analysis results are also provided for samples of the graphite, resin, and the graphite/resin blend. A Certificate of Conformance to SPC-1285, Rev. 1 is attached in Appendix B.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Performance Demonstration Program Plan for RCRA Constituent Analysis of Solidified Wastes (Rev 8)

The Performance Demonstration Program (PDP) for Resource Conservation and Recovery Act (RCRA) constituents distributes test samples for analysis of volatile organic compounds (VOCs), semivolatile organic compounds (SVOCs), and metals in solid matrices. Each distribution of test samples is termed a PDP cycle. These evaluation cycles provide an objective measure of the reliability of measurements performed for transuranic (TRU) waste characterization. The primary documents governing the conduct of the PDP are the Quality Assurance Program Document (QAPD; DOE/CBFO-94-1012) and the Waste Isolation Pilot Plant (WIPP) Waste Analysis Plan (WAP) contained in the Hazardous Waste Facility Permit (NM4890139088-TSDF) issued by the New Mexico Environment Department. The WAP requires participation in the PDP; the PDP must comply with the QAPD and the WAP. This plan implements the general requirements of the QAPD and the applicable requirements of the WAP for the RCRA PDP. Participating laboratories demonstrate acceptable performance by successfully analyzing single- blind performance evaluation samples (subsequently referred to as PDP samples) according to the criteria established in this plan. PDP samples are used as an independent means to assess laboratory performance regarding compliance with the WAP quality assurance objectives (QAOs). The concentrations of analytes in the PDP samples address levels of regulatory concern and encompass the range of concentrations anticipated in waste characterization samples. The WIPP requires analyses of homogeneous solid wastes to demonstrate compliance with regulatory requirements. These analyses must be performed by laboratories that demonstrate acceptable performance in this PDP. These analyses are referred to as WIPP analyses, and the samples on which they are performed are referred to as WIPP samples. Participating laboratories must analyze PDP samples using the same procedures used for WIPP samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Dataset 1: A National and City Dataset on Human Factors in Pooled Rideshare, 2021

Dataset 1: A National and City Dataset on Human Factors in Pooled Rideshare, 2021. Dataset Description: Pooled Rideshare Acceptance Survey - Phase 1 (2021, N = 5,385). This dataset captures responses from a nationally representative sample of 5,385 adults across the United States to understand public acceptance, preferences, and behavioral intentions related to pooled rideshare (PR) services. The primary objective of this research is to provide actionable insights to inform the design, deployment, and policy development of sustainable shared mobility systems. Data was collected via an online survey administered through a national panel provider. Participants ranged in age from 18 to 95 years, and representation from all U.S. regions. The survey instrument was designed to explore numerous dimensions related to PR adoption including demographic traits, current travel habits, rideshare familiarity, trust, safety, environmental attitudes, and user experience preferences. Both rideshare users and non-users were included, offering a diverse range of perspectives. - Phase_1_Final - The dataset includes survey items developed from literature reviews, and prior field studies. Each row represents an individual respondent, and each column corresponds to a variable such as willingness to use pooled rideshare, attitudes toward specific service features, and sociodemographic data. The data is available in both .CSV and .SAV formats. - Phase_1_Final_MapFile - The accompanying data dictionary explains all variable labels, response scales, and codes. An .XLSX format of the full survey instrument is also included to support interpretation and reuse of the dataset.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

ISS External Microorganisms: A Planetary Protection Experiment to Inform Requirements for Crewed Missions to Mars

We have developed, tested, and flown a caddy capable of collecting aseptic samples from external surfaces of the ISS (International Space Station). The sampling caddy is certified for use during US EVA (extra vehicular activity) and was launched to ISS in the summer of 2023. We are scheduled to collect samples from 6 locations outside ISS during an EVA in May of 2024. We will freeze these samples at -80°C on orbit and return them to Earth. We will then extract and sequence any DNA collected during the EVA using next generation sequencing technologies to characterize the community composition and function of each sample. Measuring the type and quantity of microbes present on the exterior of ISS will allow us to address knowledge gap 2B, “Acceptable levels of microbial/organic releases from humans and support systems” described in a 2019 COSPAR report. Collecting data about microbial release from current crewed vehicles will inform requirements for acceptable leak rates for future crewed missions to Mars. The sampling kit consists of eight commercially available, sterile, DNA free, macrofoam swabs ( 23 mm. diameter ) installed in custom aluminum end effectors. Each end effector is housed in and individual aluminum canister. Each canister contains a 0.2 μm Teflon filter to allow the interior volume to accommodate pressure changes without permitting microbial contaminants to enter the sterile interior volume. A handle repurposed from the space shuttle tile repair kit is used to remove the end effector from the sample canister, collect a sample by swabbing a surface and then replace the end effector in its canister. The canisters and end effectors were cleaned and assembled on Earth. Prior to installing the sterile swab the canisters and end effectors were sterilized in an autoclave at 134°C, 215 kPA, for 7 min.. The final assembly occurred in a sterilized class II biosafety cabinet. We will collect six samples from the 1) airlock vestibule, 2) airlock thermal cover, 3) a gap in the micrometeorite shielding near the airlock, 4) a handrail near the airlock, 5) the CDRA (Carbon Dioxide Removal Assembly) vent, and 6) the VES (Vacuum Exhaust System) vent. The remaining two swabs will be reserved as controls. One swab will be exposed during the EVA without touching any surfaces to act as a blank. The final swab will remain sealed until the entire sampling kit is returned to earth. Based on previously published results from the Russian segment, we hypothesize that there will be detectable microbes at some or all of these locations. Ground-based testing of this sampling caddy confirms that the swabs remain sterile as the canisters transition in and out of vacuum. We were able to retrieve, viable bacterial and fungal cells as well as DNA from samples collected from US space suits during vacuum chamber tests lasting as long as seven hours. Based on these results and feedback from the test subjects the sampling caddy was modified to improve ergonomics and meet US EVA safety requirements. Bayonet probes were added to the sides of the sample kit as alternate mounting points. Additional locking features were added to the end effector and the filter stack to prevent inadvertent release during use. The opening mechanism was changed from one where the end effector was rocked laterally to defeat a ball detent to a twist-to-open threaded closure for similar reasons. Demonstrating, this sampling caddy’s effectiveness during a US EVA will allow us to address knowledge gaps identified in COSPAR reports and begin to define planetary protection requirements for life support systems on crewed missions to mars. This kit could also be used to collect contamination control samples during Artemis missions to verify requirements and could be easily modified for robotic sample collection.

Planetary Protection↗

ISS External Microorganisms: Collecting Planetary Protection Samples During Extravehicular Activity

We have developed, tested, and flown a caddy capable of collecting aseptic samples from external surfaces of the ISS (International Space Station). The sampling caddy is certified for use during US EVA (extra vehicular activity) and was launched to ISS in the summer of 2023. We are scheduled to collect samples from 6 locations outside ISS during an EVA in May of 2024. We will freeze these samples at -80°C on orbit and return them to Earth. We will then extract and sequence any DNA collected during the EVA using next generation sequencing technologies to characterize the community composition and function of each sample. Measuring the type and quantity of microbes present on the exterior of ISS will allow us to address knowledge gap 2B, “Acceptable levels of microbial/organic releases from humans and support systems” described in a 2019 COSPAR report. Collecting data about microbial release from current crewed vehicles will inform requirements for acceptable leak rates for future crewed missions to Mars. The sampling kit consists of eight commercially available, sterile, DNA free, macrofoam swabs ( 23 mm. diameter ) installed in custom aluminum end effectors. Each end effector is housed in and individual aluminum canister. Each canister contains a 0.2 μm Teflon filter to allow the interior volume to accommodate pressure changes without permitting microbial contaminants to enter the sterile interior volume. A handle repurposed from the space shuttle tile repair kit is used to remove the end effector from the sample canister, collect a sample by swabbing a surface and then replace the end effector in its canister. The canisters and end effectors were cleaned and assembled on Earth. Prior to installing the sterile swab the canisters and end effectors were sterilized in an autoclave at 134°C, 215 kPA, for 7 min.. The final assembly occurred in a sterilized class II biosafety cabinet. We will collect six samples from the 1) airlock vestibule, 2) airlock thermal cover, 3) a gap in the micrometeorite shielding near the airlock, 4) a handrail near the airlock, 5) the CDRA (Carbon Dioxide Removal Assembly) vent, and 6) the VES (Vacuum Exhaust System) vent. The remaining two swabs will be reserved as controls. One swab will be exposed during the EVA without touching any surfaces to act as a blank. The final swab will remain sealed until the entire sampling kit is returned to earth. Based on previously published results from the Russian segment, we hypothesize that there will be detectable microbes at some or all of these locations. Ground-based testing of this sampling caddy confirms that the swabs remain sterile as the canisters transition in and out of vacuum. We were able to retrieve, viable bacterial and fungal cells as well as DNA from samples collected from US space suits during vacuum chamber tests lasting as long as seven hours. Based on these results and feedback from the test subjects the sampling caddy was modified to improve ergonomics and meet US EVA safety requirements. Bayonet probes were added to the sides of the sample kit as alternate mounting points. Additional locking features were added to the end effector and the filter stack to prevent inadvertent release during use. The opening mechanism was changed from one where the end effector was rocked laterally to defeat a ball detent to a twist-to-open threaded closure for similar reasons. Demonstrating, this sampling caddy’s effectiveness during a US EVA will allow us to address knowledge gaps identified in COSPAR reports and begin to define planetary protection requirements for life support systems on crewed missions to mars. This kit could also be used to collect contamination control samples during Artemis missions to verify requirements and could be easily modified for robotic sample collection.

Planetary Protection↗

Human Mars Surface Science Operations

Human missions to the surface of Mars will have challenging science operations. This paper will explore some of those challenges, based on science operations considerations as part of more general operational concepts being developed by NASA's Human Spaceflight Architecture (HAT) Mars Destination Operations Team (DOT). The HAT Mars DOT has been developing comprehensive surface operations concepts with an initial emphasis on a multi-phased mission that includes a 500-day surface stay. This paper will address crew science activities, operational details and potential architectural and system implications in the areas of (a) traverse planning and execution, (b) sample acquisition and sample handling, (c) in-situ science analysis, and (d) planetary protection. Three cross-cutting themes will also be explored in this paper: (a) contamination control, (b) low-latency telerobotic science, and (c) crew autonomy. The present traverses under consideration are based on the report, Planning for the Scientific Exploration of Mars by Humans1, by the Mars Exploration Planning and Analysis Group (MEPAG) Human Exploration of Mars-Science Analysis Group (HEM-SAG). The traverses are ambitious and the role of science in those traverses is a key component that will be discussed in this paper. The process of obtaining, handling, and analyzing samples will be an important part of ensuring acceptable science return. Meeting planetary protection protocols will be a key challenge and this paper will explore operational strategies and system designs to meet the challenges of planetary protection, particularly with respect to the exploration of "special regions." A significant challenge for Mars surface science operations with crew is preserving science sample integrity in what will likely be an uncertain environment. Crewed mission surface assets -- such as habitats, spacesuits, and pressurized rovers -- could be a significant source of contamination due to venting, out-gassing and cleanliness levels associated with crew presence. Low-latency telerobotic science operations has the potential to address a number of contamination control and planetary protection issues and will be explored in this paper. Crew autonomy is another key cross-cutting challenge regarding Mars surface science operations, because the communications delay between earth and Mars could as high as 20 minutes one way, likely requiring the crew to perform many science tasks without direct timely intervention from ground support on earth. Striking the operational balance between crew autonomy and earth support will be a key challenge that this paper will address.

Bobskill, Marianne R.↗

Global Threat Reduction Initiative Fuel Thermo-Physical Characterization Project: Sample Management Plan

This sample management plan provides guidelines for sectioning, preparation, acceptance criteria, analytical path, and end-of-life disposal for the fuel element segments utilized in the Global Threat Reduction Initiative (GTRI), Fuel Thermo-Physical Characterization Project. The Fuel Thermo-Physical Characterization Project is tasked with analysis of irradiated Low Enriched Uranium (LEU) Molybdenum (U-Mo) fuel element samples to support the GTRI conversion program. Sample analysis may include optical microscopy (OM), scanning electron microscopy (SEM) fuel-surface interface analysis, gas pycnometry (density) measurements, laser flash analysis (LFA), differential scanning calorimetry (DSC), thermogravimetry and differential thermal analysis with mass spectroscopy (TG /DTA-MS), Inductively Coupled Plasma Spectrophotometry (ICP), alpha spectroscopy, and Thermal Ionization Mass Spectroscopy (TIMS). The project will utilize existing Radiochemical Processing Laboratory (RPL) operating, technical, and administrative procedures for sample receipt, processing, and analyses. Test instructions (TIs), which are documents used to provide specific details regarding the implementation of an existing RPL approved technical or operational procedure, will also be used to communicate to staff project specific parameters requested by the Principal Investigator (PI). TIs will be developed, reviewed, and issued in accordance with the latest revision of the RPL-PLN-700, RPL Operations Plan. Additionally, the PI must approve all project test instructions and red-line changes to test instructions.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

Waveform processing using neural network algorithms on the front-end electronics

In a multi-channel radiation detector readout system, waveform sampling, digitization, and raw data transmission to the data acquisition system constitute a conventional processing chain. The deposited energy on the sensor is estimated by extracting peak amplitudes, area under pulse envelopes from the raw data, and starting times of signals or time of arrivals. However, such quantities can be estimated using machine learning algorithms on the front-end Application-Specific Integrated Circuits (ASICs), often termed as “edge computing”. Edge computation offers enormous benefits, especially when the analytical forms are not fully known or the registered waveform suffers from noise and imperfections of practical implementations. In this work, we aim to predict peak amplitude from a single waveform snippet whose rising and falling edges containing only 3 to 4 samples. We thoroughly studied two well-accepted neural network algorithms, Multi-Layer Perceptron (MLP) and Convolutional Neural Network (CNN) by varying their model sizes. Further, to better fit front-end electronics, neural network model reduction techniques, such as network pruning methods and variable-bit quantization approaches, were also studied. By combining pruning and quantization, our best performing model has the size of 1.5 KB, reduced from 16.6 KB of its full model counterpart. It can reach mean absolute error of 0.034 comparing to that of a naive baseline of 0.135. Such parameter-efficient and predictive neural network models established feasibility and practicality of their deployment on front-end ASICs.

47 OTHER INSTRUMENTATION↗

A Step-Down Test Procedure for Wavelet Shrinkage Using Bootstrapping

Wavelet thresholding (or shrinkage) attempts to remove the noises existing in the signals while preserving inherent pattern characteristics in the reconstruction of true signals. For data-denoising purpose, we present a new wavelet thresholding procedure which employs the step-down testing idea of identifying active contrasts in unreplicated fractional factorial experiments. The proposed method employs bootstrapping methods to a step-down test for thresholding wavelet coefficients. By introducing the concept of a false discovery error rate in testing wavelet coefficients, we shrink the wavelet coefficients with p -values higher than the error rate. The error rate controls the expected proportion of wrongly accepted coefficients among chosen wavelet coefficients. Bootstrap samples are used to approximate the p -value for computational efficiency. We also present some guidelines for selecting the values of hyper-parameters which affect the performance in the step-down thresholding procedure. Based on some common testing signals and an air-conditioner sounds example, the comparison of our proposed procedure with other thresholding methods in the literature is performed. The analytical results show that the proposed procedure has a potential in data-denoising and data-reduction in a variety of signal reconstruction applications.

42 ENGINEERING↗

SU-E-J-251: Fast MR-Based DRR Generation Using Highly Undersampled 3D Radial Trajectories

Purpose: The construction of a digitally reconstructed radiograph (DRR) from a magnetic resonance image (MRI) is possible if the cortical bone signal can be acquired and separated from air and soft tissue. This may be accomplished by subtracting a long echo-time, in-phase, gradient echo (GRE) image volume from an ultra-short echo time free induction decay (FID) image to produce a bone-enhanced (BE) image that reveals cortical bone. One limitation of this approach is the length of time required for data acquisition, which can limit the quality of the DRRs due to patient and organ motion. This study aimed to significantly reduce the acquisition time without compromising DRR quality. Methods: Brain data were acquired from two volunteers using a 3T MR scanner (Ingenia, Philips Healthcare). The FID and GRE images were acquired in a single acquisition using a 3D radial readout sequence with the following parameters: TE1=0.142ms (ultra-short), TE2=2.197ms (nearly in-phase), 2*2*2mm3 isotropic voxels, 250*250*250mm3 FOV. To reduce the acquisition time, k-space was sampled at 75, 50 and 25% of a full 3D sphere . The TE2 image was subtracted from the TE1 image to generate the BE images. The BE images were used to generate DRRs using the Pinnacle treatment planning system (Philips-version 9.2). The quality of the DRRs was evaluated qualitatively by 5 board certified medical physicists for clinical usefulness. Results: The acquisition time for 75, 50 and 25% sampling schemes were 219s, 146s, and 73s, respectively, the latter of which was a four-fold reduction in scan time compared to a 300s fully-sampled acquisition. All DRRs obtained were of acceptable quality and were shown to have sufficient information for clinical 2D image matching. Conclusion: Undersampling k-space while maintaining the same range of frequency information results in significantly reduced scan time and clinically acceptable DRR image quality. Drs. B Traughber and R Muzic have research support from Philips Healthcare. Drs. M Traughber and L Hu are employees of Philips Healthcare.

60 APPLIED LIFE SCIENCES↗

Metal oxide core shell nanostructures as building blocks for efficient light emission (SISGR)

The objective of this research is to synthesize core-shell nano-structured metal oxide materials and investigate their structural, electronic and optical properties to understand the microscopic pathways governing the energy conversion process, thereby controlling and improving their efficiency. Specifically, the goal is to use a single metal oxide core-shell nanostructure and a single excitation source to generate photons with long emission lifetime over the entire visible spectrum and when controlled at the right ratio, generating white light. In order to achieve this goal, we need to control the energy transfer between light emitting elements, which dictates the control of their interatomic spacing and spatial distribution. We developed an economical wet chemical process to form the nanostructured core and to control the thickness and composition of the shell layers. With the help from using DOE funded synchrotron radiation facility, we delineated the growth mechanism of the nano-structured core and the shell layers, thereby enhancing our understanding of structure-property relation in these materials. Using the upconversion luminescence and the lifetime measurements as effective feedback to materials sysnthes is and integration, we demonstrated improved luminescence lifetimes of the core-shell nano-structures and quantified the optimal core-multi-shell structure with optimum shell thickness and composition. We developed a rare-earths co-doped LaPO 4 core-multishell structure in order to produce a single white light source. It was decided that the mutli-shell method would produce the largest increase in luminescence efficiency while limiting any energy transfer that may occur between the dopant ions. All samples resulted in emission spectra within the accepted range of white light generation based on the converted CIE color coordinates. The white light obtained varied between warm and cool white depending on the layering architecture, allowing for the utilization into a wide range of applications. With DOE’s overall mandate to reduce the US’s dependence on rare-earth elements, this work demonstrated how to make every RE atom count toward white light generation by controlling their spatial distribution thereby significantly reducing the amount needed. This is one approach toward reducing the dependence on RE elements and the strategies we developed can be used in discovering RE-free systems. The project is of benefit to the general public as it improves the optical efficiency of these materials, while reducing US’s dependence on RE elements.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Martian sandstorms and their effects on the 1975 Viking lander system

A model of a Martian sandstorm has been derived from presently available data. The erosional effects of such a storm on the Viking lander were determined by test, and modifications involving the application of silicone-based protective material were made to insure lander survivability over the planned 60-day mission. Material eroded by windblown sand is expected to provide a source of contaminant for the soil samples used in the organic analysis experiment. Results of analyses predicting the level of such contamination indicate that soil sample contaminant concentration will be below the acceptable maximum.

Maegley, W. J.↗

Fraction-storage unit for drug-identification system

Device, connecting outputs of all gas chromatographs to single, relatively inexpensive IR spectrometer, reduces costs of system. Storage unit provides buffer storage of samples until infrared spectrometer is ready to accept them. Storage unit can be used to separate overlapping peaks.

Campen, C. F.↗

Biasing errors and corrections

The dependence of laser velocimeter measurement rate on flow velocity is discussed. Investigations outlining that any dependence is purely statistical, and is nonstationary both spatially and temporally, are described. Main conclusions drawn are that the times between successive particle arrivals should be routinely measured and the calculation of the velocity data rate correlation coefficient should be performed to determine if a dependency exists. If none is found, accept the data ensemble as an independent sample of the flow. If a dependency is found, the data should be modified to obtain an independent sample. Universal correcting procedures should never be applied because their underlying assumptions are not valid.

Meyers, James F.↗

Separable Organic Evaluation: Waste Feed Delivery Impacts - 17563

The potential for separable organic materials to separate out from Hanford tank waste requires consideration for future Waste Feed Delivery operations. Separable organic materials are organic compounds of very limited solubility in bulk waste that can form a separate phase or layer. If the organic materials bound to waste separates during mixing and transfer operations, the feed batch would be disqualified under the Hanford Tank Waste Treatment and Immobilization Plant (WTP) waste acceptance criteria for 'no visible immiscible layer.' Sample data and process history were used to identify tanks with the potential to contain separable organic materials. Centrifuge testing was performed on available archived tank samples and on waste simulants developed to mimic characteristics of the archived tank samples. A separable layer formed during centrifuge testing of archived samples 241-C-204, 241-SY-102, and for all developed simulants tested. Due to the formation of a separable organic layer during the centrifugation studies, an impact assessment was performed. This impact assessment identified forty-four potential tanks of concern regarding the release of organic material bound to solids during waste disturbing activities. A Hanford Tank Waste Operations Simulator model run was modified to trace the origin of each batch to the WTP. The outputs of the model run indicated that a separable organic layer would form during High Level Waste Feed Delivery operations and would cascade to all tanks containing or receiving significant amounts of organic solvents/diluents. Hence, there is a potential for a ripple effect across the feed batches. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

X-Ray Fluorescence Quantitative and Qualitative Analysis Using Micro Glass Beads

The fused glass bead method is the accepted 'best practice' method of preparation of samples for X-ray fluorescence (XRF) analysis. It minimizes the effects of sample heterogeneity and simplifies calibration by dissolving the sample into a uniform glass matrix. Glass fusion XRF samples are typically prepared by grinding sample powder with Lithium Tetraborate / Lithium Bromide and fusing the mixture at 1000 deg. C. In most cases sample-to-flux ratios of between 1:1 to 1:10 are used (1:1 for determination of trace elements and 1:10 for major elements). Typical sample mass consumed is in the range of 1000 to 2500 mg. It would be advantageous to reduce this sample mass in cases where the sample material is rare, valuable or highly radioactive. This study examines the effects of using lower sample-to-flux ratios and smaller fusion bead size on the detection and quantification of major and trace elements by XRF analysis. We have employed a micro fused glass bead process, using sample-to-flux ratios of 1:10, 1:15 and 1:25, to determine the effects on measurement precision, accuracy and detection limit. Objectives: - Created micro fused glass beads of a series of standards and andesite sample with sample-to-flux ratios of 1:10, 1:15 and 1:25. - Perform an qualitative analysis of the different sample-to-flux ratio micro beads and compare the results with the 1:5.3 beads routinely used at SRNL. - Quantitate the major components in the different sample-to-flux ratio micro beads using a wavelength dispersive x-ray fluorescence instrument. Advantages: - Reduce sample amount needed. - Speed up waste tank characterization. - Reduce personnel exposure. - Potential sealed source. Fused micro glass beads with sample-to-flux ratios of 1:10, 1:15 and 1:25 were created using sample amounts of 123 mg, 82 mg and 52 mg respectively. It was possible to detect most of the major oxides and some trace elements in the fused micro glass beads with different sample-to-flux ratios. The quantitative analysis showed good linear correlation between the intensity of the analysis and the concentration of the elements. Good precision and accuracy results were obtained for the majority of the major oxides in the three fused micro glass beads with different sample-to-flux ratios. Path Forward: Enhance the precision and accuracy of the method by optimizing different sample preparation steps, such as weighing and sample transfer. Continue to increase the sample-to-flux ratio to determine the minimum amount of sample needed to perform a multielement analysis. Consider the use of synthetic standards to lower the detection limit of the analysis. Used the micro bead sample preparation method to analyze radioactive samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

Laser-Induced Spectrochemical Assay for Uranium Enrichment (LISA-UE)

Uranium hexafluoride (UF6) is the uranium compound typically involved in uranium enrichment process. As the first line of defense against nuclear proliferation, accurate determinations of the uranium enrichment ratio in UF6 are critical for materials verification, accounting and safeguards. Shipping gaseous UF6 samples off-site for analysis with mass spectrometry is cumbersome and costly, and results are not available for some time (months). In-field UF6 enrichment assay has the potential to substantially reduce the time, logistics and expense of sample handling. At present, COMPUCEA is the only accepted method for UF6 enrichment assay in the field. Laser-Induced Spectrochemical Assay for Uranium Enrichment (LISA-UE) is an all-optical (based on laser induced plasma emission) analytical technique intended for fieldable, accurate, precise and rapid UF6 enrichment assay. In its operation, laser induced plasma is created directly in the gaseous UF6 sample. Because different U isotopes emit at slightly different wavelengths, the isotopic information of the UF6 sample is inherently encoded in the atomic emission from the plasma. Isotopic emissions from 235U and 238U are measured simultaneously, which eliminate correlated noise from the laser induced plasma. Isotopic information of the UF6 sample can be extracted from the acquired spectrum with theoretical multi-variable non-linear spectral fitting. To date, advances made by the LISA-UE research team include optimization of the spectral window for direct gaseous UF6 enrichment assay with laser induced plasma, development of data reduction algorithms, and demonstrations of the LISA-UE technique with gaseous UF6 samples. In this presentation, the technical aspect of LISA-UE will be overviewed, the data reduction algorithm will be described, and performance of the technique will be discussed.

Chan, George↗

Influence of sampling frequency and estimation method on phosphorus load uncertainty in the Western Lake Erie Basin, Ohio, USA

Accurate estimates of nutrient loads are necessary to identify critical source areas and quantify the impact of management practices on pollutant export. Previous studies have investigated nutrient load estimate uncertainty, but they often focus on nutrient loads estimated using an interpolation method for large-scale watersheds with short-term datasets. The study objective was to quantify uncertainty in soluble reactive phosphorus (SRP), total phosphorus (TP), and suspended solids (SS) load estimates from two small (<10 3 km 2 ) agricultural watersheds in the western Lake Erie Basin resulting from different sampling frequencies. Each watershed had high temporal resolution datasets of discharge (15 min) and nutrient concentration (1 to 3 samples per day) collected over a 30-year period (1990–2020). Firstly, SRP, TP, and SS loads were calculated using the high temporal resolution datasets, which was assumed as “true loads”. Secondly, the high temporal concentration data were decomposed to semiweekly, weekly, biweekly, and monthly sampling and annual loads were estimated using four common load estimation methods to assess the effect of sampling frequency and load estimation method on load estimate error. Across the four different methods, the composite method had the lowest relative root mean square and absolute bias, but the rectangular interpolation method was the most precise. Furthermore, even with semiweekly sampling, the composite method resulted in an unacceptable level of precision (average imprecision = 39 %), while the interpolation method resulted in an unacceptable bias (average absolute bias = 16 %). Because neither method could provide acceptable accuracy and precision at the lowest decrease in sampling (e.t. semiweekly sampling), continued daily sampling is recommended in these watersheds.

54 ENVIRONMENTAL SCIENCES↗