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NASA NTRSDate not supplied

Meteorite Sample Section Repair at NASA Johnson Space Center

Introduction: Meteorite thin and thick sections are routinely shipped from NASA Johnson Space Center to fulfill sample allocation requests from principle investigators around the world. Sections are also re-turned to JSC when researchers are finished studying them since, in most cases, they can be reused for other studies. The sections are very fragile unfortunately, and sometimes return to us needing repairs. The fol-lowing should give you an idea of how we repair sections here in the very lab where they were created. NOTE: Please do not attempt to repair ANSMET meteorite sections that are in your possession. We will perform the repairs for you at NASA JSC if you send the section back to us. Section Delamination: The majority of the meteorite sections that we produce here are secured to the glass slide using a high quality, two-part epoxy. Occasionally, we are asked to use superglue if the researcher wishes to dismount the section from the slide. Both epoxy and superglue are excellent adhesives, but they both tend to embrittle with time which results in delamination from the slide. Exposure to vacuum can also degrade the adhesion between the sample section and the glass slide. Repeated handling of the slide edges can accelerate delamination and, as a preventive measure, the outer 1-2 mm of epoxy is trimmed from newly created sections at JSC. If conductive tapes (copper, carbon, etc.) are used on the section during analysis, great care must be taken in removing the tape so that the epoxy is not pulled up with it. If in doubt, the tape can be left on the section when it is returned to JSC. Before we perform any repairs to sample sections, carbon, gold, or other coatings are removed. We accomplish this using a slurry of 0.05 micron alumina and 190 proof ethyl alcohol applied to a felt polishing pad fitted to a rotating lap wheel. Coatings are re-moved in this manner from all sections that are re-turned to JSC. The extent of the delamination determines how we proceed with the section repair. If the meteorite sample area of the section is not disturbed, then we carefully remove the delaminated epoxy. This is done using a binocular microscope with a 6X zoom, cut-proof gloves, and a very sharp, single edged razor blade. We cut the delaminated epoxy with the blade angled away from the sample area and using very light pressure. The trimmed section is then cleaned in an ultrasonic bath of 200 proof ethyl alcohol for no more than 10 seconds and carefully dried using a lint-free clean room wipe. The section is then placed into a lab oven at 110o F in preparation for epoxy. We mix the resin and hardener components of the low viscosity epoxy and very small amounts are applied to the cut edges of the section using a needle probe and the binocular microscope. Warming the epoxy helps secure the existing section by filling any voids between the glass slide and the section. After the new epoxy cures, we give the section a light polish on a lap wheel fitted with cotton polishing paper that is charged with 1 micron diamond paste. If the section has delaminated to the point of sample area being lifted from the glass, then it may be irreparable. We employ the above technique along with clamping the section in a Teflon pad arrangement in order to flatten the sample while the epoxy cures. Otherwise, the sample will tend to curl. This works to some degree, but once the sample area curls, it seldom re-turns to the original flatness without cracking or bending. Canada Balsam and Crystalbond: We repair damaged sections that had originally been prepared using Canada Balsam or Crystalbond adhesives through the gradual application of heat. We take great care with these samples since these bonding materials tend to get brittle with age. The section is heated in gradual steps (40-50o F per hour) to the melting point of the adhesive. We repair the sample while the adhesive is fluid and then the section is cooled in the same gradual manner in which it was heated. Slide Cracks and Breaks: Accidents happen. Especially with something as small and fragile as a thin/thick section. We all know someone who has driven a microscope objective into a section. As bad as the damage may look, the section can be repaired in most instances. NOTE: Please do not try to tape or glue section pieces back together prior to returning the dam-aged section. This practice usually renders the section irreparable. If the glass slide is cracked but the section is still in one piece, we repair it by infilling the crack with the low viscosity epoxy mentioned earlier. If the slide is in pieces, we can reassemble it with epoxy on a new backer slide. This is a tricky task as the pieces need to be in the correct plane with respect to each other, especially if the sample area is split among several pieces.

Meteorite↗

NASA NTRSDate not supplied

Advances in X-ray Instruments to Support Mars Sample Return

The Mars 2020 Perseverance rover is currently collecting drill cores of ancient igneous and sedimentary rock in and around Jezero crater for potential transport to Earth. These samples from the martian surface will enable detailed mineralogical, geochemical, and petrological measurements to characterize ancient depositional and diagenetic environments, quantitatively age-date the samples, and identify the building blocks for life or evidence for life itself. Furthermore, these drill cores are especially precious because they may represent the most pristine samples from the martian surface and our best chance at identifying martian life, as future sample return missions may be conducted by humans that can introduce biological contaminants to the samples. Because of the importance of these samples, we must take great care in their handling, curation, and preliminary analyses so that they are preserved for scientific measurements for decades to come. In-situ measurements by Perseverance have identified minerals that further warrant special treatment of the returned samples. Hydrated sulfate carbonate, swelling clay minerals, and oxychlorine salts are extremely sensitive to changes in temperature and relative humidity. The structures of hydrated sulfates and oxychlorine minerals, in particular, readily change when exposed to different conditions, meaning the mineral assemblage of the as-returned samples may be lost if the samples aren’t handled properly. Characterizing the as-returned mineral assemblage, particularly of the salts, is essential for reconstructing past aqueous conditions and habitability. To characterize the as-returned mineral assemblage, the samples must be analyzed rapidly before phase changes occur and/or under controlled conditions (e.g., within a glove box). Significant recent advances in X-ray instrumentation for robotic exploration of the solar system have resulted in high-resolution miniaturized instruments that would provide mineralogical, geochemical, and petrological information on the returned martian samples without degradation of the mineral assemblage. Here, we describe a combined X-ray diffractometer/X-ray fluorescence spectrometer (XRD/XRF), an X-ray computed tomographic (XCT) instrument, and a scanned beam XRF mapping instrument that could be used in a glove box so that the martian samples remain under controlled conditions.

E. B. Rampe↗

DOE OSTI2015

System and method for extracting a sample from a surface

A system and method is disclosed for extracting a sample from a sample surface. A sample is provided and a sample surface receives the sample which is deposited on the sample surface. A hydrophobic material is applied to the sample surface, and one or more devices are configured to dispense a liquid on the sample, the liquid dissolving the sample to form a dissolved sample material, and the one or more devices are configured to extract the dissolved sample material from the sample surface.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Post-Closure Environmental Sampling and Inspection at the Amchitka Island, Alaska, Site - 17251

In the 1960's and early 1970's, three underground nuclear tests were conducted on Amchitka Island, Alaska. In 1965, the US Department of Defense-in conjunction with the US Atomic Energy Commission (AEC)-conducted the first of these nuclear tests, Long Shot, to provide data that would improve US capabilities for detecting underground nuclear explosions. In 1969, AEC conducted the second test, Milrow, to explore the feasibility of detonating a much larger device. In 1971, AEC conducted the third test, Cannikin, which was the largest underground test ever conducted by the US. The Long-Term Surveillance Plan (LTSP) for the Amchitka, Alaska, Site details how the US Department of Energy Office of Legacy Management (LM) intends to fulfill its mission to protect human health and the environment at and around the Amchitka Island site. The LTSP calls for monitoring to be performed every 5 years, at least during the initial phase of the project. The purpose of the monitoring is to develop a baseline of activity concentrations for selected radionuclides in biota, water, and soil, both on Amchitka Island and at the reference location on Adak Island, approximately 322 kilometers (200 miles) northeast of Amchitka. In addition to the environmental monitoring activities, seven mud pit caps that contain diesel-contaminated soils are inspected. The plan for biological and water sampling (both seawater and freshwater) during the May 2016 sampling event was developed through close coordination with the primary stakeholders, including the Alaska Department of Environmental Conservation, the Aleutian Pribilof Islands Association, and the US Fish and Wildlife Service. The environmental sampling in 2016 is a continuation of LM's evaluation of Amchitka Island's environment. Previous results from similar monitoring programs in 2004 and 2011 indicate that the environment is not being impacted by radionuclide migration and uptake from the underground nuclear testing conducted beneath Amchitka Island; consequently, subsistence and commercial-catch seafood is safe for human consumption. The collection of biota samples (rockfish, Irish lords, greenling, and rockweed) for cesium-134 ({sup 134}Cs), cesium-137 ({sup 137}Cs), plutonium-239 ({sup 239}Pu), plutonium-240 ({sup 240}Pu), and freshwater and seawater samples for {sup 134}Cs, {sup 137}Cs, and tritium ({sup 3}H) was the primary objective of the 2016 sampling effort. Rockfish, Irish lords, and greenling are resident, nonmigratory fish species that spend their entire life cycle in the marine environment, and rockweed is an inter-tidal species that may concentrate cesium. The seawater samples were collected primarily to determine if leakage from the Long Shot detonation could be detected and, secondarily, to compare with the background seawater samples collected from Adak Island. Cesium isotopes are also being analyzed to better understand the potential impact that the Fukushima-Daiichi release might have on the Amchitka and Adak environments. The target detection limits used for the 2016 sampling are lower than those used in previous studies. The lower detection limits make it possible for LM to delineate background activity levels for the radionuclides of interest. Data from the 2016 sampling event go beyond assessing food safety and focus on detecting leakage from the underground nuclear explosions. Additionally, the baseline activity concentrations obtained for the reference area (Adak Island) will enable identification of quantitative statistical trends in the results of future sampling programs. Sampling programs conducted in 2021 and beyond will have an objective to assess the statistical trends of radioactivity levels in the Amchitka Island environment. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2017

Challenges to Collection of High Quality Samples of Saltstone - 17468

The Savannah River Site (SRS) Saltstone Disposal Facility (SDF) is used to dispose of low-level radioactive liquid waste in the form of grout. The SDF is comprised of a series of concrete saltstone disposal units (SDUs) that receive the grout. The grout solidifies into a cementitious waste form known as saltstone. Properties of saltstone that influence contaminant release have been measured on simulant material but not on samples of emplaced saltstone because samples of emplaced radioactive saltstone are difficult to obtain, transport, and store in a manner that protects the properties of interest. Savannah River Remediation (SRR) initiated a project to obtain samples of emplaced saltstone such that the two critical properties, hydraulic conductivity and reduction capacity, are negligibly impacted by the sample collection effort. The sample collection project was established to manage sample collection efforts beginning with sample collection mock-up activities through field execution. The project focused on three phases: mock-up in a clean environment, development of equipment needed to maintain an inert environment during sample transport and laboratory storage, and coordination of Facility operations and support resources and schedules to support sample collection. A mock-up facility was constructed at SRS to mimic the SDU. Core drill equipment was tested, procedures developed, and operator training conducted using the mockup facility. Concurrent with mock-up activities, inert transportation and storage equipment was designed, manufactured, tested, and specific operating instruction included in the sample collection procedure. Inerting equipment minimized oxidation from the atmosphere as the samples were removed from the disposal unit, transported, and stored in the laboratory awaiting analysis. Coordination with the Saltstone Facility began during construction of the mock-up platform to collect current as-built information for platform construction. Baseline data was collected from the disposal unit vapor space to assess the potential for personnel exposure from chemical hazards associated with trapped vapors. Based on this data, mitigating actions were incorporated into the project scope. Finally, project and facility schedules were integrated to assure that facility non-processing windows, support personnel, equipment fabrication, and field preparation activities were in alignment and supportive of the overall sample collection objectives. During May 2014, 485 linear cm of approximately 5 cm diameter radioactive core material was successfully collected from three access ports in SDU Cell 2A, inerted, transported to the laboratory, and stored in an inert environment for analysis. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS2012

Rotary Percussive Sample Acquisition Tool

As part of a potential Mars Sample Return campaign NASA is studying a sample caching mission to Mars, with a possible 2018 launch opportunity. As such, a Sample Acquisition Tool (SAT) has been developed in support of the Integrated Mars Sample Acquisition and Handling (IMSAH) architecture as it relates to the proposed Mars Sample Return (MSR) campaign. The tool allows for core generation and capture directly into a sample tube. In doing so, the sample tube becomes the fundamental handling element within the IMSAH sample chain reducing the risk associated with sample contamination as well as the need to handle a sample of unknown geometry. The tool's functionality was verified utilizing a proposed rock test suite that encompasses a series of rock types that have been utilized in the past to qualify Martian surface sampling hardware. The corresponding results have shown the tool can effectively generate, fracture, and capture rock cores while maintaining torque margins of no less than 50% with an average power consumption of no greater than 90W and a tool mass of less than 6kg.

Sample Acquisition and Caching (SAC)↗

NASA NTRSDate not supplied

The Unique Scientific Value of Returned Samples

Most of the materials in the universe are so distant or inaccessible that the only way we can study them is remotely using various types of telescopes. However, in some cases we can study these materials directly because the samples become physically available to us. Some samples come to us of their own accord in the form of meteorites and cosmic dust. In other cases we have to work hard to carry out sample return missions like Apollo, Stardust, OSIRIS-REx, Hayabusa, and Hayabusa2 in order to get the samples ourselves. Once samples are physically available in terrestrial laboratories, we can learn details about their compositions and histories that could never be established by remote observations. This talk will highlight some of the unique scientific advances that can be made through the study of extraterrestrial materials, and will describe the various ways in which samples become available for study, with a focus on the acquisition of samples by sample return spacecraft missions. Aspects of NASA’s Stardust comet sample return mission and JAXA’s Hayabusa asteroid sample return mission will be highlighted and scientific highlights of these missions will be discussed. Finally, the presentation will end with an overview of the current status of NASA’s OSIRIS-Rex mission, which will is currently at Asteroid (101955) Bennu and will be returning samples to Earth in 2023.

Extraterrestrial Samples↗

DOE OSTI2018

Improved Nested Sampling and Surrogate-Enabled Comparison With Other Marginal Likelihood Estimators

Estimating marginal likelihood is of central importance to Bayesian model selection and/or model averaging. The nested sampling method has been recently used together with the Metropolis-Hasting (M-H) sampling algorithm for estimating marginal likelihood. This study develops a new implementation of nested sampling by using the DiffeRential Evolution Adaptive Metropolis (DREAMzs) sampling algorithm. The two implementations of nested sampling are evaluated for four models of a synthetic groundwater flow modeling. The DREAMzs-based nested sampling outperforms the M-H-based nested sampling in terms of their accuracy, convergence, efficiency, and stability, which is attributed to the fact that DREAMzs is more robust than M-H for parameter sampling. The nested sampling method is also compared with four other methods (arithmetic mean, harmonic mean, stabilized harmonic mean, and thermodynamic integration) commonly used for estimating marginal likelihood and posterior probability of the four groundwater models. The comparative study requires hundreds of millions of model executions, which would not be possible without using surrogate models to replace the original models. Using the arithmetic mean estimator as the reference, the comparison reveals that thermodynamic integration outperforms nested sampling in terms of accuracy and stability, whereas nested sampling is more computationally efficient to reach to convergence. Here, the harmonic mean and stabilized harmonic mean methods give the worst marginal likelihood estimation. Accurate marginal likelihood estimation is important for accurate estimation of posterior model probability and better predictive performance of Bayesian model averaging.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2022

Modular automated bottom-up proteomic sample preparation for high-throughput applications

Manual proteomic sample preparation methods limit sample throughput and often lead to poor data quality when thousands of samples must be analyzed. Automated liquid handler systems are increasingly used to overcome these issues for many of the sample preparation steps. Here, we detail a step-by-step protocol to prepare samples for bottom-up proteomic analysis for Gram-negative bacterial and fungal cells. The full modular protocol consists of three optimized protocols to: (A) lyse Gram-negative bacteria and fungal cells; (B) quantify the amount of protein extracted; and (C) normalize the amount of protein and set up tryptic digestion. These protocols have been developed to facilitate rapid, low variance sample preparation of hundreds of samples, be easily implemented on widely-available Beckman-Coulter Biomek automated liquid handlers, and allow flexibility for future protocol development. By using this workflow 50 micrograms of protein from 96 samples can be prepared for tryptic digestion in under an hour. We validate these protocols by analyzing 47 Pseudomonas putida and Rhodosporidium toruloides samples and show that this modular workflow provides robust, reproducible proteomic samples for high-throughput applications. The expected results from these protocols are 94 peptide samples from Gram-negative bacterial and fungal cells prepared for bottom-up quantitative proteomic analysis without the need for desalting column cleanup and with protein relative quantity variance (CV%) below 15%.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2016

Analysis of Tank 38H (HTF-38-16-26, 27) and Tank 43H (HTF-43-16-28, 29) Samples for Support of the Enrichment Control and Corrosion Control Programs

Savannah River National Laboratory analyzed samples from Tank 38H and Tank 43H to support Enrichment Control Program and Corrosion Control Program. The total uranium in the Tank 38H samples ranged from 20.5 to 34.0 mg/L while the Tank 43H samples ranged from 47.6 to 50.6 mg/L. The U-235 percentage ranged from 0.62% to 0.64% over the four samples. The total uranium and percent U-235 results appear consistent with previous Tank 38H and Tank 43H uranium measurements. The Tank 38H plutonium results show a large difference between the surface and sub-surface sample concentrations and a somewhat higher concentration than previous sub-surface samples. The two Tank 43H samples show similar plutonium concentrations and are within the range of values measured on previous samples. The plutonium results may be biased high due to the presence of plutonium contamination in the blank samples from the cell sample preparations. The four samples analyzed show silicon concentrations ranging from 47.9 to 105 mg/L.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Pacific Northwest National Laboratory Facility Radionuclide Emission Points and Sampling Systems

Battelle–Pacific Northwest Division operates numerous research and development laboratories in Washington State. The U.S. Department of Energy (DOE) contracts to Battelle at Richland facilities on both the DOE Hanford Site and the Pacific Northwest National Laboratory (PNNL) Richland campus. These facilities have the potential for radionuclide air emissions. The PNNL contract with DOE also includes operations at the PNNL-Sequim campus in Sequim, where there is also the potential for radionuclide air emissions. This document is a periodic update that describes current PNNL facility emission units and sampling systems. The National Emission Standard for Hazardous Air Pollutants (NESHAP [40 Code of Federal Regulations 61, Subpart H]) requires an assessment of all emission units that have the potential for radionuclide air emissions. Emission units are registered with the State of Washington. Potential emissions from emission units are assessed annually by PNNL staff. Sampling, monitoring, and other regulatory compliance requirements are designated based on the potential to-emit dose criteria, a graded approach to facility-identified potential impact categories, and regulatory requirements. The purpose of this document is to describe the facility radionuclide air emission sampling program and provide current and historical facility emission unit system performance, operation, and design information. For sampled emission units, the building, exhaust unit, control technologies, and sample extraction details are provided. Additionally, applicable configuration drawings, figures, and photographs are included. For non-sampled emission units, emission estimation and radionuclide source details are provided. Site-wide permits for the lowest potential impact category are described. Deregistered/transitioned emission unit details are also provided as necessary for at least 5 years post-closure/transition. Currently, five emission units are sampled continuously for particulate radionuclides at PNNL managed facilities on the PNNL-Richland campus (3 of the 5) and on the Hanford Site (2 of the 5). Four of these units have sampling systems that comply with the American National Standards Institute/Health Physics Society (ANSI/HPS) N13.1–2011 standard for sampling from stacks and ducts of nuclear facilities, and the fifth is grandfathered and compliant with the older ANSI N13.1–1969 standard. In addition, the PNNL-managed Hanford Site 325 Building EP 325-01-S stack is sampled continuously for emissions of tritium. No emissions sampling is required for the single licensed emission unit on the PNNL-Sequim campus.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2015

OSIRIS-REx, Returning the Asteroid Sample

This paper addresses the technical aspects of the sample return system for the upcoming Origins, Spectral Interpretation, Resource Identification, and Security-Regolith Explorer (OSIRIS-REx) asteroid sample return mission. The overall mission design and current implementation are presented as an overview to establish a context for the technical description of the reentry and landing segment of the mission.The prime objective of the OSIRIS-REx mission is to sample a primitive, carbonaceous asteroid and to return that sample to Earth in pristine condition for detailed laboratory analysis. Targeting the near-Earth asteroid Bennu, the mission launches in September 2016 with an Earth reentry date of September 24, 2023.OSIRIS-REx will thoroughly characterize asteroid Bennu providing knowledge of the nature of near-Earth asteroids that is fundamental to understanding planet formation and the origin of life. The return to Earth of pristine samples with known geologic context will enable precise analyses that cannot be duplicated by spacecraft-based instruments, revolutionizing our understanding of the early Solar System. Bennu is both the most accessible carbonaceous asteroid and one of the most potentially Earth-hazardous asteroids known. Study of Bennu addresses multiple NASA objectives to understand the origin of the Solar System and the origin of life and will provide a greater understanding of both the hazards and resources in near-Earth space, serving as a precursor to future human missions to asteroids.This paper focuses on the technical aspects of the Sample Return Capsule (SRC) design and concept of operations, including trajectory design and reentry retrieval. Highlights of the mission are included below.The OSIRIS-REx spacecraft provides the essential functions for an asteroid characterization and sample return mission: attitude control propulsion power thermal control telecommunications command and data handling structural support to ensure successful rendezvous with Bennu characterization of Bennus properties delivery of the sampler to the surface, and return of the spacecraft to the vicinity of the Earth sample collection, performed by the Touch-and-Go Sample Acquisition Mechanism (TAGSAM), to acquire a regolith sample from the surface Earth re-entry and SRC recovery. Following sample collection, OSIRIS-REx drifts away from Bennu until the Asteroid Departure Maneuver is commanded on March 4, 2021, sending OSIRIS-REx on a ballistic return cruise to Earth. No additional large deterministic maneuvers are required to return the SRC to Earth. During the cruise, tracking and trajectory correction maneuvers (TCMs) are performed as necessary to precisely target the entry corridor. As OSIRIS-REx approaches Earth, the reentry plans are reviewed starting about a year before arrival, and preparations begin. The spacecraft is targeted away from the Earth until 7 days before entry. The final two trajectory correction maneuvers bring the spacecraft on target toward the Utah Test and Training Range (UTTR), with sufficient time for contingency resolution. The SRC releases 4 hours prior to atmospheric entry interface and, using the Stardust capsule heritage design, employs a traditional drogue and main parachute descent system for a soft touchdown.

reentry↗

DOE OSTI2023

Molten Salt Sampling Techniques and Analytical Approaches

Recent global interest in pyroprocessing and molten salt reactors has brought salt sampling methods and techniques back to the forefront of nuclear safeguards concerns. Issues with uranium supplies have also encouraged various countries to pursue advanced nuclear fuel cycles. Tracking nuclear material in molten salt has proven to be a challenge and updating molten salt sampling will greatly help in this endeavor. Molten salt is problematic to sample due to salt stratification, lack of homogeneity, solids, and difficulty with hot cell adaptations. Various salt sampling techniques have been used since before the 1960s including surface, spoon/spatula, and bar solidification. Since then, new types of sampling techniques have been developed to improve sampling results. These include rod/dip, pipet, suction, filtered sampling along with devices such as the Valve Core Sampler and the Multi-Level Sampler. These different approaches are being analyzed and improved upon along with developing requirements for an improved salt sampling device. Work continues to develop salt samplers that are more robust, easier to segment, collect at a specific depth, can work with filters, and can collect fines. Sampling parameters are also being narrowed in terms of stirring, settling time, filtration, depth, etc. In the future, we hope to address deficiencies for process control and nuclear material accountancy control by determining the best way to collect samples that minimizes contaminants and is representative. A compilation of salt sampling approaches, analyses techniques, and an evaluation of findings will be presented.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

High energy X-ray characterization of the microstructure of PuGa alloy samples at macroscopic depths and non-ambient conditions

High energy (95 keV) X-rays were utilized to characterize the microstructure of eight PuGa alloy samples at room temperature and during cooling to ∼10 K. The samples had different Ga content (nominally 0-3.4 at.%), age, and history. A ninth sample, similarly characterized with neutron diffraction, was included to extend the Ga range to 7 at.%. The samples span the range from single phase α (monoclinic) to δ (face-centered cubic) PuGa, as well as a two-phase α′/δ sample. The crystallographic textures, phase fractions, lattice parameters and dislocation densities of each sample were evaluated through distinct analysis techniques. The textures of the samples were modest. In each case, the dislocation densities were relatively high, comparable to cold worked metals and metals exposed to similar radiation dose. At room temperature, the lattice parameters determined in the predominantly single-phase samples were larger than expected based on the nominal Ga concentration. The observed lattice thermal expansions of the single-phase δ samples to 10 K are self-consistent across the samples and consistent with previous measurements reported in the literature. Significantly larger thermal lattice strain is observed in the δ phase of the two-phase material due to mechanical constraint from the α′ phase, which has a three times larger thermal expansion and is much harder than the δ phase. In conclusion, the results demonstrate the unique value of high-energy X-rays for relatively routine microstructural characterization of Pu alloy samples.

36 MATERIALS SCIENCE↗

DOE OSTI2021

A numerical and experimental approach to compare the effect of sample thickness in small in-situ SEM and large ex-situ tensile testing in Alloy 709

ASTM standards for tensile tests define specific sample size requirements regardless of grain size of the material. However, sample size requirements for testing should be considered in conjunction with the number of grains within its reduced cross-sectional area. This is particularly important for in-situ Scanning Electron Microscope (SEM) tensile tests, as they have to be conducted on smaller samples. In this study, a comprehensive experimental and numerical evaluation of the effect of specimen thickness (and the resulting number of grains within the cross-section) were conducted using in-situ SEM tensile test (on submillimeter thick samples) and ex-situ tensile tests (on samples of 0.68–5.9 mm thickness) and the results are compared with FEM simulations outcome. All tests were conducted at room temperature and the results are correlated to the number of grains within the thickness of specimens. The tensile test results indicated that even though the 0.2% proof stress and the tensile strength do not vary for the current range of thicknesses (with number of grains in the cross-section varying from 13 to 118), a difference in necking mechanism exists. Post tensile strength, thinner samples undergo more shear failure and diagonal localized necking whereas thicker samples experience more diffuse necking indicated by decreased area of shear failure at the edges and increased area of dimpled tensile failure at the center of the sample. Further, FEM results complement the experimental findings by showing the formation of conjugated localized shear bands on the upper and lower surface in the 0.68 mm thick sample and shear bands combining to form singular shear bands in thicker samples. These results also confirm the validity of the in-situ SEM tensile tests conducted on thinner samples as long as the required minimum number of grains exist within the cross-section.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Combined Falling Drop/Open Port Sampling Interface System for Automated Flow Injection Mass Spectrometry

The aim of this work was to demonstrate and to evaluate the analytical performance of a combined falling drop/open port sampling interface (OPSI) system as a simple noncontact, no-carryover, automated system for flow injection analysis with mass spectrometry. The falling sample drops were introduced into the OPSI using a widely available autosampler platform utilizing low cost disposable pipet tips and conventional disposable microtiter well plates. The volume of the drops that fell onto the OPSI was in the 7–15 μL range with an injected sample volume of several hundred nanoliters. Sample drop height, positioning of the internal capillary on the sampling end of the probe, and carrier solvent flow rate were optimized for maximum signal. Sample throughput, signal reproducibility, matrix effects, and quantitative analysis capability of the system were established using the drug molecule propranolol and its isotope labeled internal standard in water, unprocessed river water and two commercially available buffer matrices. A sample-to-sample throughput of ~45 s with a ~4.5 s base-to-base flow injection peak profile was obtained in these experiments. In addition, quantitation with minimally processed rat plasma samples was demonstrated with three different statin drugs (atorvastatin, rosuvastatin, and fluvastatin). Direct characterization capability of unprocessed samples was demonstrated by the analysis of neat vegetable oils. Employing the autosampler system for spatially resolved liquid extraction surface sampling exemplified by the analysis of propranolol and its hydroxypropranolol glucuronide phase II metabolites from a rat thin tissue section was also illustrated.

47 OTHER INSTRUMENTATION↗

DOE OSTI2021

Efficient Sampling of Complex Interdependent and Multiplex Networks

Efficient sampling of interdependent and multiplex infrastructure networks is critical for effectively applying failure and recovery algorithms in real-world settings, as well as to generate property-preserving reduced-order graph-based ensembles that address topological uncertainties. In this paper, we first explore the performance, i.e. the success in preserving graph properties, of graph sampling algorithms for interdependent and multiplex networks with synthetic and real-world graphs. We simulate sampling algorithms under different parameter settings. These settings include probabilistic graph generators, coupling patterns, and various performance metrics. Our results show that while Random Node and Random Walk sampling algorithms perform best for interdependent networks, Random Edge and Forest Fire sampling algorithms perform best for multiplex networks. Second, we propose and implement a novel similarity-based sampling algorithm for multiplex networks that samples only log(N) number of layers of an N-layer multiplex network while yielding computational savings with performance guarantees. Experimental results show that similarity sampling outperforms complete sampling of all layers while decreasing performance costs from a linear scale to a logarithmic one. Our results also indicate that similarity-based sampling outperforms complete sampling and random selection in nearly all scenarios when tested with real-world data.

Subasi, Omer↗

DOE OSTI2019

Producing a BOSS CMASS sample with DES imaging

We present a sample of galaxies with the Dark Energy Survey (DES) photometry that replicates the properties of the BOSS CMASS sample. The CMASS galaxy sample has been well characterized by the Sloan Digital Sky Survey (SDSS) collaboration and was used to obtain the most powerful redshift-space galaxy clustering measurements to date. A joint analysis of redshift-space distortions (such as those probed by CMASS from SDSS) and a galaxy-galaxy lensing measurement for an equivalent sample from DES can provide powerful cosmological constraints. Unfortunately, the DES and SDSS-BOSS footprints have only minimal overlap, primarily on the celestial equator near the SDSS Stripe 82 region. Using this overlap, we build a robust Bayesian model to select CMASS-like galaxies in the remainder of the DES footprint. The newly defined DES-CMASS (DMASS) sample consists of 117,293 effective galaxies covering $1,244 {\rm deg}^2$. Through various validation tests, we show that the DMASS sample selected by this model matches well with the BOSS CMASS sample, specifically in the South Galactic cap (SGC) region that includes Stripe 82. Combining measurements of the angular correlation function and the clustering-z distribution of DMASS, we constrain the difference in mean galaxy bias and mean redshift between the BOSS CMASS and DMASS samples to be $\Delta b = 0.010^{+0.045}_{-0.052}$ and $\Delta z = \left( 3.46^{+5.48}_{-5.55} \right) \times 10^{-3}$ for the SGC portion of CMASS, and $\Delta b = 0.044^{+0.044}_{-0.043} $ and $\Delta z= ( 3.51^{+4.93}_{-5.91}) \times 10^{-3}$ for the full CMASS sample. These values indicate that the mean bias of galaxies and mean redshift in the DMASS sample is consistent with both CMASS samples within $1\sigma$.

79 ASTRONOMY AND ASTROPHYSICS↗