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NASA NTRS2023

Fluid Inclusions in Extraterrestrial Samples: Failures, Successes, Possibilities, and A Note of Caution

Over the past half century the search for life in the solar system and beyond has become a major research focus, with much effort devoted to finding evidence for liquid H2O and reduced carbon-bearing (organic) species in extraterrestrial samples. The most direct and convincing evidence for the presence of water and organic molecules is provided by fluid inclusions (FI)trapped in minerals that formed on the parent bodies. Beginning in the 1970s, reports of FI in extraterrestrial samples generated much enthusiasm within the planetary sciences community. However, many of the reported FI were determined to be artifacts of sample preparation, or incomplete characterization of features that appear to be FI, or were inconsistent with the inferred PT history of the meteorite sample. An early report of aqueous (and hydrocarbon-bearing) FI in stony meteorites and the subsequent follow-up study that showed that most or all of the “FI” contained water used during cutting and polishing of the samples led to a general unwillingness to believe later reports of FI in meteorites. One of the first confirmed occurrences of extraterrestrial aqueous (liquid) fluid inclusions in a meteorite was reported by Zolensky et al. (1999; Science), who described aqueous inclusions in halite in the Monahans and later the Zag meteorites. These meteorite falls were collected shortly after landing on earth and were prepared without using water or other fluids that could introduce artifacts. The oxygen and hydrogen isotopic composition of water in FI in these same samples was later measured, showing that the fluids represent various degrees of water-rock interaction on the parent body .In more recent years, careful studies of FI trapped in extraterrestrial samples combining synchrotron X-ray computed tomography to locate FI in samples followed by cryo-TOF-SIMS analysis of the FI have identified the presence of molecular fragments suggesting the presence of H2O and various organic molecules in the fluids. Challenges associated with studying FI in extraterrestrial samples include the limited abundance of potential host phases for FI, such as carbonates and phosphates, the often poor optical quality of the host phases, and the small size of the FI, with few as large as 5 microns and most less than 1-2 microns in maximum dimension

Robert Bodnar↗

NASA NTRS2024

Contamination Results of MISSE 8 Wake and Nadir Samples After 2 Years of Space Exposure on the International Space Station

Spacecraft in low Earth orbit (LEO) are subjected to harsh environmental conditions, including radiation (cosmic rays, ultraviolet, x-ray and charged particle radiation), micrometeoroids and orbital debris, temperature extremes, thermal cycling, and atomic oxygen. In addition, on-orbit spacecraft contamination is a serious spaceflight issue, with silicone contamination being a particular concern. In an effort to understand on-orbit contamination of Materials International Space Station Experiment 8 (MISSE 8) flight samples and other International Space Station (ISS) payloads, contamination studies were conducted post-flight on retrieved Teflon fluorinated ethylene propylene (FEP) samples flown in the wake and nadir orientations on MISSE 8. The wake sample was Teflon FEP (M8-W11) flown as part of the Glenn MISSE 8 Polymers Experiment on the Optical Reflector Materials Experiment-III Ram/Wake (ORMatE-III R/W) tray and exposed to the LEO wake environment for 2.0 years. The nadir samples were silver-Teflon FEP radiator pieces taken from the MISSE 8 Single Events Upset Xilinx-Sandia Experiment II (SEUXSE II) Power Box and exposed to the LEO nadir environment for 2.14 years. The Teflon FEP flight materials were analyzed for changes in surface morphology and chemistry as compared to pristine control samples. The wake samples were also analyzed for changes in optical properties. There was no evidence of a molecular contamination layer present on the surface of the MISSE 8 wake or nadir facing Teflon FEP flight samples, although both the wake and nadir flight samples contained particulate contamination in some regions. The analyzed nadir particles were primarily zinc rich. The majority of analyzed wake particles were comprised of oxidized aluminum with small amounts of zinc and magnesium. The wake particles appear to have arrived early in the mission (or pre-flight) during a single event. This paper provides details of the MISSE 8 sample contamination analyses.

Erosion↗

DOE OSTI2019

Electronic device and method for compressing sampled data

An electronic device for compressing sampled data comprises a memory element and a processing element. The memory element is configured to store sampled data points and sampled times. The processing element is in electronic communication with the memory element and is configured to receive a plurality of sampled data points, a slope for each sampled data point in succession, the slope being a value of a change between the sampled data point and its successive sampled data point, and store the sampled data point in the memory element when the slope changes in value from a previous sampled data point.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2021

Electronic device and method for compressing sampled data

Morrow, Mitchell Hedges↗

DOE OSTI2021

Electronic device and method for compressing sampled data

Tohlen, Michael Aaron↗

DOE OSTI2020

Multimodal Mass Spectrometry Imaging (MSI) of Archean and Jurassic Geologic Samples

Current geochemical analytical techniques such as gas chromatography-mass spectrometry (GC-MS and $G\acute{C}GC-MS$) can effectively determine the composition and structure of the organic biosignatures within a sample but cannot resolve the spatial distribution of organic biosignatures within rocks or sediments. The spatial distribution can be used to determine the character of the organic biosignatures [1], which can be indigenous (deposited with host rocks), non-indigenous (incorporated after deposition via fluid migration), or contaminant. Determining the character of organic biosignatures is critical for ancient samples [2] and will be critical if organics are observed in samples returned from Mars [3].Fs-LDPI-MS has the ability to map organic compounds across the surface of samples at 2 - 10 μm lateral resolution. Furthermore, fs-LDPI-MS can be used to carry out multiple analyses in the same location for micron-scale analysis of previously buried material [4]. We used fs-LDPI-MS to examine a ~164 million year old organic-rich mudstone from SW England (14.2 wt. % total organic carbon) [5] and determined the spatial distribution of likely indigenous components buried below potentially contaminated surface layers.We then used ToF-SIMS to re-analyze the mudstone to directly compare ToF-SIMS to fs-LDPI-MS datasets, and to analyze a series of ~2.7 billion year old geologic samples from Timmins, ON, CA [6]. Ref. [6] previously analyzed the Archean samples and observed a series of archaeal biomarkers, as well as hopanes and steranes. Using ToF-SIMS analysis, we were able to detect hopanes and steranes in the mudstone samples, but not in the Archean samples indicating that the hopanes and steranes are most likely contaminants in the Archean samples. We also did not observe the archaeal biomarkers; however, this may be from the lack of molecular ion preservation during ToF-SIMS.

Pasterski, Michael↗

DOE OSTI2021

Electronic device and method for compressing sampled data

Morrow, Mitchell Hedges↗

DOE OSTI2021

Single-Use Destructive Assay for Uranium Hexafluoride Sampling

Sampling uranium hexafluoride (UF6) for the determination of enrichments by destructive analysis (DA) is a critical component in the International Atomic Energy Agency’s layered safeguards approach for uranium processing facilities. Typically, gram-quantity UF6 samples are collected during inspections and stored under tag-and-seal until transportation to an off-site analytical laboratory. The shipping times can be long, and evolving restrictions on radioactive/corrosive materials shipments may increasingly limit the IAEA’s ability to transport UF6 samples easily. Pacific Northwest National Laboratory has developed a low-cost UF6 sampling technology called Single-Use Destructive Assay (SUDA) that addresses these challenges, as well as provides DA sample geometries that can be tailored for different analytical methods, including potential on-site analyses. The SUDA samplers, along with a unique holder, are designed for direct attachment to existing taps at uranium processing facilities, allowing gaseous UF6 to come into direct contact with a zeolite film. The SUDA technology features the ability to capture uranium in a more easily shipped and handled form as the solid, more stable, and relatively less hazardous hydrated uranyl fluoride (UO2F2•nH2O), which is formed through the controlled hydrolysis of UF6. We have recently simulated uranium collection under enrichment plant sampling conditions to further improve our understanding of SUDA sampling. Presented here is our recent work on measuring the relationship between sampling conditions and uranium collection, which includes control of the uranium-mass-to-zeolite ratio and assessing variable UF6 gas and sampling parameters that can affect collection using the SUDA sampler.

Pope, Timothy R.↗

DOE OSTI2021

Data Report on Post-Irradiation Dimensional Change of AGC-1 Samples

This report documents the measured post irradiation dimensional change in the AGC-1 samples. The AGC-1 capsule is the first in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. AGC-1 irradiation began September 5, 2009 in the Advanced Test Reactor (ATR) and was completed on January 8, 2011. The capsule was cooled for 3 months in the ATR Canal, and then shipped to MFC in April 2011 for disassembly and sample extraction. After extraction the samples were shipped to the INL Research Center (IRC) for initial post-irradiation examination (PIE) and storage in the irradiated graphite vault. The AGC-1 capsule design contained “matched pair” samples to ascertain the irradiation-induced dimensional changes and levels of creep experienced in different graphite types. The irradiation-induced dimensional changes and creep levels are determined by comparing the total dimensional change for stressed and unstressed samples of the same type of graphite exposed to the same dose levels and at similar temperatures. Under irradiation creep (i.e. permanent strain due to irradiation, stress, and temperature) the stressed samples should demonstrate more dimensional change than the unstressed samples. This additional dimensional change in the stressed samples is designated as “irradiation-induced creep” in graphite. The data are further presented using the parameters influencing dimensional change in graphite; levels of induced stress, temperature, graphite type, and dose. However, the AGC-1 post-irradiation examination is a significant endeavor and this data report serves to provide irradiation-induced dimensional change data for AGC capsule design refinement as well as a status on the progress of the PIE activities. The dimensional changes of both the samples and graphite body are very important to the design of the future AGC capsules (AGC-3 through AGC-6) and are provided as soon as the data are available in order to determine whether design changes to the next capsule are required. A complete evaluation of the irradiation-induced dimensional change data will be performed for a final AGC-1 PIE report that will include full analysis of pre- and post-irradiation data, with verified AGC-1 irradiation conditions of temperature and dose.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Per-instruction energy debugging using instruction sampling hardware

A processor utilizes instruction based sampling to generate sampling data sampled on a per instruction basis during execution of an instruction. The sampling data indicates what processor hardware was used due to the execution of the instruction. Software receives the sampling data and generates an estimate of energy used by the instruction based on the sampling data. The sampling data may include microarchitectural events and the energy estimate utilizes a base energy amount corresponding to the instruction executed along with energy amounts corresponding to the microarchitectural events in the sampling data. The sampling data may include switching events associated with hardware blocks that switched due to execution of the instruction and the energy estimate for the instruction is based on the switching events and capacitance estimates associated with the hardware blocks.

Wei, Shijia↗

DOE OSTI2015

Prompt Gamma Ray Analysis of Soil Samples

Neutron moderation effects were measured in bulk soil samples through prompt gamma ray measurements from water and benzene contaminated soil samples using 14 MeV neutron inelastic scattering. The prompt gamma rays were measured using a cylindrical 76 mm x 76 mm (diameter x height) LaBr{sub 3}:Ce detector. Since neutron moderation effects strongly depend upon hydrogen concentration of the sample, for comparison purposes, moderation effects were studied from samples containing different hydrogen concentrations. The soil samples with different hydrogen concentration were prepared by mixing soil with water as well as benzene in different weight proportions. Then, the effects of increasing water and benzene concentrations on the yields of hydrogen, carbon and silicon prompt gamma rays were measured. Moderation effects are more pronounced in soil samples mixed with water as compared to those from soil samples mixed with benzene. This is due to the fact that benzene contaminated soil samples have about 30% less hydrogen concentration by weight than the water contaminated soil samples. Results of the study will be presented. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2021

WHOLESCALE Catalog of Rock Samples at San Emidio Nevada collected in January 2021

This submission contains information on thirty-six rock samples collected from San Emidio, Nevada during January, 2021 for Subtask 2.3 of the WHOLESCALE project. The following resources include a .zip of rock sample photos taken in the field, a .zip of rock sample photos taken in the laboratory at UW-Madison, and an excel catalog of rock samples with information on sample name, rock type, coordinates of sample location, structural measurements, field notes, observations for plug preparation (e.g., weathering, ability to be cut and cored), and rock descriptions. It should be noted that not every sample was photographed in the field. Names and descriptions of rock formation units are taken from Rhodes et al. (2011). The README.txt file is a description of this submission.

15 GEOTHERMAL ENERGY↗

DOE OSTI2021

Integrated sample-handling and mounting system for fixed-target serial synchrotron crystallography

Serial synchrotron crystallography (SSX) is enabling the efficient use of small crystals for structure–function studies of biomolecules and for drug discovery. An integrated SSX system has been developed comprising ultralow background-scatter sample holders suitable for room and cryogenic temperature crystallographic data collection, a sample-loading station and a humid `gloveless' glovebox. The sample holders incorporate thin-film supports with a variety of designs optimized for different crystal-loading challenges. These holders facilitate the dispersion of crystals and the removal of excess liquid, can be cooled at extremely high rates, generate little background scatter, allow data collection over >90° of oscillation without obstruction or the risk of generating saturating Bragg peaks, are compatible with existing infrastructure for high-throughput cryocrystallography and are reusable. The sample-loading station allows sample preparation and loading onto the support film, the application of time-varying suction for optimal removal of excess liquid, crystal repositioning and cryoprotection, and the application of sealing films for room-temperature data collection, all in a controlled-humidity environment. The humid glovebox allows microscope observation of the sample-loading station and crystallization trays while maintaining near-saturating humidities that further minimize the risks of sample dehydration and damage, and maximize working times. This integrated system addresses common problems in obtaining properly dispersed, properly hydrated and isomorphous microcrystals for fixed-orientation and oscillation data collection. Its ease of use, flexibility and optimized performance make it attractive not just for SSX but also for single-crystal and few-crystal data collection. Fundamental concepts that are important in achieving desired crystal distributions on a sample holder via time-varying suction-induced liquid flows are also discussed.

47 OTHER INSTRUMENTATION↗

DOE OSTI2016

Underground Test Area Calendar Year 2014 Annual Sampling Analysis Report Nevada National Security Site, Nevada, Revision 0

This report presents the analytical data for the 2014 fiscal year (FY) and calendar year (CY) (October 1, 2013, through December 31, 2014), and an evaluation of the data to ensure that the Sampling Plan’s objectives are met. In addition to samples collected and analyzed for the Sampling Plan, some NNSS wells are monitored by NNSA/NFO to demonstrate compliance with State-issued water discharge permits; with protection of groundwater from ongoing radiological waste disposal activities (compliance wells); and to demonstrate that the onsite drinking water supply is below SDWA maximum contaminant levels (MCLs) (public water system [PWS] wells). While not all sampled locations are required by the Sampling Plan, these samples are relevant to its objectives and are therefore presented herein for completeness purposes. Special investigations that took place in 2014 that are relevant to the Sampling Plan are also presented. This is the first annual report released to support Sampling Plan implementation.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2012

Rotary Percussive Sample Acquisition Tool (SAT): Hardware Development and Testing

In support of a potential Mars Sample Return (MSR) mission an Integrated Mars Sample Acquisition and Handling (IMSAH) architecture has been proposed to provide a means for Rover-based end-to-end sample capture and caching. A key enabling feature of the architecture is the use of a low mass sample Acquisition Tool (SAT) that is capable of drilling and capturing rock cores directly within a sample tube in order to maintain sample integrity and prevent contamination across the sample chain. As such, this paper will describe the development and testing of a low mass rotary percussive SAT that has been shown to provide a means for core generation, fracture, and capture.

Integrated Mars Sample Acquisition and Handling (I↗

DOE OSTI2022

How to avoid multiple scattering in strongly scattering SANS and USANS samples

Small Angle Neutron Scattering (SANS) and Ultra Small Angle Neutron Scattering (USANS) are the only available experimental techniques to provide seamless non-destructive measurements of the geometry of the accessible and inaccessible pore structure of rocks from sub-nanopore size to the scale of macropores. They have therefore become the measurement of choice for tight reservoir rocks such as organic rich shales. A simplifying assumption in the analysis is, however, that during the path of neutrons through the sample each neutron is only scattered once. Shales are samples with a high scattering power and Multiple Scattering (MS) may occur which requires special modelling for deconvolution of the results. The approach to avoid MS is to simply reduce the sample thickness to <0.15–0.5 mm. Here, in this work, we present a systematic method on wavelength selection and preparation of samples to optimise extraction of microstructural data and minimise parasitic errors. Experimentally measured SAS transmission (TSAS) values are used as a practical criterion for estimation of the extent of MS. Generous beamtime allocations allowed robust testing revealing that sample thicknesses can be twice as thick as predicted using the standard protocol. Analysing thicker samples is particularly beneficial for statistically relevant characterisation of heterogeneous samples making the new protocol the method of choice for such samples.

(U)SANS↗

DOE OSTI2021

Adversarial sampling of unknown and high-dimensional conditional distributions

Many engineering problems require the prediction of realization-to-realization variability or a refined description of modeled quantities. In that case, it is necessary to sample elements from unknown high-dimensional spaces with possibly millions of degrees of freedom. While there exist methods able to sample elements from probability density functions (PDF) with known shapes, several approximations need to be made when the distribution is unknown. In this paper the sampling method, as well as the inference of the underlying distribution, are both handled with a data-driven method known as generative adversarial networks (GAN), which trains two competing neural networks to produce a network that can effectively generate samples from the training set distribution. In practice, it is often necessary to draw samples from conditional distributions. When the conditional variables are continuous, only one (if any) data point corresponding to a particular value of a conditioning variable may be available, which is not sufficient to estimate the conditional distribution. This work handles this problem using an a priori estimation of the conditional moments of a PDF. Herein, two approaches, stochastic estimation, and an external neural network are compared for computing these moments; however, any preferred method can be used. The algorithm is demonstrated in the case of the deconvolution of a filtered turbulent flow field. It is shown that all the versions of the proposed algorithm effectively sample the target conditional distribution with minimal impact on the quality of the samples compared to state-of-the-art methods. Additionally, the procedure can be used as a metric for the diversity of samples generated by a conditional GAN (cGAN) conditioned with continuous variables.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2022

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↗