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DOE OSTI2026

Post-fire time series of sensor and geochemistry sample data from surface water, groundwater, precipitation, soil, and vegetation across Oak Creek watershed, Washington

This dataset supports a broader study examining wildfire impacts on hydrologic connectivity across 5 sites within the Oak Creek watershed and the resulting biogeochemical impacts. Stream sites were selected using the Advanced Terrestrial Simulator (ATS) hydrologic model to identify locations with varying groundwater contributions and hydrologic responses across different burn severity scenarios. The Retreat Fire burned from July 23 to August 2 in 2024, affecting the five study sites at varying burn severities. Each site is equipped with YSI EXO2 sondes logging sub-hourly throughout the year, and grab samples are collected approximately every six weeks. YSI sondes are used to measure temporally resolved proxies for groundwater inputs (specific conductivity) and organic matter (fluorescent dissolved organic matter; fDOM) along with basic water quality and depth. Grab samples of surface water, groundwater, and precipitation are analyzed for water stable isotopes and conductivity to understand endmembers for hydrologic mixing Grab samples of surface water, groundwater, soil water, and litter/vegetation/soil leachates are analyzed for organic matter composition measured by Fourier-Transform Ion Cyclotron Resonance Mass Spectrometry (FTICR-MS) to understand organic matter dynamics. Game camera photos are provided in a separate data package available at https://data.ess-dive.lbl.gov/datasets/doi:10.15485/3018598. Future versions of this dataset will include time series data from YSI EXO2 sondes (fDOM, dissolved oxygen, temperature, depth, specific conductance, turbidity, pH), BaroTROLL sensors (air temperature and barometric pressure), rain gauges (precipitation), and data from the soil and vegetation samples. Because this study is ongoing, this data package will be updated regularly to include newly collected data and the additional data types. For details on how to navigate data packages generated by this project, see https://data.ess-dive.lbl.gov/portals/PNNLRiverCorridorSFA/About. In addition to a readme, this data package also includes a file-level metadata (FLMD) file that describes each file and a data dictionary (DD) that describes all column/row headers and variable definitions. This dataset is comprised of (1) a folder of field photos; (2) a folder of surface water sample data; (3) a folder of raw Fourier transform ion cyclotron resonance mass spectrometry (FTICR-MS) data; (4) a data checks report; (5) file-level metadata; (6) data dictionary; (7) field metadata; (8) readme; (9) international generic sample number (IGSN) mapping file; and (10) field protocols. The sample data subfolder contains (1) dissolved organic carbon (DOC, measured as non-purgeable organic carbon, NPOC) data and averages; (2) total dissolved nitrogen data and averages; (3) stable water isotopes and averages; (4) methods codes; (5) FTICR-MS methods; and (15) a subfolder of 9.4 Tesla (9.4T) FTICR-MS data. This folder contains the processed data and three subfolders, one containing the .xml files, one containing the water CoreMS output files, and the other containing instructions and scripts for processing the files in CoreMS (https://github.com/EMSL-Computing/CoreMS). All files are .csv, .pdf, .R, .xml, .d, .html, .Rmd, .py, .cal, .json, .jpg, .jpeg, .png, .mov, or .mp4.

Biogeochemistry↗

DOE OSTI2017

Quantification of in-contact probe-sample electrostatic forces with dynamic atomic force microscopy

Here, atomic force microscopy (AFM) methods utilizing resonant mechanical vibrations of cantilevers in contact with a sample surface have shown sensitivities as high as few picometers for detecting surface displacements. Such a high sensitivity is harnessed in several AFM imaging modes. Here, we demonstrate a cantilever-resonance-based method to quantify electrostatic forces on a probe in the probe-sample junction in the presence of a surface potential or when a bias voltage is applied to the AFM probe. We find that the electrostatic forces acting on the probe tip apex can produce signals equivalent to a few pm of surface displacement. In combination with modeling, the measurements of the force were used to access the strength of the electrical field at the probe tip apex in contact with a sample. We find an evidence that the electric field strength in the junction can reach ca. 1 V nm –1 at a bias voltage of a few volts and is limited by non-ideality of the tip-sample contact. This field is sufficiently strong to significantly influence material states and kinetic processes through charge injection, Maxwell stress, shifts of phase equilibria, and reduction of energy barriers for activated processes. Besides, the results provide a baseline for accounting for the effects of local electrostatic forces in electromechanical AFM measurements as well as offer additional means to probe ionic mobility and field-induced phenomena in solids.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Dielectric Barrier Discharge Electrothermal Heating and Additive Manufacturing of Thermoset Parts

Additive manufacturing of thermosets requires a mechanism for solidifying deposited layers in order to prevent part collapse. To accomplish this, non‐equilibrium plasma is proposed for its ability to target, heat, and cure printed thermosetting resin. Non‐equilibrium plasmas have not been used for the curing of liquid thermoset composites, and so their impact on an uncured resin is unknown. Here this work investigates the mechanism through which dielectric barrier discharge (DBD) heats an epoxy/carbon nanotube (CNT) composite under atmospheric conditions. Plasma applied to resin surfaces is found to cause rapid heating, with heating rate controlled by adjusting the applied power. Heating is localized to within the top 0.5 mm of the sample surface and maximum temperature is found to depend on sample conductivity, indicating the heating reaction occurs through a combination of electron conduction and ion bombardment. Characterization of composites cured using plasma shows oxidation and roughening of the surface. Based on the heating and surface studies, several demonstrative prints are performed using in situ plasma curing. This work shows the potential of DBD plasma to rapidly heat liquid substrates and demonstrates how plasma curing expands the capability of existing direct ink write (DIW) printer technologies.

3D printing↗

DOE OSTI2014

Experimental study of crack initiation and propagation in high- and gigacycle fatigue in titanium alloys

Fatigue (high- and gigacycle) crack initiation and its propagation in titanium alloys with coarse and fine grain structure are studied by fractography analysis of fracture surface. Fractured specimens were analyzed by interferometer microscope and SEM to improve methods of monitoring of damage accumulation during fatigue test and to verify the models for fatigue crack kinetics. Fatigue strength was estimated for high cycle fatigue regime using the Luong method [1] by “in-situ” infrared scanning of the sample surface for the step-wise loading history for different grain size metals. Fine grain alloys demonstrated higher fatigue resistance for both high cycle fatigue and gigacycle fatigue regimes. Fracture surface analysis for plane and cylindrical samples was carried out using optical and electronic microscopy method. High resolution profilometry (interferometer-profiler New View 5010) data of fracture surface roughness allowed us to estimate scale invariance (the Hurst exponent) and to establish the existence of two characteristic areas of damage localization (different values of the Hurst exponent). Area 1 with diameter ∼300 μm has the pronounced roughness and is associated with damage localization hotspot. Area 2 shows less amplitude roughness, occupies the rest fracture surface and considered as the trace of the fatigue crack path corresponding to the Paris kinetics.

36 MATERIALS SCIENCE↗

DOE OSTI2021

macroMS: Image-Guided Analysis of Random Objects by Matrix-Assisted Laser Desorption/Ionization Time-of-Flight Mass Spectrometry

Mass spectrometry imaging is well-suited to characterizing sample surfaces for their chemical content in a spatially resolved manner. However, when the surface contains small objects with significant empty spaces between them, more efficient approaches to sample acquisition are possible. Image-guided mass spectrometry (MS) enables high-throughput analysis of a diverse range of sample types, such as microbial colonies, liquid microdroplets, and others, by recognizing and analyzing selected location targets in an image. Here, we describe an imaging protocol and macroMS, an online software suite that can be used to enhance MS measurements of macroscopic samples that are imaged by a camera or a flatbed scanner. Furthermore, the web-based tool enables users to find and filter targets from the optical images, correct optical distortion issues for improved spatial location of selected targets, input the custom geometry files into an MS device to acquire spectra at the selected locations, and finally, perform limited data analysis and use visualization tools to aid locating samples containing compounds of interest. Using the macroMS suite, an enzyme mutant library of Saccharomyces cerevisiae and nL droplet arrays of Escherichia coli and Pseudomonas fluorescens have been assayed at a rate of ~2 s/sample.

47 OTHER INSTRUMENTATION↗

DOE OSTI2012

Low-temperature formation of epitaxial graphene on 6H-SiC induced by continuous electron beam irradiation

It is observed that epitaxial graphene forms on the surface of a 6H-SiC substrate by irradiating electron beam directly on the sample surface in high vacuum at relatively low temperature ({approx}670 Degree-Sign C). The symmetric shape and full width at half maximum of 2D peak in the Raman spectra indicate that the formed epitaxial graphene is turbostratic. The gradual change of the Raman spectra with electron beam irradiation time increasing suggests that randomly distributed small grains of epitaxial graphene form first and grow laterally to cover the entire irradiated area. The sheet resistance of epitaxial graphene film is measured to be {approx}6.7 k{Omega}/sq.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

DOE OSTI2018

Electron-Stimulated Desorption of Cesium Atoms from Graphene-Covered Iridium

Electron-stimulated desorption (ESD) of cesium atoms from graphene on a metal (iridium) substrate has been directly observed for the first time using the time-of-flight technique with a surface-ionization detector. The appearance threshold of the yield of Cs atoms from the sample surface at 160 K was 20 eV. An additional ESD peak of Cs atoms was observed at an electron energy of 56 eV. The observed ESD of Cs atoms from graphene is related to the nonmetal nature of this carbon film on the metal substrate surface.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

DOE OSTI2019

Genome-resolved metagenomics of eukaryotic populations during early colonization of premature infants and in hospital rooms

Background: Fungal infections are a significant cause of mortality and morbidity in hospitalized preterm infants, yet little is known about eukaryotic colonization of infants and of the neonatal intensive care unit as a possible source of colonizing strains. This is partly because microbiome studies often utilize bacterial 16S rRNA marker gene sequencing, a technique that is blind to eukaryotic organisms. Knowledge gaps exist regarding the phylogeny and microdiversity of eukaryotes that colonize hospitalized infants, as well as potential reservoirs of eukaryotes in the hospital room built environment. Results: Genome-resolved analysis of 1174 time-series fecal metagenomes from 161 premature infants revealed fungal colonization of 10 infants. Relative abundance levels reached as high as 97% and were significantly higher in the first weeks of life (p = 0.004). When fungal colonization occurred, multiple species were present more often than expected by random chance (p = 0.008). Twenty-four metagenomic samples were analyzed from hospital rooms of six different infants. Compared to floor and surface samples, hospital sinks hosted diverse and highly variable communities containing genomically novel species, including from Diptera (fly) and Rhabditida (worm) for which genomes were assembled. With the exception of Diptera and two other organisms, zygosity of the newly assembled diploid eukaryote genomes was low. Interestingly, Malassezia and Candida species were present in both room and infant gut samples. Conclusions: Increased levels of fungal co-colonization may reflect synergistic interactions or differences in infant susceptibility to fungal colonization. Discovery of eukaryotic organisms that have not been sequenced previously highlights the benefit of genome-resolved analyses, and low zygosity of assembled genomes could reflect inbreeding or strong selection imposed by room conditions.

59 BASIC BIOLOGICAL SCIENCES↗

NASA NTRS2019

Mars Ascent Vehicle Hybrid Propulsion Development

Hybrid propulsion is being investigated as a propulsion method for a possible Mars Ascent Vehicle (MAV) application. MAV is part of a proposed larger Mars Sample Return (MSR) campaign plan to bring samples from Mars to earth for examination. The Mars Ascent Vehicle would launch Mars surface samples found and packaged by the Mars 2020 mission to orbit around Mars. This version of hybrid propulsion is based on a wax based solid fuel, called SP7A, and a Mixed Oxides of Nitrogen oxidizer, MON-25. SP7 is a new fuel formulation developed by Space Propulsion Group and was modified for this application to be resistant to Mars temperature extremes and modified again to lower the regression rate to become SP7A. MON-25 was chosen for its low freezing temperature. Due to cost constraints, MON-3 was the oxidizer used during testing through 2018. In 2019, full scale hybrid testing with MON-25 commenced in Mojave, CA by Whittinghill Aerospace. One flight motor will be subjected to thermal cycling in a vacuum and later fired in a vacuum to demonstrate the proposed Liquid Injection Thrust Vector Control system performance at White Sands Test Facility (WSTF). In addition, there will be MON-25 characterization work done at Purdue University and WSTF. Additional testing of subscale and full scale motors will be conducted with MON-3 with fuel grain stress, fuel grain support and case design test objectives by Space Propulsion Group Inc. of Butte, MT. This paper documents some of the testing, issues and accomplishments with the MAV hybrid propulsion option that is being considered (along with a two-stage solid propulsion option).

Story, G. T.↗

DOE OSTI2018

LIBS Measurement in Vitrification of HLW Process: Towards a Development of Online Chemical Analyses - 18290

Research programs are currently underway in the Joint CEA-AREVA Vitrification Laboratory (LCV) to develop and optimize Laser Induced Breakdown Spectroscopy (LIBS) for nuclear waste streams analyses. The laboratory has full scale prototypes with the advantage of working on simulated inactive solutions of fission products. LIBS is an elemental chemical analysis technology that uses a short laser pulse to create a micro-plasma on the sample surface. This analytical technique offers many advantages compared to other techniques. It includes a sample preparation-free measurement and an extremely fast measurement time, from a few seconds to a few minutes. This paper presents the LIBS technique available in the laboratory. The first LIBS analyzes results of liquid samples from the off-gas treatment unit integrated on the full scale vitrification process are also presented and discussed. These complex solutions contain suspended particles and up to 30 chemical elements. A vision of an online LIBS analysis cell is also proposed with the development and associated research steps. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2018

Optimization of LIBS Acquisition Parameters for Chemical Analysis on HLW Liquid Solution - 18291

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRSDate not supplied

Microbial Characterization of Heat Melt Compaction for Treatment of Space Generated Solid Wastes

One treatment process in development for solid waste management in space has been the Trash Compaction Processing System (TCPS). Human space mission wastes typically contain large percentages of contaminated wet solid waste. The Heat Melt Compactor (HMC) is being developed to be a multi-function means of water recovery, volume reduction, and the making safe of contaminant-rich trash with the potential for waste stabilization and/or sterilization. To determine the efficacy of the HMC treatment to kill microorganisms in solid waste and remain biologically stable, testing was conducted on three tiles produced by HMC-Gen 2 at Ames Research Center. Samples were shipped to Kennedy Space Center to test for microbial viability after compaction, determine the bio-stability of the HMC disks during storage (43 days), and assess potential airborne contaminate microbial growth on surfaces at low and high humidity conditions. In addition to the products of solid waste processing technologies, there is a concern that the crew might come into contact with hardware surfaces that have been contaminated by microorganisms during waste processing. The extent of microbial surface contamination of waste processing hardware was determined by surface sample swabbing and analysis for total bacterial and yeast counts and cultivable counts of aerobic and anaerobic bacteria, spore-forming bacteria, and fungi. Results indicate that trash processing increased bacterial counts on the surfaces of the compacter. All but one biological indicator spore strip imbedded in the HMC produced tiles were negative for growth after incubation for five days indicating effective sterilization through the heat melt compaction process. Analysis of core samples as well as surface growth of tiles inoculated with Aspergillus niger fungal spores incubated at three levels of humidity indicate that HMC created tiles did not support the proliferation of bacterial and fungal growth.

Mary E Hummerick↗

NASA NTRS2011

Crosscutting Development- EVA Tools and Geology Sample Acquisition

Exploration to all destinations has at one time or another involved the acquisition and return of samples and context data. Gathered at the summit of the highest mountain, the floor of the deepest sea, or the ice of a polar surface, samples and their value (both scientific and symbolic) have been a mainstay of Earthly exploration. In manned spaceflight exploration, the gathering of samples and their contextual information has continued. With the extension of collecting activities to spaceflight destinations comes the need for geology tools and equipment uniquely designed for use by suited crew members in radically different environments from conventional field geology. Beginning with the first Apollo Lunar Surface Extravehicular Activity (EVA), EVA Geology Tools were successfully used to enable the exploration and scientific sample gathering objectives of the lunar crew members. These early designs were a step in the evolution of Field Geology equipment, and the evolution continues today. Contemporary efforts seek to build upon and extend the knowledge gained in not only the Apollo program but a wealth of terrestrial field geology methods and hardware that have continued to evolve since the last lunar surface EVA. This paper is presented with intentional focus on documenting the continuing evolution and growing body of knowledge for both engineering and science team members seeking to further the development of EVA Geology. Recent engineering development and field testing efforts of EVA Geology equipment for surface EVA applications are presented, including the 2010 Desert Research and Technology Studies (Desert RATs) field trial. An executive summary of findings will also be presented, detailing efforts recommended for exotic sample acquisition and pre-return curation development regardless of planetary or microgravity destination.

Source record↗

NASA NTRS1988

Laboratory simulations of comet surfaces

The geometric albedos of frozen mixtures consisting of colloidal silica and carbon black mixed with water have been measured over the wavelength range of 400 to 800 nm to compare with recent observations of Comet Halley. Data were obtained as a function of sample temperature, scattering angle, and wavelength as the frozen samples warmed to 0 C in vacuum. Scattering from water ice, flat black paint, and Kodak white reflectance paint were also measured. Lab simulations show that the change in albedo of the samples show that sublimation of the water from the sample surface can have a major effect on the albedo of a particle/ice sample in the visible. Such processing may have a marked effect on the visible albedo of comet surfaces as well.

Stephens, John R.↗

NASA NTRSDate not supplied

Apollo Sample 64455: Petrologic and Geochemical Characterization of a Glass-Coated Impact Melt Rock

Introduction and Background: Impact melts are a key product of the impact cratering process. Impact melts can turbulently entrain pre-existing rock fragments, and melt part of those entrained materials until thermal equilibrium is achieved [1–3]. Lunar impact melt rocks are valuable for determining the precise ages of basin-forming and cratering events, which anchor the cratering chronology and dynamics of the entire solar system [4, and references therein]. Additionally, entrained clasts can inform on the petrology and age of crustal materials that predate the melt-forming impact. In lithologies where no pristine samples are available, entrained materials may hold the record of endogenous lunar volatiles, provided we can untangle their impact histories as high temperature impact melt can heat the clasts and may alter their native volatiles or isotopic signatures [5–6]. Here, we characterize an Apollo 16 sample, 64455,70B, in an effort to understand the physical, microstructural, and geochemical consequences of impact melt contact metamorphism. We acquired optical light and x-ray maps of the sample, as well as quantitative analyses via electron probe microanalysis (EPMA). These tasks allow us to better understand the interaction between impact melts and entrained clasts, ultimately closing knowledge gaps in high-temperature impact processing on planetary surfaces. Sample Description: Sample 64455 is an oblong crystalline rock encased in glass to form an egg-like shape [7–8]. The impact melt coating has altered the outer (1 to 2 mm) rind of the crystalline rock and has preserved schlieren. The interior crystalline rock is likely a crystalline impact melt rock based on its bulk Ir content of 2.25 parts per billion [9]. The composition of the impact melt glass rind cannot be solely derived from the crystalline interior, the glassy rind is more aluminous and less magnesian [10]. Neither the crystalline interior nor the glassy rind were radiometrically age dated, although several studies investigated its cosmogenic isotopes and exposure ages, which reveal the sample was exposed on the lunar surface for ~1–2 Ma [11–13]. Preliminary Results: The interior crystalline rock consists primarily of plagioclase with interstitial pyroxene and olivine. Plagioclase grains are zoned and compositions range from An97–89, while pyroxene compositions generally range from En68Fs19Wo13 to En82Fs15Wo3 and olivine are Fo77 to Fo85. Minor phases include Fe-Ni metal, Ca-phosphates, a K- and Si-rich phase, sulfides, and Fe-phosphides. The glass rind contains approximately 44 wt.% SiO2, 25 wt.% Al2O3, 6 wt.% FeO, 8 wt.% MgO, and 14 wt.% CaO, with other oxides at <1 wt.% each, although the composition of the glass becomes more variable closest to the crystalline rock. The rind consists of rounded plagioclase, pyroxene, and olivine crystals with interstitial melt. In some locations, the rounded crystals are surrounded by closely-packed, blade-like crystals, <5 µm in width. These results indicate that the crystalline interior has partially melted where in contact with the high-temperature impact melt and while further investigation is needed, pyroxene may have preferentially melted relative to olivine and plagioclase. Future Work: We plan to conduct electron backscatter diffraction (EBSD) mapping in order to determine crystallinity and crystal orientation. Next using transmission electron microscopy (TEM) data in conjunction with EBSD and EPMA information, we will model the diffusion of moderately volatile elements between the melt and remnant crystals.

A C Stadermann↗

DOE OSTI2014

A Lapping Technique for Metallic, Alpha-Phase, Plutonium: Achieving and Measuring Nano-Meter Roughness and Sub-Micron Flatness

There are various processes and techniques by which one can achieve well polished (highly reflective) and smooth, flat (low roughness) surfaces on a wide variety of materials. Historically, precision lapping processes were first applied to optical materials for the production of lenses for telescopes and microscopes. These processes have been developed by a multitude of technicians over the centuries and reported in countless publications. These same grinding, lapping and polishing processes have been of great importance in the fabrication and structural characterization of countless optical materials and engineering structures, e.g. optics, Si wafers, precision machined surfaces, engineered devices, low-friction surfaces, mechanical systems, metallographic examination of microstructures, to name but a few. The development of lapping and polishing processes and techniques as applied to extremely hazardous and highly (chemically) reactive materials, such as metallic plutonium (Pu), has been limited. This is due in part due to the sensitive nature of the work as applied to nuclear applications, and limited access and need to work with these materials. For the limited information regarding polishing and lapping of Pu materials that has been documented, there has been virtually no quantitative assessment of qualities such as surface roughness and flatness on the nanometer scale. In this report we use the word “lapping” to refer to the traversing of a specimen surface across an abrasive surface in a controlled manner in order to achieve smooth/flat surfaces. We differentiate lapping from polishing, in that we define polishing as traversing of a sample surface across a non-abrasive surface that contains loose abrasive particles, e.g. diamond paste on nylon nap, in order to achieve a highly reflective surface. In this report, we will detail a simple and repeatable lapping process as applied to alpha-phase metallic Pu. We will provide quantitative measurements of the surface roughness and flatness. We will demonstrate the ability to achieve sub-10 nm surface roughness and to lap millimeter-size areas to a flatness of approximately 1.0 µm. Additionally, we will assess the current limitations and discuss any artifacts that arise as a result of our polishing processes applied to metallic Pu materials.

36 MATERIALS SCIENCE↗

NASA NTRS1972

Review of methods used in lunar organic analysis - Extraction and hydrolysis techniques.

Extraction, hydrolysis, and crushing procedures have been useful in discovering some of the carbon compounds in lunar samples from the Apollo 11 and 12 missions. The nonaqueous solvent system used mostly in lunar sample work has been benzene:methanol. Two methods of extraction have been sonication and Soxhlet extraction, sonication appearing to be the preferred method. Extraction of lunar samples with water and acid hydrolysis of the water extract has proved to be the best method in the search for amino acids or their precursors. Direct acid hydrolysis of lunar samples provided evidence for the presence of carbides or carbide-like materials in lunar surface samples. Hydrolysis of lunar samples with DF, DC1, and NaOD has shown that methane and ethane are indigenous to the moon.

Kvenvolden, K. A.↗

NASA NTRS1974

A mass spectrometric system for analyzing thermal desorption spectra of ion-implanted argon and cesium in tungsten

A mass spectrometric system for determining the characteristics of materials used in instrumental development and aerospace applications was developed. The desorption spectra of cesium that was ion-implanted into polycrystalline tungsten and the effects on the spectra of bombardment of the tungsten by low energy (70 eV) electrons were investigated. Work function changes were measured by the retarding potential diode method. Flash desorption characteristics were observed and gas-reaction mechanisms of the surface of heated metal filaments were studied. Desorption spectra were measured by linearly increasing the sample temperature at a selected rate, the temperature cycling being generated from a ramp-driven dc power supply, with the mass spectrometer tuned to a mass number of interest. Results of the study indicate an anomolous desorption mechanism following an electron bombardment of the sample surface. The enhanced spectra are a function of the post-bombardment time and energy and are suggestive of an increased concentration of cesium atoms, up to 10 or more angstroms below the surface.

Wood, G. M., Jr.↗