Results for “SAMPLING” — Page 32

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2025

Develop Accurate Techniques for Passive SiC Temperature Monitoring of Miniature Samples for Cross-Cutting Applications

Passive thermometry is critically important because most fuels and materials irradiation experiments are not instrumented, and it is necessary to understand the irradiation temperature to properly interpret any post-irradiation examination data, including evolving properties and/or microstructures. The standard passive thermometry approach uses continuous dilatometry to evaluate changes in the instantaneous coefficient of thermal expansion during post-irradiation thermal annealing. This approach has limitations in terms of sample size (minimum length requirements) and the maximum irradiation temperature that can be accurately determined, which is limited by the reduced swelling (and therefore recovery) following higher temperature irradiation and limitations on the furnaces used with push-rod dilatometers. This work evaluates two new proposed techniques for post-irradiation evaluation of passive SiC temperature monitors: differential scanning calorimetry (DSC) and Raman spectroscopy. DSC is an extremely sensitive technique that can be used for any specimen geometry and is capable of higher temperature operation. Raman spectroscopy is similar in that it is a surface technique capable of examining extremely small samples (submillimeter), can be used with a heated stage up to 1,500°C (planned for future work), and is capable of mapping local irradiation temperatures throughout a sample. Existing SiC samples that were previously irradiated over a wide range of temperatures were cut into multiple pieces to allow for annealing studies using multiple different techniques: dilatometry, DSC, and Raman spectroscopy. This approach mitigates the concern that samples analyzed using one technique may have a slightly different irradiation history than those analyzed using a different technique. Recovery was clearly observed during annealing using both DSC and dilatometry. In some cases, a direct comparison could not be made due to some of the DSC runs accidentally including material from multiple specimens and issues with using an alternative DSC sample holder for the highest temperature annealing studies. Nevertheless, one trend was clear: the DSC runs resulted in higher irradiation temperatures compared to those of the dilatometry runs. Part of this could be attributed to the higher temperature ramp rates used during the DSC runs, which are often preferred to reduce noise in the measurements. By comparison, dilatometry has previously been shown to produce better data at lower ramp rates. Future work should further investigate the ideal ramp rate for both techniques to produce consistent results. Additional work should evaluate the best holder material to use for DSC runs exceeding 1,000°C to provide reliable data while preventing interactions between SiC and the holder.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Genomic-based biosurveillance for avian influenza: whole genome sequencing from wild mallards sampled during autumn migration in 2022–2023 reveals a high co-infection rate on migration stopover site in Georgia

The Caucasus region, including Georgia, is an important intersection for migratory waterbirds, offering potential for avian influenza virus (AIV) transmission between populations from different geographic areas. In 2022 and 2023, wild ducks were sampled during autumn migration events in Georgia to study the genetic relationships and molecular characteristics of influenza strains. Sequencing and phylogenetic analysis were used to compare the sampled strains to reference sequences from Africa, Asia, and Europe, allowing assessment of genetic relationships and virus transmission between migratory birds. Protein language modeling identified potential co-infections. Of 225 duck samples, 128 tested positive for the influenza M gene. 55 influenza-positive samples underwent whole-genome sequencing, revealing significant diversity. Analysis of the hemagglutinin (HA) segment showed notable differences among subtypes. Most samples were H6N1 and H6N6, but co-infections with combinations like H6H3, N8N1, N6H9, N2N6, and H9H6/N1N2 were also identified. These findings demonstrate the high variability of influenza viruses in migratory waterbirds in Georgia, including a notable rate of co-infections. Some samples exhibited uncommon genetic characteristics compared to other strains from the same year, suggesting Georgia’s role as a mixing vessel for influenza viruses. This facilitates reassortment during co-infections and contributes to the genetic diversity observed across flyways.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2024

Transmission electron microscopy of ion irradiated ODS MA956 samples

Oxide dispersion strengthened (ODS) alloys are promising candidate materials for the next generation advanced nuclear reactors due to their superior irradiation resistance and mechanical properties. To better understand the effect of irradiation on MA956, it is essential to study higher dose (50-100 dpa) samples, so that the general trend of microstructural evolution and the resulting radiation-hardening can be deduced. Currently, ion irradiations are considered the only way to achieve doses beyond ~50 dpa in a practical time frame relevant to alloy and welding development programs. This dataset contains TEM characterization results of ODS MA956 samples that were ion irradiated under different conditions: Sample #5 (1.25 dpa at 190℃); Sample #9 (50 dpa at 190℃); Sample #15 (1.25dpa under 320℃); and Sample 17 (25 dpa at 320℃). TEM characterization focused on the irradiation induced defects (dislocation lines and loops) using the on-zone axis bright field STEM technique. These data were collected using a FEI Tecnai G2 F30 S/TEM at Microscopy and Characterization Suite (MaCS) at Center for Advanced Energy Studies (CAES), Idaho Falls, ID. This project (ion irradiation and TEM studies) was supported by the U.S. Department of Energy, Office of Nuclear Energy under DOE Idaho Operations Office Contract DE-AC07-05ID14517 as part of Nuclear Science User Facilities award #18-14784 (PI: Ramprashad Prabhakaran, PNNL).

Prabhakaran, Ramprashad↗

DOE OSTI2024

TRAC Time Tags of individual particle samples collected for microscopy analysis at RMBL [AMF2] from June 2023 to August 2023

The dataset presents the time tags of individual particle samples collected on microscopy substrates during the Surface Atmosphere Integrated Field Laboratory (SAIL) campaign in Gothic, CO. A Time Resolved Aerosol Collector was deployed at the Rocky Mountain Biological Laboratory, 200 m north of AMF2 to collect ambient particles. The instrument inlet was placed 5 m above ground level. Particles are deposited on 400 mesh copper carbon-B film TEM grids (Ted Pella 01814-F). Samples are sealed and currently stored at Purdue University. A subset of the samples can be shared. Please contact dataset authors for more information. The dataset reports the sample start times in UTC and MST along with the sample ID, used to guide its location and retrieval from the storage plate. TRAC sampling started on June 17, 2023, and ended on July 31, 2023.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS1972

Chemical features of the Luna 16 regolith sample.

The Luna 16 regolith sample differs from Apollo 11, 12 and 14 regolith and basalt samples by having smaller negative Eu and Sr anomalies and nearly chondritic Eu/Sm and Eu/Sr ratios although the overall REE, Ba, Sr and U concentrations are 25 to 45 times chondrites. Major element data, in particular FeO vs Al2O3, show that the Luna 16 regolith sample is composed of materials that follow a quantitatively different Fe/Al variation than do Apollo 11, 12, 14 and 15 samples. The small Eu and Sr anomalies and the displaced Fe/Al variation are two chemical features unique to the Luna 16 regolith sample. The Luna 16 regolith sample can contain little if any of the rock types abundant at Apollo sites, thus indicating that the unique chemical features are typical of local or nearby materials and indicate a separate petrogenetic province for major component rock types of the Luna 16 regolith.

Hubbard, N. J.↗

NASA NTRS1972

Sampling functions for geophysics

A set of spherical sampling functions is defined such that they are related to spherical-harmonic functions in the same way that the sampling functions of information theory are related to sine and cosine functions. An orderly distribution of (N + 1) squared sampling points on a sphere is given, for which the (N + 1) squared spherical sampling functions span the same linear manifold as do the spherical-harmonic functions through degree N. The transformations between the spherical sampling functions and the spherical-harmonic functions are given by recurrence relations. The spherical sampling functions of two arguments are extended to three arguments and to nonspherical reference surfaces. Typical applications of this formalism to geophysical topics are sketched.

Giacaglia, G. E. O.↗

NASA NTRS1972

Nuclear magnetic resonance properties of lunar samples.

Nuclear magnetic resonance spectra of Na-23, Al-27, and P-31 in fines samples 10084,60 and 14163,168 and in crystalline rock samples 12021,55 and 14321,166, have been recorded over a range of frequencies up to 20 MHz. A shift in the field at which maximum absorption occurs for all of the spectra relative to the field at which maximum absorption occurs for terrestrial analogues is attributed to a sample-dependent magnetic field at the Na, Al, and P sites opposing the laboratory field. The magnitude of these fields internal to the samples is sample dependent and varies from 5 to 10 G. These fields do not correlate with the iron content of the samples. However, the presence of single-domain particles of iron distributed throughout the plagioclase fraction that contains the principal fraction of Na and Al is inferred from electron magnetic resonance spectra shapes.

Kline, D.↗

NASA NTRS1972

Dielectric properties of Apollo 14 lunar samples.

Laboratory characterization of dielectric properties of lunar samples 14301,41, 14310,75, 14318,30 and 14321,163 is made. Our measurements of dielectric constants and losses were made over a range of frequency from 100 Hz to 10 MHz and temperature from 77 to 473 K by two-terminal capacitance substitution methods. The dielectric behavior of these samples is generally similar to other lunar samples from Apollo 11 and Apollo 12 sites when these samples are free from absorbed moisture. As did sample 12002,58, sample 14310,75 showed a distinctive dispersion that may be associated with the presence of water, and different values of the activation energy for conduction as the temperature was varied. The activation energies range from about 0.03 to 0.5 eV.

Chung, D. H.↗

NASA NTRS1974

Nondestructive activation analysis of sample of lunar surface material returned by Luna 16 automatic station

The composition of a sample of lunar surface material returned by the Luna 16 automatic station from the Sea of Fertility was studied, using nondestructive activation analysis. The structure of the returned surface material is inhomogeneous; the surficial material is thin, quite homogeneous, and the granularity increases with depth. Based on grain size, the sample was separated into five zones. The activation analysis was conducted on a sample taken from the friable surficial layer, zone A. The content of Al, Mn, Na, Cr, Co, Fe, and Sc was determined by nondestructive activation analysis of the sample. In determining Cr, Co, Fe, and Sc, the sample was irradiated for 24 hours and cooled for 10 days. Gamma spectra of the samples were recorded with a semiconductor Ge(Li)-detector and a multichannel analyzer, and measurement data were processed with an electronic computer.

Chayko, M.↗

NASA NTRS1975

Test evaluation of potential heatshield contamination of an outer planet probe's gas sampling system

The feasibility of retaining the heat shield for outer planet probes was investigated as a potential source of atmospheric sample contamination by outgassing. The onboard instruments which are affected by the concept are the pressure sensor, temperature sensor, IR detector, nephelometer, and gas sampling instruments. It was found that: (1) The retention of the charred heatshield and the baseline atmospheric sampling concepts are compatible with obtaining noncontaminated atmospheric samples. (2) Increasing the sampling tube length so that it extends beyond the viscous boundary layer eliminates contamination of the atmospheric sample. (3) The potential for contamination increases with angle of attack.

Kessler, W. C.↗

NASA NTRS1977

A high pressure modulated molecular beam mass spectrometric sampling system

The current state of understanding of free-jet high pressure sampling is critically reviewed and modifications of certain theoretical and empirical considerations are presented. A high pressure, free-jet expansion, modulated molecular beam, mass spectrometric sampling apparatus was constructed and this apparatus is described in detail. Experimental studies have demonstrated that the apparatus can be used to sample high temperature systems at pressures up to one atmosphere. Condensible high temperature gaseous species have been routinely sampled and the mass spectrometric detector has provided direct identification of sampled species. System sensitivity is better than one tenth of a part per million. Experimental results obtained with argon and nitrogen beams are presented and compared to theoretical predictions. These results and the respective comparison are taken to indicate acceptable performance of the sampling apparatus. Results are also given for two groups of experiments related to hot corrosion studies. The formation of gaseous sodium sulfate in doped methane-oxygen flames was characterized and the oxidative vaporization of metals was studied in an atmospheric pressure flowing gas system to which gaseous salt partial pressures were added.

Stearns, C. A.↗

NASA NTRS1976

The surface chemical composition of lunar samples and its significance for optical properties

The surface Fe, Ti, Ca, and Si concentrations in a variety of soil and rock samples from all the Apollo sites are determined using an Auger spectrometer plus a single-pass cylindrical-mirror analyzer with a standard 15-stage BeCu electron multiplier. It is found that there are no great differences between the surface and bulk concentrations of any of the four elements in the rock samples, but the surface Fe and Ti concentrations in soil samples are higher than the bulk concentrations. Results are also reported for solar-wind simulation experiments in which a pulverized rock sample was bombarded with 2-keV alpha-particles corresponding to about a 30,000-yr dose of the solar-wind proton component. These results indicate that the chemical change induced on the surface of a rock powder by positive-ion bombardment is similar to the change from bulk to surface chemical composition in lunar soil samples. A clear correlation is observed between the surface Fe concentration and albedo of the soil samples.

Gold, T.↗

NASA NTRS1978

Apollo 14 rock samples

Petrographic descriptions of all Apollo 14 samples larger than 1 cm in any dimension are presented. The sample description format consists of: (1) an introductory section which includes information on lunar sample location, orientation, and return containers, (2) a section on physical characteristics, which contains the sample mass, dimensions, and a brief description; (3) surface features, including zap pits, cavities, and fractures as seen in binocular view; (4) petrographic description, consisting of a binocular description and, if possible, a thin section description; and (5) a discussion of literature relevant to sample petrology is included for samples which have previously been examined by the scientific community.

Carlson, I. C.↗

NASA NTRS1979

Determination of trace gases in learjet and U-2 whole air samples collected during the intertropical convergence zone experiment

The contribution of Washington State University (WSU) to the Intertropical Convergence Zone (ITCZ) study, conducted in the Panama Canal Zone in July 1977 is reported. The ITCZ program had the objective to study the meteorology and air chemistry to determine, if possible, the magnitude of injection of tropospheric air into the stratosphere in the ITCZ. WSU was responsible for two phases of the air chemistry program for the ITCZ study: (1) the collection of whole-air samples from ground level to 13.7 km using a Learjet as a sampling platform, and the analysis of the samples for selected halocarbons, C2 hydrocarbons, N2O, and SF6; and (2) the analysis for selected halocarbon species and N2O of low pressure whole-air samples, collected between 13.7 km and 21.3 km by a U-2 aircraft. The report is divided into separate sections describing the Learjet and the U-2 sampling methods, analytical methods, and results. Complete data tables for all samples analyzed are given.

Cronn, D. R.↗

NASA NTRS1981

Mineralogical, optical, geochemical, and particle size properties of four sediment samples for optical physics research

X-ray diffraction and spectroscopy were used to investigate the mineralogical and chemical properties of the Calvert, Ball Old Mine, Ball Martin, and Jordan Sediments. The particle size distribution and index of refraction of each sample were determined. The samples are composed primarily of quartz, kaolinite, and illite. The clay minerals are most abundant in the finer particle size fractions. The chemical properties of the four samples are similar. The Calvert sample is most notably different in that it contains a relatively high amount of iron. The dominant particle size fraction in each sample is silt, with lesser amounts of clay and sand. The indices of refraction of the sediments are the same with the exception of the Calvert sample which has a slightly higher value.

Bice, K.↗

NASA NTRS1982

Distribution and evolution of Zn, Cd, and Pb in Apollo 16 regolith samples and the average U-Pb ages of the parent rocks

The concentration of surface (low temperature site) and interior (high temperature site) Cd, Zn, and Pb in 13 Apollo 16 highland fines samples, pristine rock 65325, and mare fines sample 75081 were analyzed directly from the thermal release profiles obtained by flameless atomic absorption technique (FLAA). Cd and Zn in pristine ferroan anothosite 65325, anorthositic grains of the most mature fines 65701, and basaltic rock fragments of mare fines 75081 were almost all surface Cd and Zn indicating that most volatiles were deposited on the surfaces of vugs, vesicles and microcracks during the initial cooling process. A considerable amount of interior Cd and Zn was observed in agglutinates. This result suggests that high temperature site interior volatiles originate from entrapment during the lunar maturation processes. Interior Cd found in the most mature fines sample 65701 was only about 15% of the total Cd in the sample. Interior Pb present in Apollo 16 fines samples went up to 60%. From our Cd studies we can assume that this interior Pb in highland fines samples is largely due to the radiogenic decay which occurred after the redistribution of the volatiles took place. We obtained an average age of 4.0 b.y. for the parent rocks of Apollo 16 highland regolith from our interior Pb analyses.

Cirlin, E. H.↗

NASA NTRS1984

Case study of sample spacing in planar near-field measurement of high gain antennas

Far field antenna patterns can be reconstructed from planar near field measurements acquired at a sample spacing of lambda/2 or less. For electrically large antennas, sampling at the Nyquist rate may result in errors due to system electronic drift over long acquisition times. The computer capacity may limit the largest size of the near field data set. The requirement to sample at the Nyquist rate is relaxed for high gain antennas which concentrate most of the radiated energy into a small angular region of the far field. The criteria for sample spacing at greater than lambda/e through the use of a priori information of the antenna radiation characteristics are presented. Far field patterns of a 30 GHz dual offset reflector system with a 2.7 m parabolic main reflector are computed from near field data obtained at sample spacings ranging from 0.1 lambda to 10 lambda. The effects of sampling interval and spectrum cutoff on the far field patterns are discussed.

Acosta, R. J.↗