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At least 685 records · Page 38
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Melting rate correlation with batch properties and melter operating conditions during conversion of nuclear waste melter feeds to glasses

The rate of conversion of nuclear waste melter feed to glass is affected by the selection of melter feed materials and by melter design and operation. The melting rate correlation (MRC) is an equation that relates the glass production rate with two types of variables: (1) feed and melt properties: conversion heat, cold-cap bottom temperature, and glass melt viscosity; and (2) melter design and operation parameters: melter geometry, melter operating temperature, and gas bubbling rate. The MRC shows good agreement for an extended melting-rate data set of high-level waste (HLW) melter feeds and a data set generated for low-activity waste (LAW) melter feeds. Laboratory observation of heated melter feed samples is often used to assess the cold-cap bottom temperature of HLW melter feeds (moderately foaming feeds), but this technique appears inadequate for LAW melter feeds (vigorously foaming feeds). For LAW feeds, an adequate assessment of the cold-cap bottom temperature was achieved using evolved gas analysis, which allows identification of the collapse of primary foam for oxidized feeds. This assessment shows that the cold-cap bottom temperature for vigorously foaming LAW feeds is higher than that for moderately foaming HLW feeds. When the results of MRC are compared, LAW feeds are generally less sensitive to the bubbling rate and melt viscosity, and more sensitive to the cold-cap bottom temperature than HLW feeds. The MRC qualifies as a promising tool to support the selection of melter feed materials and melter operating conditions, which is determined from expensive independent scaled melter experiments, and sophisticated mathematical models.

Lee, Seung Min↗
DOE OSTI2018

Characterization of Electrospray Ionization (ESI) Parameters on In-ESI Hydrogen/Deuterium Exchange of Carbohydrate-Metal Ion Adducts

The conformations of glycans are crucial for their biological functions. In-electrospray ionization (ESI) hydrogen/deuterium exchange-mass spectrometry (HDX-MS) is a promising technique for studying carbohydrate conformations since rapidly exchanging functional groups, e.g., hydroxyls, can be labeled on the timeframe of ESI. However, regular application of in-ESI HDX to characterize carbohydrates requires further analysis of the in-ESI HDX methodology. For instance, in this method, HDX occurs concurrently to the analyte transitioning from solution to gas-phase ions. Therefore, there is a possibility of sampling both gas-phase and solution-phase conformations of the analyte. Herein, we differentiate in-ESI HDX of metal-adducted carbohydrates from gas-phase HDX and illustrate that this method analyzes solvated species. We also systematically examine the effects of ESI parameters, including spray solvent composition, auxiliary gas flow rate, sheath gas flow rate, sample infusion rate, sample concentration, and spray voltage, and discuss their effects on in-ESI HDX. Further, we model the structural changes of a trisaccharide, melezitose, and its intramolecular and intermolecular hydrogen bonding in solvents with different compositions of methanol and water. These molecular dynamic simulations support our experimental results and illustrate how an individual ESI parameter can alter the conformations we sample by in-ESI HDX. Overall, this work illustrates how the fundamental processes of ESI alter the magnitude of HDX for carbohydrates and suggest parameters that should be considered and/or optimized prior to performing experiments with this in-ESI HDX technique.

Carbohydrate Conformation↗
DOE OSTI2019

Identification of Porphyrin-Silica Composite Nanoparticles using Atmospheric Solids Analysis Probe Mass Spectrometry

Porphyrins are critical pigments involved in biological energy transduction processes. Their abilities to absorb light, then convert it to energy, have raised the interest of using porphyrin nanoparticles as photosensitizers in photodynamic therapy. A current study showed that self- assembled porphyrin-silica composite nanoparticles can selectively destroy tumor cells, but detection of the cellular uptake of porphyrin-silica composite nanoparticles was limited to imaging microscopy. In this work, we developed a novel method to rapidly identify porphyrin-silica composite nanoparticles using Atmospheric Solids Analysis Probe-Mass Spectrometry (ASAP-MS). ASAP-MS can directly analyze complex mixtures without the need for sample preparation. Porphyrin-silica composite nanoparticles were vaporized using heated nitrogen desolvation gas, and their thermo-profiles were examined to identify distinct mass- to-charge (M/Z) signatures. HeLa cells were incubated in growth media containing the nanoparticles, and after sufficient washing to remove residual nanoparticles, the cell suspension was loaded onto the end of ASAP glass capillary probe. Upon heating, HeLa cells were degraded and porphyrin-silica composite nanoparticles were released. Vaporized nanoparticles were ionized and detected by MS. Furthermore, the cellular uptake of porphyrin-silica composite nanoparticles was identified using this ASAP-MS method.

36 MATERIALS SCIENCE↗
NASA NTRS1984

Preparation and cleanliness verifications of a space simulation chamber for contamination sensitive test specimens

Contamination sensitive optical devices were to be evaluated under thermal vacuum conditions. Test specifications called for an extremely clean chamber environment, ambient temperature chamber walls, and optical surface temperatures at approximately - 30 C. Chamber preparation included the replacement of diffusion pumps with cryopumps and the cleaning of the chamber walls to reduce contamination levels. Chamber cleaning using vacuum bake was tried and abandoned as time consuming and ineffective. Chemical cleaning and cleanliness verification methods were developed. Gas chromatograph analysis techniques were used extensively throughout the cleaning process to verify cleanliness levels prior to evacuating the chamber. A chamber cleanliness verification test using a thermoelectric quartz crystal microbalance and witness samples was performed to demonstrate that an appropriate cleanliness level was achieved.

Koch, W. R.↗
NASA NTRS2018

Constraining Upper Troposphere/Lower Stratosphere Aerosol Physical Processes with High-Altitude Aircraft Measurements

Interest in a more complete understanding of the sources, composition and microphysics of stratospheric aerosol particles has intensified during recent years for several reasons: (1) small volcanic eruptions have been recognized as a driver of short-term changes in climate forcing; (2) emissions of sulfur dioxide (SO2) and other aerosol precursors have shifted to south Asia and other low latitude regions with intense vertical transport; (3) organic material has been recognized as a key contributor to lower stratospheric aerosol mass; and (4) interest in possible solar radiation management (geoengineering) through significant enhancements in stratospheric aerosols has intensified. To address stratospheric aerosol science issues, we are proposing a NASA Earth Ventures mission to NASA to provide extensive high-altitude aircraft measurements of critical gas-phase and aerosol properties at multiple locations across the planet. In this presentation, we will discuss the objectives of the proposed campaign, the measurements provided, the sampling strategy, and the modeling and analysis approaches that would be used to address specific science questions.

Jensen, Eric↗
NASA NTRS2010

Detection of Cometary Amines in Samples Returned by the Stardust Spacecraft

The delivery of amino acids to the early Earth by comets and their fragments could have been a significant source of the early Earth's prebiotic organic inventory that led to the emergence of life (Chyba and Sagan, 1992). Over 20 organic molecules including methane, ethane, ammonia, cyanic acid, formaldehyde, formamide, acetaldehyde, acetonitrile, and methanol have been identified by radio spectroscopic observations of the comae of comets Hale-Bopp and Hyakutake (Crovisier et al. 2004). These simple molecules could have provided the organic reservoir to allow the forn1ation of more complex prebiotic organic compounds such as amino acids. After a 7 -year mission, the Stardust spacecraft returned to Earth samples from comet Wild 2 on January 15, 2006 providing the opportunity to analyze the organic composition and isotopic distribution of cometary material with state-of-the-art laboratory instrun1entation. The Preliminary Examination Team analyses of organics in samples returned by Stardust were largely focused on particles that impacted the collector aerogel and aluminum foil (Sandford et al. 2006). However, it is also possible that Stardust returned a "diffuse" sample of gas-phase organic molecules that struck the aerogel directly or diffused away from the grains after impact. To test this possibility, samples of Stardust flight aerogel and foil were carried through a hot water extraction and acid hydrolysis procedure to see if primary amine compounds were present in excess of those seen in controls. Here we report highly sensitive liquid chromatography time-of-flight mass spectron1etry measurements of amino acids and amines in samples returned from a comet (Glavin et al. 2008). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. However, the enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (1 to 2) that are distinct from preflight aerogels (7 to 10), suggest that these amines were captured from Wild 2. It is possible that MA and EA were formed on energetically processed icy grains containing methane, ethane, and ammonia. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of pre biotic organics on the early Earth. To better understand their origin, a systematic compound specific carbon isotopic analysis (C-CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GC-QMS/IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of amino acids extracted from Stardust samples.

Glavin, Daniel P.↗
NASA NTRS1990

Circumnuclear molecular gas in starburst and Seyfert galaxies

In order to investigate circumnuclear molecular gaseous contents and their relation to the nuclear activity, researchers made a search for circumnuclear (12)CO (J=1-0) emission from 28 starburst-nucleus galaxies (SBNs) and 12 Seyfert galaxies with the recession velocities less than 5000 km/s, using the Nobeyama Radio Observatory 45-m telescope. The full half-power beam width of 17 arcsec covers a region of less than about 5 kpc in diameter for the sample galaxies. The circumnuclear CO emission was detected from twelve SBNs (one is marginal) and four Seyfert galaxies. The main results and conclusions are summarized. Researchers derived the circumnuclear surface density of molecular gas which is corrected for inclination of the galaxies. This analysis shows that the surface density spans a wide range over two orders of magnitude. Further, there is no significant difference in the surface densities between types 1 and 2 Seyfert galaxies. Thus, we may conclude that the circumnuclear molecular content is not a key parameter producing the dichotomy of the Seyfert galaxies. It is also shown that there is no significant difference in the circumnuclear surface densities of molecular gas among the Seyfert, starburst, and normal galaxies. This implies that the circumnuclear gaseous content is not a key parameter determining which activity occurs in nuclei. We may conclude that more centrally condensed (i.e., less than 10 - 100 pc in diameter) gas components play an essential role on the occurrence of nuclear activities. Comparing results with the previous ones, researchers deduced radial distribution of surface density of molecular gases. They cannot obtain evidence for strong central concentration of molecular gas in the sample Seyfert galaxies except for NGC 3227. This is consistent with the previous result by Blitz, Mathieu, and Bally (1986). Comparing the CO emission line profiles with the previous ones taken with the larger beams, researchers discovered circumnuclear components of molecular gases. In particular, they found that molecular gas clouds may be absent in the SE of the nucleus of NGC 7469 where the high-excitation emitting region is discovered by Heckman et al. (1986). It is suggested that the nuclear activity (strong radiation and/or wind) may destruct the molecular clouds in that region.

Taniguchi, Yoshiaki↗
DOE OSTI2024

Large-Volume Injection and Assessment of Reference Standards for n -Alkane δD and δ 13 C Analysis via Gas Chromatography Isotope Ratio Mass Spectrometry

Compound-specific stable isotope analysis of hydrogen (δD) and carbon (δ 13 C) in organic compounds is a valuable tool in biogeochemical research. A key limitation of this method is the relatively large amount of sample required to achieve desirable precision. We developed a large-volume (20 μL) injection method that allows for high throughput analysis of less concentrated samples and tested it for δ 13 C and δD measurements of n-alkanes. We also conducted a comparison of reference standards and assessed several methods to normalize and correct n-alkane δD and δ13C measurements. The mean precision of the δD method based on 233 environmental n-alkane samples (two to three replications per sample) is 4.0‰ (1σ, estimated from the weighted mean of the pooled unbiased standard deviations) and 0.46‰ (1σ) for δ 13 C from 37 environmental samples (two to three replications per sample). The evaluation of reference standards shows that the use of n-alkane standards with large offsets in δD values in adjacent n-alkane chains can lead to biases in measurement correction. The large-volume injection method shows good reproducibility of δ 13 C and δD measurements of n-alkanes and reduces the required sample concentration by about 80%. We propose that for δD measurements, a reference standard set should be used in which each reference standard has a limited range of δD values and no adjacent n-alkane chains, to minimize memory effects.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1987

Rare gas analysis of size fractions from the Fayetteville meteorite

Eight size separates of grains from the Fayetteville meteorite ranging from less than 20 microns to greater than 1 millimeter are being analyzed for their rare gas elemental and isotopic composition. Measurements on five samples were performed. All five reveal a mixture of solar, planetary, cosmic ray produced and radiogenic gases. The solar component is of particular interest since it suggest that the meteorite may represent a fragment of an ancient protoplanetary regolith which was exposed to the solar wind. Solar wind elements are implanted in the outer few hundred Angstroms of exposed grains and are therefore expected to be surface correlated. At present the data do not suggest that such a correlation exists, but the final conclusion must await further analyses and data reduction.

Jordan, Jim L.↗
NASA NTRS1970

Analysis of the F-1 Acoustic Liner

An analytical study was performed to re-evaluate data obtained during the F-1 Acoustic Absorber program. The acoustic liner had failed to produce substantial improvements in stability. Oscillatory-pressure, temperature and gas sampling data obtained from liner firings were employed to calculate the damping produced by the liner and the potential for increasing the damping by varying the liner dimensions. The results indicate the damping can be substantially increased. The liner damping was predicted by calculating temporal damping-coefficient contributions due to the liner.

Oberg, C. L.↗
DOE OSTI2024

Proof-of-concept chemometric approach for environmental forensic sourcing of crude oil samples using SPME-GC-MS

Environmental exposure to crude oil through seepage and spillage poses risks to the immediate environment and the broader ecosystem as areas along the oil distribution path are affected by the influx of crude petroleum as well as the environmental, economic, and civil unrest that accompanies it. There is a large financial burden associated with the lost resources, including the cost of rehabilitation, and the affected sources of revenue for communities affected by oil spills. As such, it is crucial to determine the responsible parties. This work outlines an environmental forensics approach to determining the source of an un-weathered crude oil sample. The researchers employed solid phase microextraction coupled with gas chromatography mass spectrometry (SPME-GC-MS) to capture and analyze the gaseous components emitted by crude oil samples sourced from five locations. Samples were analyzed using Spearman's rank correlation and 3D covariance analysis. Both chemometric approaches yielded optimal performance results with no misclassifications, true positive rate (TPR) = 100 % and false positive rate (FPR) = 0 %. The similarity metrics calculated by each test noted clear delineations between the values of same-source and differently sourced samples. The Spearman's rank correlation test and 3D covariance calculations both demonstrated the ability to correctly identify sample source origin in this dataset. Finally, the authors outline an approach to the future application of these tests and suggest their joint use in future crude oil sourcing endeavors.

3D covariance mapping↗
DOE OSTI2017

Investigation of the influence of electron irradiation on the properties of cobalt nanotubes

Cobalt nanotubes have been synthesized by electrochemical deposition in pores of ion track membranes. The structures obtained have been studied by scanning electron microscopy, energy-dispersive spectroscopy, X-ray diffraction analysis, and gas permeability method. The influence of electron irradiation on the cobalt nanotube structure has been investigated. It is shown that an increase in the irradiation dose leads to the transformation of the sample crystal structure. This fact can be explained by the simultaneous reduction of the β-Co metastable phase and relaxation of the microstress formed by the fcc phase in the lattice. The degree of sample texturing along the [100] direction increases under electron irradiation. The dependences of the resistive and magnetic properties of cobalt nanotubes on the irradiation dose have been analyzed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2021

Reference document for LANL stack sampling and ANSI N13.1 (Article) Gielow RL and McNamee MR 1993. Numerical Flue Gas Flow Modeling for Continuous Emissions Monitoring Applications. EPRI CEM Users Group Meeting. Baltimore. RP1961-13

American National Standard N13.1 “sets forth guidelines and performance criteria for sampling the emissions of airborne radioactive substances in the air discharge ducts and stacks of nuclear facilities. Emphasis is on extractive sampling from a location in a stack or duct where the contaminant is well mixed. At such a location, sampling may be conducted at a single point. This standard provides performance-based criteria for the use of air sampling probes, transport lines, sample collectors, sample monitoring instruments, and gas flow measuring methods. This standard also covers sampling program objectives, quality assurance issues, developing air sampling action levels, system optimization, and system performance verification. Workplace, containment, and environmental air monitoring are not addressed. Specific sample analysis methods and the reporting or interpreting of results are also not addressed.” (HPS 2011).

61 RADIATION PROTECTION AND DOSIMETRY↗
NASA NTRS2013

Detection of Reduced Nitrogen Compounds at Rocknest Using the Sample Analysis At Mars (SAM) Instrument on the Mars Science Laboratory (MSL)

The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected nitrogen-bearing compounds during the pyrolysis of Rocknest material at Gale Crater. Hydrogen cyanide and acetonitrile were identified by the quadrupole mass spectrometer (QMS) both in direct evolved gas analysis (EGA). SAM carried out four separate analyses from Rocknest Scoop 5. A significant low temperature release was present in Rocknest runs 1-4, while a smaller high temperature release was also seen in Rocknest runs 1-3. Here we evaluate whether these compounds are indigenous to Mars or a pyrolysis product resulting from known terrestrial materials that are part of the SAM derivatization.

Sample Analysis at Mars↗
NASA NTRS2017

Documenting Surface and Sub-surface Volatiles While Drilling in Frozen Lunar Simulant

NASA's Resource Prospector (RP) mission is intended to characterize the three-dimensional nature of volatiles in lunar polar regions and permanently shadowed regions. RP is slated to carry two instruments for prospecting purposes. These include the Neutron Spectrometer System (NSS) and Near-Infrared Volatile Spectrometer System (NIRVSS). A Honybee Robotics drill (HRD) is intended to sample to depths of 1 m, and deliver a sample to a crucible that is processed by the Oxygen Volatile Extraction Node (OVEN) where the soil is heated and evolved gas is delivered to the gas chromatograph / mass spectrometer of the Lunar Advanced Volatile Analysis system (LAVA). For several years, tests of various sub-systems have been undertaken in a large cryo-vacuum chamber facility (VF-13) located at Glenn Research Center. In these tests a large tube (1.2 m high x 25.4 cm diameter) is filled with lunar simulant, NU-LHT-3M, prepared with known abundances of water. There are thermo-couples embedded at different depths, and also across the surface of the soil tube. The soil tube is placed in the chamber and cooled with LN2 as the pressure is reduced to approx.5-6x10(exp -6) Torr. Here we discuss May 2016 tests where two soil tubes were prepared and placed in the chamber. Also located in the chamber were 5 crucibles, an Inficon mass spectrometer, and a trolly permitting x-y translation, where the HRD and NIRVSS, were mounted. The shroud surrounding the soil tube was held at different temperatures for each tube to simulate a warm and cold lunar environment.

Oxygen Volatile Extraction Node↗
DOE OSTI2018

Quantitative analysis of changes in antioxidant in crosslinked polyethylene (XLPE) cable insulation material exposed to heat and gamma radiation

Quantitative analysis of the antioxidant poly(1,2-dihydro-2,2,4-trimethylquinoline) (pTMQ) was conducted on pristine, thermally-aged, and gamma radiation-aged commercial cross-linked polyethylene-(XLPE-)based cable insulation material aged at temperatures 60, 90, and 115?°C, with gamma radiation exposure dose rates of 0, 120, 300, and 540?Gy/h for 15 days. The quantification of antioxidant was performed using pyrolysis gas chromatography-mass spectrometry (Py-GCMS). Oxidation induction time (OIT) was measured using differential scanning calorimetry (DSC) and correlation was made between the quantified depletion of antioxidant and measured OIT. It was observed that, in the case of isothermal aging, the quantity of antioxidant and OIT decreased with increasing gamma radiation dose. In the case of samples exposed to the same gamma radiation dose, the quantity of antioxidant and OIT were observed to decrease with increasing aging temperature. Depletion in the quantity of antioxidant relative to that in the pristine material ranged from 7 to 93% for differently aged samples. The measured decline in OIT ranged from 0 to 80%. Change in the quantity of antioxidant in the material was observed to follow the same trend as the change in OIT when the samples were aged under various conditions. The observations are explained in terms of the reaction between the antioxidant and free radicals created during exposure of the samples to thermal and gamma radiation.

Pyrolysis gas chromatography-mass spectroscopy, an↗
DOE OSTI2024

Pore-scale visualization of natural hydrate-bearing sediments

Accurate modeling of gas hydrate reservoir productivity and geomechanical risks associated with subsurface dissociation of natural gas hydrates (NGH) requires the determination of model parameters through physical testing on natural hydrate-bearing sediments (HBS). This involves investigating the hydro-mechanical behavior of undisturbed hydrate samples from nature under in situ conditions using pressure core characterization and analysis, which provides a unique opportunity for research. By employing state-of-the-art micro computed tomography imagery on cryogenically preserved, hydrate-bearing sediment samples, we can determine hydrate saturation as well as permeability with and without the presence of hydrates in the sediment. Furthermore, utilizing a machine learning based image segmentation technique, it is possible to extract pore space and grain information. Subsections of the entire image volume were used to determine anisotropic permeabilities using a finite-difference method Stokes solver (FDMSS). Additionally, permeability measurements on whole pressure and temperature preserved hydrate-bearing core were analyzed by utilizing the National Energy Technology Laboratory’s (NETL) Pressure Core Characterization and X-ray CT Visualization Tool (PCXT) to manipulate, cut, and analyze pressure preserved sediment. Permeabilities were measured under a broad range of vertical stress states to simulate expected pressure changes during production scenarios, and the results show that permeabilities derived from images are in agreement with those from traditional core derived experiments. The collected stress-dependent permeability, permeability anisotropy, and corresponding gas hydrate saturations provide valuable input into numerical simulations of reservoir productivity. These properties have been proven to be key parameters determining a long-term reservoir response under depressurization.

Liu, Mengwei [Oak Ridge Institute for Science and ↗