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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 127 records · Page 7
All sourcesNASA NTRSDOE OSTI
NASA NTRS2022

Compositional Measurements of Saturn's Upper Atmosphere and Rings From Cassini INMS: An Extended Analysis of Measurements From Cassini's Grand Finale Orbits

The Cassini spacecraft's final orbits sampled Saturn's atmosphere and returned surprisingly complex mass spectra from the Ion and Neutral Mass Spectrometer (INMS). Signal returned from the instrument included native Saturn species, as expected, as well as a significant amount of signal attributed to vaporized ices and higher mass organics believed to be flowing into Saturn's atmosphere from the rings. In this paper, we present an in-depth compositional analysis of the mass spectra returned from Cassini's last few orbits. We use a mass spectral deconvolution algorithm designed specifically to handle the complexities involved with unit resolution spaceflight mass spectrometry data to determine the relative abundance of species detected in the observations. We calculate the downward external flux and mass deposition rates of ring volatile species into Saturn's atmosphere and conclude that during these observations ring material was being deposited into Saturn's equatorial region at a rate on the order of 10(exp 4) kg/s.

Saturn↗
DOE OSTI2021

Reducing Sample Loss in Measurement of Heat of Vaporization of Ethanol/Gasoline Blends by Differential Scanning Calorimetry/Thermogravimetric Analysis

Higher gasoline Heat of Vaporization (HOV) can enable higher compression-ratio direct injection spark ignition engines by providing evaporative cooling that effectively increases fuel knock resistance. Methods to directly measure this fuel property in complex gasoline samples are not well developed. The objective of the present study was to further improve a Differential Scanning Calorimetry/Thermogravimetric Analyzer (DSC/TGA) method to measure the total and partial HOV of gasoline. Ten market gasoline samples were chosen to have a wide range of properties to assess the method's capability across the entire volatility range with an emphasis on understanding how well the method captures the initial 10 percent (%) of sample evaporation and how much sample is left unevaporated at the end of the experiment. Modifications to the sample preparation/introduction method as well as to the instrument itself were made to reduce initial sample losses which included measurements of the HOV at 10 degrees C and 5 degrees C (in a cold chamber) as well as under (uncontrolled) ambient conditions. Experimental results from the DSC/TGA were compared to calculated total HOV results based on Detailed Hydrocarbon Analysis (DHA). Results from the two methods agreed very well with the difference being 5% or less in almost every case. In addition, the repeatability of the method was investigated by analyzing samples in triplicate at the three temperatures investigated. One valuable conclusion from the study was that the lower temperatures of 10 degrees C and 5 degrees C enabled more reproducible measurements for both total and partial HOV. This improved precision may be caused by the fact that temperature control in the cold chamber was more reliable than the ambient laboratory temperature control. Additionally, cold chamber experiments, due to ergonomic limitations, did not allow for the use of a lid on the sample pan. The reproducibility of the evaporation rate was found to be highly dependent on the pan/lid fit which can vary significantly such that elimination of the lid improved measurement precision while operation at sub-ambient temperature slowed the evaporation rate. Results detailing sample preparation and instrument modifications as well as a detailed comparison of total and partial HOV results are presented.

ADVANCED PROPULSION SYSTEMS,BIOMASS FUELS↗
NASA NTRS2004

Insight into Primordial Solar System Oxygen Reservoirs from Returned Cometary Samples

The recent successful rendezvous of the Stardust spacecraft with comet Wild-2 will be followed by its return of cometary dust to Earth in January 2006. Results from two separate dust impact detectors suggest that the spacecraft collected approximately the nominal fluence of at least 1,000 particles larger than 15 micrometers in size. While constituting only about one microgram total, these samples will be sufficient to answer many outstanding questions about the nature of cometary materials. More than two decades of laboratory studies of stratospherically collected interplanetary dust particles (IDPs) of similar size have established the necessary microparticle handling and analytical techniques necessary to study them. It is likely that some IDPs are in fact derived from comets, although complex orbital histories of individual particles have made these assignments difficult to prove. Analysis of bona fide cometary samples will be essential for answering some fundamental outstanding questions in cosmochemistry, such as (1) the proportion of interstellar and processed materials that comprise comets and (2) whether the Solar System had a O-16-rich reservoir. Abundant silicate stardust grains have recently been discovered in anhydrous IDPs, in far greater abundances (200 5,500 ppm) than those in meteorites (25 ppm). Insight into the more subtle O isotopic variations among chondrites and refractory phases will require significantly higher precision isotopic measurements on micrometer-sized samples than are currently available.

Brownlee, D. E.↗
DOE OSTI2021

ExoMars Mars Organic Molecule Analyzer (MOMA) Laser Desorption/Ionization Mass Spectrometry (LDI-MS) Analysis of Phototrophic Communities from a Silica-Depositing Hot Spring in Yellowstone National Park, USA

The Mars Organic Molecule Analyzer (MOMA) is a key scientific instrument on the ExoMars Rover mission. MOMA is designed to detect and characterize organic compounds, over a wide range of volatility and molecular weight, in samples obtained from up to two meters below the martian surface. Thorough analog sample studies are required to best prepare to interpret MOMA data collected on Mars. We present here the MOMA characterization of Mars analog samples collected from an alkaline silica depositing hot spring in Yellowstone National Park, WY, USA. These samples contain microbial streamer communities composed primarily of oxygenic and anoxygenic phototrophs. Additionally, in a study focused on detection of key classes of nonvolatile organics, samples of microbial streamers and their total lipid extract (TLE) have been measured on a MOMA Engineering Test Unit (ETU) instrument using its laser desorption/ionization mass spectrometry (LDI-MS) mode. MOMA LDI-MS detected a variety of lipids and pigments in the TLE sample. Species such as chlorophyll a were also detected from the streamer sample with the help of mass isolation. The results add to the LDI-MS sample characterization database, as well as demonstrate the benefit of using mass isolation on the MOMA instrument to reveal the presence of complex organics, and potential biomarkers, preserved in a natural sample, providing guidance to the in situ analysis of surface samples during Mars operations.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2025

Large field-of-view event-mode camera for high-precision epithermal neutron resonance imaging

A large-area event-mode camera system coupled with a 6 LiF-ZnS:Ag scintillator is applied for neutron resonance imaging (NRI) on the energy-resolved neutron imaging (ERNI) flight path, also known as Flight Path 5 (FP5), at the Los Alamos Neutron Science Center (LANSCE). This novel neutron imaging system, featuring a 120 x 120 mm 2 field of view, efficiently captures resonance information across the entire image in a single acquisition, significantly reducing beam time requirements compared to conventional energy-resolved neutron imaging systems. High-quality neutron radiographs with enhanced spatial resolution are achieved through the reconstruction of neutron events based on observations of individual photons emitted from the scintillator. The system demonstrates reduced background through neutron/gamma discrimination capabilities while maintaining sharpness across a large fields of view. In the measurements presented here, a spatial resolution of approximately 340 μm was achieved using center-of-gravity photon cluster centroiding. We demonstrate the system’s capability for quantitatively determining isotopic distributions in various thin samples, as well as automatically reconstructing complex scenes with overlapping resonances from diverse samples. These results are obtained using standard data analysis tools, despite the relatively slow 6 LiF-ZnS:Ag scintillator, which may not be optimal for absorption resonance detection. The capabilities demonstrated here offer a valuable, versatile, and cost-effective solution for high spatial and temporal resolution, large field-of-view energy-resolved neutron imaging, with potential applications across various scientific and industrial domains.

36 MATERIALS SCIENCE↗
DOE OSTI2021

High pressure, high flow rate batch mixing apparatus for high throughput experiments

An automated, high pressure, high flow rate batch mixing apparatus has been designed and constructed for rapid, stable, and repeatable mixing of multiple gases and vapors. The apparatus operates as an intermittent batch mixer with cycles of topping off fresh mixture to maintain pressure in an accumulator tank until consumed in an experimental apparatus. At high duty cycles, the apparatus can also function at steady state. This style of mixing is suitable for experiments such as high repetition rate shock tubes and other devices with intermittent flow demands. It is compact and portable, facilitating use in locations such as synchrotron light sources. The entire apparatus is heated to permit the mixing of vapors from species with low volatilities. The apparatus is fully automated and runs for extended periods with the only intervention being to refresh reagent supplies. Here, the accuracy and repeatability of the apparatus were verified by periodic gas sampling and analysis with gas chromatography. Multi-component mixtures spanning a wide range of complexity, dilution, and volatility of constituents have been prepared. The compositions of the majority of the mixture were found to be stable over several filling cycles, repeatable, and with the proper calibration of set-point conditions, accurate. Challenges were encountered preparing a mixture from multi-component liquids, and potential solutions are discussed.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Analyzing Mass Spectrometry Imaging Data of 13C-Labeled Phospholipids in Camelina sativa and Thlaspi arvense (Pennycress) Embryos

The combination of 13C-isotopic labeling and mass spectrometry imaging (MSI) offers an approach to analyze metabolic flux in situ. However, combining isotopic labeling and MSI presents technical challenges ranging from sample preparation, label incorporation, data collection, and analysis. Isotopic labeling and MSI individually create large, complex data sets, and this is compounded when both methods are combined. Therefore, analyzing isotopically labeled MSI data requires streamlined procedures to support biologically meaningful interpretations. Using currently available software and techniques, here we describe a workflow to analyze 13C-labeled isotopologues of the membrane lipid and storage oil lipid intermediate―phosphatidylcholine (PC). Our results with embryos of the oilseed crops, Camelina sativa and Thlaspi arvense (pennycress), demonstrated greater 13C-isotopic labeling in the cotyledons of developing embryos compared with the embryonic axis. Greater isotopic enrichment in PC molecular species with more saturated and longer chain fatty acids suggest different flux patterns related to fatty acid desaturation and elongation pathways. The ability to evaluate MSI data of isotopically labeled plant embryos will facilitate the potential to investigate spatial aspects of metabolic flux in situ.

metabolomics↗
NASA NTRS2014

A Compact Tandem Two-Step Laser Time-of-Flight Mass Spectrometer for In Situ Analysis of Non-Volatile Organics on Planetary Surfaces

Two-step laser desorption mass spectrometry is a well suited technique to the analysis of high priority classes of organics, such as polycyclic aromatic hydrocarbons, present in complex samples. The use of decoupled desorption and ionization laser pulses allows for sensitive and selective detection of structurally intact organic species. We have recently demonstrated the implementation of this advancement in laser mass spectrometry in a compact, flight-compatible instrument that could feasibly be the centerpiece of an analytical science payload as part of a future spaceflight mission to a small body or icy moon.

time-of-flight↗
NASA NTRS2012

Indigenous Carbon Embedded in Apollo 17 Black Volcanic Glass Surface Deposits

The assessment of indigenous organic matter in returned lunar samples was one of the primary scientific goals of the Apollo program. The levels of such organic material were expected to be and found to be small. Previous work on this topic includes Murphy et al. [1] who reported the presence of anthropogenic organics with sub-ppm concentrations in Apollo 11 fines. In Apollo 12 samples, Preti et al. [2] detected low levels, < 10 ppb or below, of more complex organic material that may have been synthesized by abrupt heating during analysis. Kvenvolden et al. [3] detected porphyrin-like pigments at the ng to pg level in an Apollo 11 bulk sample. Hodgson et al. [4] and Ponnamperuma et al. [5] suggested that most if not all porphyrins were synthesized from rocket fuel during module landing. Chang et al. [6] reported indigenous carbon ranging from 5-20 g/g in the form of metal carbides in Apollo 11 fines. Hare et al. [7] reported amino acids at he 50 ng/g level in Apollo 11 samples but suggested the results may be explained as contamination. More recently, Clemett et al. [8] reported simple polycyclic aromatic hydrocarbons at concentrations of < 1ppm in an Apollo 16 soil. Low concentrations of lunar organics may be a consequence not only of its paucity, but also its heterogeneous distribution. If the sample size required for a measurement is large relative to the localization of organics, detection is limited not by ultimate sensitivity but rather by the ability to distinguish an indigenous signature from background contamination [9].

Thomas-Keprta, Kathie L.↗
DOE OSTI2026

Single-Particle Isotopic Analysis Using the Liquid Sampling-Atmospheric Pressure Glow Discharge Microplasma Coupled to an Orbitrap Mass Spectrometer

Isotope ratio (IR) determinations on individual particles can provide valuable information relative to the sample, including processing and dating, which could be valuable to geological and nuclear material analysis communities. In comparison to “bulk” measurements, in which all particle information is lost and homogenized within a sample, “particle” measurements allow for fingerprinting and can provide unique insights related to the sample’s nano- and micro- compositions. Furthermore, the complex nature of particles, with potential isobaric interferences from either the matrix or other elements within the same particle, poses a significant analytical challenge for conventional mass spectrometry platforms employed for elemental analysis due to their limited mass resolution. Presented here is the first demonstration of an ultrahigh resolution method for single particle (SP) isotopic analysis using the liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma ionization source coupled to an Orbitrap mass spectrometer and FTMS Booster X2T acquisition/processing system. For proof of concept, well-characterized CeO 2 microparticles with a nominal diameter of 1.0 μm were analyzed at a mass resolution of ∼330,000. Important instrumental parameters were optimized to enable the detection of single particles. The 142 Ce/ 140 Ce ratio of individual particles and the population average were determined and compared to an SP inductively coupled plasma time-of-flight mass spectrometry (ICP-TOF-MS) analysis. The isotopic accuracy and precision were determined by two methods and found to be in good agreement with the SP-ICP-TOF-MS method, with the linear regression slope method providing a more accurate ratio, showing a ∼1.4% relative difference from the ratio determined from a particle digest. The encouraging performance of the method was further supported by a determined detection limit of 2.9 fg ( 142 Ce). The developed method is anticipated to overcome many of the challenges posed by isobaric interferences encountered in conventional mass spectrometry techniques when analyzing real-world samples for particle isotopic composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Investigation of potential polyatomic interferences on uranium isotope ratio measurements for the LS-APGD-Orbitrap MS system

The determination of actinide (e.g., U and Pu) content and isotopics is of importance to the nuclear forensics and safeguards communities. However, in the analysis of environmental samples, such as those collected by the International Atomic Energy Agency, uranium measurements can be complicated by isobaric interferences from polyatomic variants of heavy elements (e.g., Pb). This leads to complex, time-consuming sample manipulations (i.e., separations) before determining isotope ratios. An alternative strategy to sample pretreatment is to use high-resolution mass spectrometric platforms during the analysis to fully resolve the uranium isotopes from potential polyatomic interferences, negating the need for prior chemical separation. The liquid sampling - atmospheric pressure glow discharge (LS-APGD) coupled with an Orbitrap mass spectrometer provides a high-resolution (>70,000 m/Δm at m/z 200) inorganic mass spectrometry platform. Further, as a demonstration of the power of this instrumental platform, and indeed, the high-resolution approach in general, uranium isotope ratios were determined in the presence of elemental impurities (e.g., Pb, Pt, Ta, W) commonly encountered with environmental sample swipe analysis, without any prior treatment. Even at elemental impurity concentrations of 1000–5000× relative to uranium, no interference was observed with the 235 U or 238 U signal. In addition, the 235 U/ 238 U isotope ratio for the samples with the concomitants present are within 2 standard deviations of the values obtained without their addition, indicating that these impurities do not impact the determined uranium isotope ratio. These findings represent a significant first step in leveraging the high resolution of the LS-APGD-Orbitrap-MS to overcome isobaric and molecular interferences instead of relying on chemical separations.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
DOE OSTI2024

Automating data analysis for hydrogen/deuterium exchange mass spectrometry using data-independent acquisition methodology

We present a hydrogen/deuterium exchange workflow coupled to tandem mass spectrometry (HX-MS 2 ) that supports the acquisition of peptide fragment ions alongside their peptide precursors. The approach enables true auto-curation of HX data by mining a rich set of deuterated fragments, generated by collisional-induced dissociation (CID), to simultaneously confirm the peptide ID and authenticate MS 1 -based deuteration calculations. The high redundancy provided by the fragments supports a confidence assessment of deuterium calculations using a combinatorial strategy. The approach requires data-independent acquisition (DIA) methods that are available on most MS platforms, making the switch to HX-MS 2 straightforward. Importantly, we find that HX-DIA enables a proteomics-grade approach and wide-spread applications. Considerable time is saved through auto-curation and complex samples can now be characterized and at higher throughput. We illustrate these advantages in a drug binding analysis of the ultra-large protein kinase DNA-PKcs, isolated directly from mammalian cells.

59 BASIC BIOLOGICAL SCIENCES↗
NASA NTRS2006

Painting Analysis of Chromosome Aberrations Induced by Energetic Heavy Ions in Human Cells

FISH, mFISH, mBAND, telomere and centromere probes have been used to study chromosome aberrations induced in human cells exposed to low-and high-LET radiation in vitro. High-LET induced damages are mostly a single track effect. Unrejoined chromosome breaks (incomplete exchanges) and complex type aberrations were higher for high-LET. Biosignatures may depend on the method the samples are collected. Recent mBAND analysis has revealed more information about the nature of intra-chromosome exchanges. Whether space flight/microgravity affects radiation-induced chromosome aberration frequencies is still an open question.

Wu, Honglu↗
DOE OSTI2021

Deep Learning Segmentation of Complex Features in Atomic-Resolution Phase-Contrast Transmission Electron Microscopy Images

Phase-contrast transmission electron microscopy (TEM) is a powerful tool for imaging the local atomic structure of materials. TEM has been used heavily in studies of defect structures of two-dimensional materials such as monolayer graphene due to its high dose efficiency. However, phase-contrast imaging can produce complex nonlinear contrast, even for weakly scattering samples. It is, therefore, difficult to develop fully automated analysis routines for phase-contrast TEM studies using conventional image processing tools. For automated analysis of large sample regions of graphene, one of the key problems is segmentation between the structure of interest and unwanted structures such as surface contaminant layers. In this study, we compare the performance of a conventional Bragg filtering method with a deep learning routine based on the U-Net architecture. We show that the deep learning method is more general, simpler to apply in practice, and produces more accurate and robust results than the conventional algorithm. We provide easily adaptable source code for all results in this paper and discuss potential applications for deep learning in fully automated TEM image analysis.

47 OTHER INSTRUMENTATION↗
DOE OSTI2021

Algorithms and file structures to enhance software workflows for ion mobility mass spectrometry (IM-MS): CRADA 410 (Final Report)

This document is the final report for CRADA 410 (Project No. 72496). The purpose of this project was supporting customizations of algorithms and raw data file structures to enhance software workflows for liquid chromatography (LC), mass spectrometry (MS) and ion mobility mass spectrometry (IM-MS)-based metabolite characterization. PNNL worked with Agilent to evaluate and improve the integration of ion mobility into existing MS data analysis methods of Agilent software tools. The project augmented PNNL’s capabilities to analyze complex omics samples. These capabilities are directly beneficial to DOE and PNNL efforts to characterize and analyze compounds in microbial and plant communities. The project assisted Agilent in further developing improved instrument-software solutions combining ion mobility with mass spectrometry for widespread applications in life sciences and other fields.

97 MATHEMATICS AND COMPUTING↗
NASA NTRS2005

NWA 2736: An Unusual New Graphite-bearing Aubrite

Aubrites are enstatite-rich achondrites that are probably related to enstatite chondrite parent bodies. The exact link, if any, is not understood. They may have formed from melting within one or more enstatite chondrite parent bodies. Description of NWA 2736: One complete stone weighing 171.51 grams was recovered from the Sahara Desert by nomads sometime before September 2004. It was completely covered with fusion crust and desert varnish. This stone is severely weathered, with caramel brown coloration throughout and calcite veins that extend into the interior of the sample. Mineral analyses were performed and elemental x-ray maps were obtained with a CAMECA SX-50 electron microprobe at the Lunar and Planetary Laboratory at the University of Arizona. The relatively high modal abundance of albitic plagioclase, presence of euhedral graphite, depletion of troilite, and occurrence of pervasive kamacite veins (some with daubreelite) all indicate that NWA 2736 has a complex history and may sample a new region of the aubrite parent body. A discussion and analysis on the overall texture of NWA 2736 is presented.

Lowe, J. J.↗