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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 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
NASA NTRS2015

Nanophase Carbonates on Mars: Does Evolved Gas Analysis of Nanophase Carbonates Reveal a Large Organic Carbon Budget in Near-Surface Martian Materials?

Evolved Gas Analysis (EGA), which involves heating a sample and monitoring the gases released, has been performed on Mars by the Viking gas chromatography/mass spectrometry instruments, the Thermal and Evolved Gas Analyzer (TEGA) on the Phoenix lander, and the Sample Analysis at Mars (SAM) instrument on the Mars Science Laboratory. All of these instruments detected CO2 released during sample analysis at abundances of approx. 0.1 to 5 wt% assuming a carbonate source. The source of the CO2 can be constrained by evaluating the temperature of the gas release, a capability of both the TEGA and SAM instruments. The samples analyzed by SAM show that the majority of the CO2 is released below 400C, much lower than traditional carbonate decomposition temperatures which can be as low as 400C for some siderites, with magnesites and calcites decomposing at even higher temperatures. In addition to mineralogy, decomposition temperature can depend on particle size (among other factors). If carbonates formed on Mars under low temperature and relative humidity conditions, the resulting small particle size (nanophase) carbonates could have low decomposition temperatures. We have found that calcite can be synthesized by exposing CaO to water vapor and CO2 and that the resulting mineral has an EGA peak of approx. 550C for CO2, which is about 200C lower than for other calcites. Work is ongoing to produce Fe and Mg-bearing carbonates using the same process. Current results suggest that nanophase calcium carbonates cannot explain the CO2 released from martian samples. If the decomposition temperatures of Mg and Fe-bearing nanophase carbonates are not significantly lower than 400C, other candidate sources include oxalates and carboxylated organic molecules. If present, the abundance of organic carbon in these samples could be greater than 0.1 wt % (1000s of ppm), a signficant departure from the paradigm of the organic-poor Mars based on Viking results.

Archer, P. Douglas, Jr.↗
NASA NTRS2014

Sulfur-bearing Phases Detected by Evolved Gas Analysis of the Rocknest Aeolian Deposit, Gale Crater, Mars

The Sample Analysis at Mars (SAM) instrument suite detected SO2, H2S, OCS, and CS2 from ~450 to 800degC during evolved gas analysis (EGA) of materials from the Rocknest aeolian deposit in Gale Crater, Mars. This was the first detection of evolved sulfur species from a Martian surface sample during in situ EGA. SO2 (~3-22 μmol) is consistent with the thermal decomposition of Fe sulfates or Ca sulfites, or evolution/desorption from sulfur-bearing amorphous phases. Reactions between reduced sulfur phases such as sulfides and evolved O2 or H2O in the SAM oven are another candidate SO2 source. H2S (~41-109 nmol) is consistent with interactions of H2O, H2 and/or HCl with reduced sulfur phases and/or SO2 in the SAM oven. OCS (~1-5nmol) and CS2 (~0.2-1 nmol) are likely derived from reactions between carbon-bearing compounds and reduced sulfur. Sulfates and sulfites indicate some aqueous interactions, although not necessarily at the Rocknest site; Fe sulfates imply interaction with acid solutions whereas Ca sulfites can form from acidic to near-neutral solutions. Sulfides in the Rocknest materials suggest input from materials originally deposited in a reducing environment or from detrital sulfides from an igneous source. The presence of sulfides also suggests that the materials have not been extensively altered by oxidative aqueous weathering. The possibility of both reduced and oxidized sulfur compounds in the deposit indicates a nonequilibrium assemblage. Understanding the sulfur mineralogy in Rocknest materials, which exhibit chemical similarities to basaltic fines analyzed elsewhere on Mars, can provide insight in to the origin and alteration history of Martian surface materials.

Gale Crater↗
NASA NTRS1981

An integrated exhaust gas analysis system with self-contained data processing and automatic calibration

An integrated gas analysis system designed to operate in automatic, semiautomatic, and manual modes from a remote control panel is described. The system measures the carbon monoxide, oxygen, water vapor, total hydrocarbons, carbon dioxide, and oxides of nitrogen. A pull through design provides increased reliability and eliminates the need for manual flow rate adjustment and pressure correction. The system contains two microprocessors to range the analyzers, calibrate the system, process the raw data to units of concentration, and provides information to the facility research computer and to the operator through terminal and the control panels. After initial setup, the system operates for several hours without significant operator attention.

Anderson, R. C.↗
DOE OSTI2022

Product specific thermal degradation kinetics of bisphenol F epoxy in inert and oxidative atmospheres using evolved gas analysis–mass spectrometry

Knowledge of the degradation kinetics for polymer materials is important for understanding thermal stability. In this study, evolved gas analysis–mass spectrometry and pyrolysis gas-chromatography-mass spectrometry were evaluated for the potential to deliver additional insight into thermal degradation kinetics of diglycidal ether of bisphenol F (DGEBF) epoxy thermoset under inert and oxidative atmospheres. Degradation products of selected precursor ions were evaluated for their uniqueness to the specific precursor using extracted ion thermographs. Unique mass peaks, solely attributed to a single reaction pathway of a specific product, were determined from extracted ion thermographs and used to determine both activation energy (E a ) and pre-exponential factors for the specific primary reaction pathways. These primary reaction pathways for DGEBF epoxy degradation were then evaluated in the context of transition state theory (TST) and related transition state enthalpies (ΔH ‡ ) and entropies (ΔS ‡ ) of activation to further elucidate the degradation process. It was determined under pyrolysis conditions, as suggested by the E a , the formation of bisphenol F monomer was the rate-limiting step toward the formation of xanthene and phenol. In contrast, under thermo-oxidative conditions, reactions involving oxygen containing species were identified as the rate-limiting step for all observed products based on the large negative ΔS ‡ calculated from TST. This work demonstrates a powerful combination of technique and theory that can provide new insight into the degradation of polymer materials.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2014

Sulfur-Bearing Phases Detected by Evolved Gas Analysis of the Rocknest Aeolian Deposit, Gale Crater, Mars

The Sample Analysis at Mars (SAM) instrument suite detected SO2, H2S, OCS, and CS2 from approx.450 to 800 C during evolved gas analysis (EGA) of materials from the Rocknest aeolian deposit in Gale Crater, Mars. This was the first detection of evolved sulfur species from a Martian surface sample during in situ EGA. SO2(approx. 3-22 micro-mol) is consistent with the thermal decomposition of Fe sulfates or Ca sulfites, or evolution/desorption from sulfur-bearing amorphous phases. Reactions between reduced sulfur phases such as sulfides and evolved O2 or H2O in the SAM oven are another candidate SO2 source. H2S (approx.41-109 nmol) is consistent with interactions of H2O, H2 and/or HCl with reduced sulfur phases and/or SO2 in the SAM oven. OCS (approx.1-5 nmol) and CS2(approx.0.2-1 nmol) are likely derived from reactions between carbon-bearing compounds and reduced sulfur. Sulfates and sulfites indicate some aqueous interactions, although not necessarily at the Rocknest site; Fe sulfates imply interaction with acid solutions whereas Ca sulfites can form from acidic to near-neutral solutions. Sulfides in the Rocknest materials suggest input from materials originally deposited in a reducing environment or from detrital sulfides from an igneous source. The presence of sulfides also suggests that the materials have not been extensively altered by oxidative aqueous weathering. The possibility of both reduced and oxidized sulfur compounds in the deposit indicates a nonequilibrium assemblage. Understanding the sulfur mineralogy in Rocknest materials, which exhibit chemical similarities to basaltic fines analyzed elsewhere on Mars, can provide insight in to the origin and alteration history of Martian surface materials.

evolved gas analysis↗
DOE OSTI2016

Isotopic gas analysis through Purcell cavity enhanced Raman scattering

Purcell enhanced Raman scattering (PERS) by means of a doubly resonant Fabry-Perot microcavity (mode volume ≈ 100 μm{sup 3} and finesse ≈ 30 000) has been investigated as a technique for isotopic ratio gas analysis. At the pump frequency, the resonant cavity supports a buildup of circulating power while simultaneously enabling Purcell spontaneous emission rate enhancement at the resonant Stokes frequency. The three most common isotopologues of CO{sub 2} gas were quantified, and a signal was obtained from {sup 13}C{sup 16}O{sub 2} down to a partial pressure of 2 Torr. Due to its small size and low pump power needed (∼10 mW) PERS lends itself to miniaturization. Furthermore, since the cavity is resonant with the emission frequency, future improvements could allow it to serve as its own spectral analyzer and no separate spectroscopic device would be needed.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2014

Application of evolved gas analysis to cold-cap reactions of melter feeds for nuclear waste vitrification

In the vitrification of nuclear wastes, the melter feed (a mixture of nuclear waste and glass-forming and modifying additives) experiences multiple gas-evolving reactions in an electrical glass-melting furnace. We employed the thermogravimetry-gas chromatography-mass spectrometry (TGA-GC-MS) combination to perform evolved gas analysis (EGA). Apart from identifying the gases evolved, we performed quantitative analysis relating the weighed sum of intensities of individual gases linearly proportional with the differential themogravimetry. The proportionality coefficients were obtained by three methods based on the stoichiometry, least squares, and calibration. The linearity was shown to be a good first-order approximation, in spite of the complicated overlapping reactions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2015

Enhanced sensitivity of Raman spectroscopy for tritium gas analysis using a metal-lined hollow glass fiber

The precise compositional analysis of tritium-containing gases is of high interest for tritium accountancy in future fusion power plants. Raman spectroscopy provides a fast and contact-free gas analysis procedure with high precision, thus being an advantageous tool for the named purpose. In this paper, it is shown that the sensitivity achieved with conventional Raman systems (in 90 degrees or forward/backward configurations) can be enhanced by at least one order of magnitude by using a metal-lined hollow glass fiber as the Raman cell. This leads to the ability of detecting low partial pressures of tritium within short measurement intervals (< 0.5 mbar in < 0.5 s) opening the way for real-time applications.

07 ISOTOPE AND RADIATION SOURCES↗
DOE OSTI2025

Evolved Gas Analysis–Mass Spectrometry Exposes Polymer Network Structures

Polymer network structures in epoxy thermosets play an important role in the final thermoset material properties. However, analytical characterization of these network structures is difficult due to their amorphous nature. In this work, the application of evolved gas analysis–mass spectrometry (EGA-MS) to characterize the polymer network structures of bisphenol A (BPA)-based thermosets is demonstrated. Analytical characterization of the polymer network structures is accomplished by monitoring the Product-Specific Kinetics (PSK) of BPA monomer formation during thermal degradation investigations. We relate observed differences in the activation energy (E a ) of BPA monomer formation to the local packing environment around the BPA monomer units within the polymer network. Variations in the local environment related to the polymer networks manifest qualitatively as broadening in the thermal profile of the BPA monomer evolution and quantitatively as changes in the activation energy (E a ). Three BPA thermoset formulations were investigated; two amine-cured thermoset with 4,4′-diaminodiphenylmethane (DDM) or poly(propylene glycol) bis(2-amino-propyl ether) (PPG400) and a homopolymerized thermoset via curing with Epikure 3253 catalyst (3253). Results revealed that the 3253 thermoset contained two distinct packing densities in the polymer network, while DDM and PPG400 thermosets had uniform distributions of packing densities. Results from the DDM thermoset revealed a gradually decreasing E a , while the apparent E a of PPG400 was consistent over the entire degradation. Furthermore, these differences in E a were concluded to stem from the flexibility of the corresponding polymer networks and the ability of the network components to rearrange and occupy formed voids. Due to the minimal sample required for analysis (100–200 μg), this EGA-MS technique has great potential for postproduction evaluation of composite parts to identify changes in the polymer networks from use and aging, which could signal compromised performance.

Degradation↗
NASA NTRS2008

The Mars Phoenix Thermal Evolved-Gas Analysis: The Role of an Organic Free Blank in the Search for Organics

The Thermal Evolved-Gas Analyzer (TEGA) instrument onboard the 2007 Phoenix Lander will perform differential scanning calorimetry (DSC) and evolved-gas analysis of soil samples collected from the surface. Data from the instrument will be compared with Mars analog mineral standards, collected under TEGA Mars-like conditions to identify the volatile-bearing mineral phases [1] (e.g., Fe-oxyhydroxides, phyllosilicates, carbonates, and sulfates) found in the Martian soil. Concurrently, the instrument will be looking for indications of organics that might also be present in the soil. Organic molecules are necessary building blocks for life, although their presence in the ice or soil does not indicate life itself. The spacecraft will certainly bring organic contaminants to Mars even though numerous steps were taken to minimize contamination during the spacecraft assembly and testing. It will be essential to distinguish possible Mars organics from terrestrial contamination when TEGA instrument begins analyzing icy soils. To address the above, an Organic Free Blank (OFB) was designed, built, tested, and mounted on the Phoenix spacecraft providing a baseline for distinguishing Mars organics from terrestrial organic contamination. Our objective in this report is to describe some of the considerations used in selecting the OFB material and then report on the processing and analysis of the final candidate material

Lauer, H. V., Jr.↗
NASA NTRS2006

Thermal and Evolved Gas Analysis of Geologic Samples Containing Organic Materials: Implications for the 2007 Mars Phoenix Scout Mission

The Thermal and Evolved Gas Analyzer (TEGA) instrument scheduled to fly onboard the 2007 Mars Phoenix Scout Mission will perform differential scanning calorimetry (DSC) and evolved gas analysis (EGA) of soil samples and ice collected from the surface and subsurface at a northern landing site on Mars. We have been developing a sample characterization data library using a laboratory DSC integrated with a quadrupole mass spectrometer to support the interpretations of TEGA data returned during the mission. The laboratory TEGA test-bed instrument has been modified to operate under conditions similar to TEGA, i.e., reduced pressure (e.g., 100 torr) and reduced carrier gas flow rates. We have previously developed a TEGA data library for a variety of volatile-bearing mineral phases, including Fe-oxyhydroxides, phyllosilicates, carbonates, and sulfates. Here we examine the thermal and evolved gas properties of samples that contain organics. One of the primary objectives of the Phoenix Scout Mission is to search for habitable zones by assessing organic or biologically interesting materials in icy soil. Nitrogen is currently the carrier gas that will be used for TEGA. In this study, we examine two possible modes of detecting organics in geologic samples; i.e., pyrolysis using N2 as the carrier gas and combustion using O2 as the carrier gas.

Lauer, H. V., Jr.↗
NASA NTRS2021

Trash Compaction and Processing System Trash Models and Evolved Gas Analysis of Trash Components

As part of the NASA Next Space Technologies for Exploration Partnerships (NextSTEP) Trash Compaction and Processing System (TCPS) program, the Generation 2 (Gen 2) Heat Melt Compactor (HMC) tests a variety of trash models (nominal, high liquid, and high cloth) in order to evaluate the technical risk associated with processing spacecraft trash. The trash components used in the trash models not only impacts the final solid trash disk quality, but also the water and gas effluent compositions. In order to better design an auxiliary system to treat the effluent streams, both the input trash components and the effluent must be characterized. Evolved gas analysis (EGA) methods are used to characterize the input trash components. The EGA results will be used to determine various HMC operational parameters, as well as to determine the optimal operation for the TCPS system.

Heat Melt Compactor↗
DOE OSTI2022

Transformer Health Monitoring Using Dissolved Gas Analysis

As integral components of any power plant, transformers supply the generated electricity to the grid. However, a transformer’s cellulose-based paper insulation and the mineral oil in which it is immersed break down over time under standard operating conditions—or more rapidly due to potential faults within the system. As the transformer’s mineral oil breaks down, gases are released that can be measured and monitored. This technical brief exhibits a collection of diagnostic and prognostic techniques that utilities can adopt in lieu of labor-intensive periodic preventive maintenance routines. Furthermore, prognostic models have been incorporated using the latest version of the Institute of Electrical and Electronics Engineers (IEEE) standard (IEEE, 2019) for dissolved gas analysis (DGA), thus expanding it to include estimation of the time to maintenance. Overall, four different methodologies are explained, each of which aids in determining a transformer’s state of health. These methodologies include the Chendong model, the IEEE thermal life consumption model (IEEE, 2012), a diagnostic model for DGA, and a prognostic model for DGA that uses an autoregressive integrated moving average (ARIMA) model. An additional improvement for estimating missing system parameters by using monitoring data (i.e., a tool for parameter estimation utilizing Powell’s method) is presented, enabling the IEEE thermal life consumption model to benefit not only the collaborating power plant, but also the power industry at large.

24 POWER TRANSMISSION AND DISTRIBUTION↗
DOE OSTI2013

Kinetics of Cold-Cap Reactions for Vitrification of Nuclear Waste Glass Based on Simultaneous Differential Scanning Calorimetry - Thermogravimetry (DSC-TGA) and Evolved Gas Analysis (EGA)

For vitrifying nuclear waste glass, the feed, a mixture of waste with glass-forming and modifying additives, is charged onto the cold cap that covers 90-100% of the melt surface. The cold cap consists of a layer of reacting molten glass floating on the surface of the melt in an all-electric, continuous glass melter. As the feed moves through the cold cap, it undergoes chemical reactions and phase transitions through which it is converted to molten glass that moves from the cold cap into the melt pool. The process involves a series of reactions that generate multiple gases and subsequent mass loss and foaming significantly influence the mass and heat transfers. The rate of glass melting, which is greatly influenced by mass and heat transfers, affects the vitrification process and the efficiency of the immobilization of nuclear waste. We studied the cold-cap reactions of a representative waste glass feed using both the simultaneous differential scanning calorimetry thermogravimetry (DSC-TGA) and the thermogravimetry coupled with gas chromatography-mass spectrometer (TGA-GC-MS) as complementary tools to perform evolved gas analysis (EGA). Analyses from DSC-TGA and EGA on the cold-cap reactions provide a key element for the development of an advanced cold-cap model. It also helps to formulate melter feeds for higher production rate.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2016

Advanced In-situ Diagnostics for Multicomponent Gas Analysis and Material Aging

Current methods of detecting material aging rely heavily on accelerated aging studies expensive, bulky, and resource-hungry diagnostics. We are developing compact gas analysis methods based on sensor platforms such as quartz crystal microbalances (QCM), using nanoporous metals and Metal-Organic Frameworks (MOFs), which enhance sensitivity and impart selectivity to analytes. Targeted analytes are O2 and other volatile analytes. In FY16 we installed and tested a new QCM system coupled to a commercial gas mixing system. This instrumentation provides a new multi-use capability that: 1) allows evaluation of detection of novel materials to enable selective detection of volatile species relevant to Enhanced Surveillance; 2) accelerates development of new thin film deposition methods for depositing these materials on sensing devices; and 3) enables in-situ monitoring, with sub-monolayer sensitivity, of the interaction of volatile species with material surfaces subject to aging or corrosion.

36 MATERIALS SCIENCE↗