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At least 271 records · Page 15

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.↗

Gas analysis system for the Eight Foot High Temperature Tunnel

This paper describes the development of a gas collection and analysis system that is to be installed in the Eight-Foot High Temperature Tunnel (8' HTT) at NASA's Langley Research Center. This system will be used to analyze the test gas medium that results after burning a methane-air mixture to achieve the proper tunnel test parameters. The system consists of a sampling rake, a gas sample storage array, and a gas chromatographic system. Gas samples will be analyzed after each run to assure that proper combustion takes place in the tunnel resulting in a correctly balanced composition of the test gas medium. The proper ratio of gas species is critically necessary in order for the proper operation and testing of scramjet engines in the tunnel. After a variety of methane-air burn conditions have been analyzed, additional oxygen will be introduced into the combusted gas and the enriched test gas medium analyzed. The pre/post enrichment sets of data will be compared to verify that the gas species of the test gas medium is correctly balanced for testing of air-breathing engines.

Leighty, Bradley D.↗

Odor intensity and characterization studies of exhaust from a turbojet engine combustor

Sensory odor tests of the exhaust from a turbojet combustor operating at simulated idle conditions were made by a human panel sniffing diluted exhaust gas. Simultaneously, samples of undiluted exhaust gas were collected on adsorbent substrates, subsequently removed by solvent flushing, and analyzed chemically by liquid chromatographic methods. The concentrations of the principal malodorous species, the aromatic (unburned fuel-related) and the oxygenated (partially burned fuel) fractions, as determined chromatographically, correlated well with the intensity of the odor as determined by sniffing. Odor intensity increased as combustion efficiency decreased. Combustor modifications which increased combustion efficiency decreased odor intensity.

Butze, H. F.↗

Odor intensity and characterization studies of exhaust from a turbojet engine combustor

Sensory odor tests of the exhaust from a turbojet combustor operating at simulated idle conditions were made by a human panel sniffing diluted exhaust gas. Simultaneously, samples of undiluted exhaust gas were collected on adsorbent substrates, subsequently removed by solvent flushing, and analyzed chemically by liquid chromatographic methods. The concentrations of the principal malodorous species, the aromatic (unburned fuel-related) and the oxygenated (partially burned fuel) fractions, as determined chromatographically, correlated well with the intensity of the odor as determined by sniffing. Odor intensity increased as combustion efficiency decreased. Combustor modifications which increased combustion efficiency decreased odor intensity.

Butze, H. F.↗

Structure of Soot Growth Region of Laminar Premixed Methane/Oxygen Flames

The structure of the soot growth region of laminar premixed methane/oxygen flames (fuel-equivalence ratios of 1.60 - 2.77) was studied both experimentally and computationally. Measurements were carried out in flames stabilized on a flat flame burner operated at standard temperature and pressure, and included velocities by laser velocimetry, soot volume fractions by laser extinction, soot temperatures by multiline emission, gas temperatures (where soot was absent) by corrected fine-wire thermocouples, major gas species concentrations by sampling and gas chromatography, and hydrogen atom concentrations by the Li/LiOH technique in conjunction with atomic absorption to find the proportion of free lithium in the flames. The measured concentrations of major gas species were in reasonably good agreement with predictions based on the detailed mechanisms of Leung and Lindstedt, and Frenklach and coworkers. The measurements also confirmed predictions of both these mechanisms that H-atom concentrations are in local thermodynamic equilibrium throughout the soot growth region even through the concentrations of major gas species are not. Thus, present findings support recent evaluations of the hydrogen-abstraction/carbon-addition (HACA) soot growth mechanism in similar flames, where the approximation that H-atom concentrations were in local thermodynamic equilibrium was adopted, based on predictions using the two mechanisms, due to the absence of direct H-atom concentration measurements.

Xu, F.↗

Structure of the Soot Growth Region of Laminar Premixed Methane/Oxygen Flames

The structure of the soot growth region of laminar premixed methane/oxygen flames (fuel-equivalence ratios of 1.60-2.77) was studied both experimentally and computationally. Measurements were carried out in flames stabilized on a flat flame burner operated at standard temperature and pressure, and included velocities by laser velocimetry, soot volume fractions by laser extinction, soot temperatures by multiline emission, gas temperatures (where soot was absent) by corrected fine-wire thermocouples, major gas species concentrations by sampling and gas chromatography, and hydrogen atom concentrations by the Li/LiOH technique in conjunction with atomic absorption to find the proportion of free lithium in the flames. The measured concentrations of major gas species were in reasonably good agreement with predictions based on the detailed mechanisms of Leung and Lindstedt, and Frenklach and coworkers. The measurements also confirmed predictions of both these mechanisms that H-atom concentrations are in local thermodynamic equilibrium throughout the soot growth region even through the concentrations of major gas species are not. Thus, present findings support recent evaluations of the hydrogen-abstraction/carbon-addition (HACA) soot growth mechanism in similar flames, where the approximation that H-atom concentrations were in local thermodynamic equilibrium was adopted, based on predictions using the two mechanisms, due to the absence of direct H-atom concentration measurements.

Xu, F.↗

Structure of the Soot Growth Region of Laminar Premixed Methane/Oxygen Flames

The structure of the soot growth region of laminar premixed methane/oxygen flames (fuel-equivalence ratios of 1.60-2.77) was studied both experimentally and computationally. Measurements were carried out in flames stabilized on a flat flame burner operated at standard temperature and pressure, and included velocities by laser velocimetry, soot volume fractions by laser extinction, soot temperatures by multiline emission, gas temperatures (where soot was absent) by corrected fine-wire thermocouples, major gas species concentrations by sampling and gas chromatography, and hydrogen atom concentrations by the Li/LiOH technique in conjunction with atomic absorption to find the proportion of free lithium in the flames. The measured concentrations of major gas species were in reasonably good agreement with predictions based on the detailed mechanisms of Leung and Lindstedt, and Frenklach and coworkers. The measurements also confirmed predictions of both these mechanisms that H-atom concentrations are in local thermodynamic equilibrium throughout the soot growth region even through the concentrations of major gas species are not. Thus, present findings support recent evaluations of the hydrogen-abstraction/carbon-addition (HACA) soot growth mechanism in similar flames, where the approximation that H-atom concentrations were in local thermodynamic equilibrium was adopted, based on predictions using the two mechanisms, due to the absence of direct H-atom concentration measurements.

Xu, F.↗

Device for quickly sensing the amount of O2 in a combustion product gas

A sensing device comprising an O2 sensor, a pump, a compressor, and a heater is provided to quickly sense the amount of O2 in a combustion product gas. A sample of the combustion product gas is compressed to a pressure slightly above one atmosphere by the compressor. Next, the heater heats the sample between 800 C and 900 C. Next, the pump causes the sample to be flushed against the electrode located in O2 sensor 6000 to 10,000 times per second. Reference air at approximately one atmosphere is provided to the electrode of O2 sensor. Accordingly, the O2 sensor produces a voltage which is proportional to the amount of oxygen in the combustion product gas. This voltage may be used to control the amount of O2 entering into the combustion chamber which produces the combustion product gas.

Singh, Jag J.↗

A Study of the Curation Protocol by Sample Analysis Working Team (SAWT) in Martian Moons eXploration (MMX) Project

Japan Aerospace Exploration Agency (JAXA) will launch a spacecraft in 2024 for a sample return mission from Phobos (Martian Moons eXploration: MMX). The major scientific goals of MMX are to constrain (1) the origin of Phobos and Deimos and (2) the evolution of the Mars-moon system [1]. The touchdown operations are planned to be performed twice at different landing sites on the Phobos surface to collect > 10 g of the surface materials [2]. After the return to the Earth, the Phobos samples will be collected from the individual sample canisters and introduced to the clean chamber installed at ISAS (Institute of Space and Astronautical Science). The Sample Analysis Working Team (SAWT) of MMX designed the procedure of Phobos sample analysis mainly conducted by the initial analysis teams [3]. For the next step, the SAWT will define the procedure of the curation process (mostly non-destructive analysis) of the Phobos samples, which will be presented here. The protocols of the Phobos sample curation is illustrated in figure 1. First, the headspace gas from the sample container will be collected during the Quick Analysis phase. The Quick Analysis will be operated by the sampler and curation teams in ISAS/JAXA. The terrestrial leak and contamination from the sampling systems will be tested using a quadrupole mass spectrometer equipped with a gas sampling system. Second, the bulk Phobos sample will be observed in the clean chamber under purified-N2 gas with an ambient condition (Pre-basic Characterization). This phase will be operated by the curation team in ISAS/JAXA and the instrument team of the MMX mission. The consistency between the data from the instruments in the clean chamber and the spacecraft will then be evaluated. Subsequently, the curation will distribute the small amount of Phobos samples to the Initial analysis team of MMX to conduct the "Preliminary Examination". The objectives of the preliminary examination are to provide (1) feedback on the subsequent sample allocation process, (2) preliminary scientific results that will address parts of MMX mission goals, and (3) evaluation of the sampling system and terrestrial alteration on Phobos samples. Because multiple models are proposed for the origin of Phobos [1] (e.g., giant impact, the capture of asteroids), the chemical and mineralogical characteristics of Phobos must be assessed before the allocation of the samples to the individual initial analysis teams. Simultaneously, the curation team in JAXA will observe the individual grains and aliquots of the samples in the clean chamber (Basic Characterization).

R Fukai↗

Discovery of solar wind neon in the Allende meteorite

Insert gases have been measured in seven sieve fractions of a disaggregated sample of the Allende meteorite. The disaggregation was done by ultrasonic treatment in water and by freeze-thawing. This sample consititutes the first gas-rich portion known to occur in the Allende meteorite. The composition of the trapped neon is solar, i.e., Neon-B, and the gas-rich samples contain more trapped Ne-20 than Ar-36. The set of sieve fractions show an anticorrelation of Ne-20 content and grain size. Gas-richness seems to be quite common among the CV3 meteorites with Allende added to the earlier known cases of Mokoia, Vigarano, and Efremovka.

Heymann, D.↗

A search for spectral alteration effects in chondritic gas-rich breccias

Several samples of gas-rich breccias were selected, including slabs of the Kapoeta howardite, the ordinary chondrites Dubrovnik, Cangas de Onis, and Dimmit. Numerous 0.8 to 2.5 micron reflection spectra of selected areas on sawed or broken surfaces were measured with the Planetary Geosciences Division spectrogoniometer. While these spectra are not directly comparable to those of powered samples, comparisons within the data set should reveal any spectral differences due to weathering. These results indicate that unknown regolith processes do not confer the ordinary-chondrite parent bodies with an altered layer exhibiting S-class spectral properties. This is consistent with recent interpretations of the new Q-class of asteroids as the ordinary-chondrite parent bodies. However, significant spectral effects do occur in asteroid regoliths: darkening and suppression of absorption bands in highly shocked material, as seen previously in the so-called black chondrites; and segregation of metal in large impact melt pools on chondritic asteroids, which may have achondritic spectra. Neither of these effects is likely to be significant in interpreting current integral-disk spectra, but should be searched for in spectral maps returned by future spacecraft.

Bell, J. F.↗

Components Refurbishment and Chemical Analysis Facility, Hot Spot 1 Solid Waste Management Unit #041 Year 4 Annual Performance Monitoring Report Kennedy Space Center, Florida

This Year 4 Annual Performance Monitoring Report (PMR) presents the operations, maintenance, and monitoring activities for the Hydraulic Containment System (HCS) Interim Measure (IM) at the Components Refurbishment and Chemical Analysis (CRCA) facility located at John F. Kennedy Space Center (KSC), Florida. The primary objective of the HCS is to attain hydraulic control of the dissolved-phase chlorinated volatile organic compound (CVOC) plume, with the secondary objective to reduce concentrations of CVOCs in the high-concentration plume to support transition to monitored natural attenuation (MNA). CRCA has been designated Solid Waste Management Unit 041 under the KSC Resource Conservation and Recovery Act Corrective Action Program. The timeframe for activities documented in this Year 4 PMR extends from November 2022 through September 2023. Baseline sampling activities were completed in June 2019, and full-scale startup of the HCS IM was completed in July-August 2019. The operational runtime of the HCS for the Year 4 reporting period was approximately 94%, with the majority of downtime attributed to associated groundwater sampling events, maintenance, and Hurricane Nicole. Almost five million gallons of groundwater were treated during Year 4 of HCS operations, and concentrations of the site’s contaminants of concern (trans-1,2-dichloroethene and vinyl chloride) have been reduced by over 99%. This PMR describes the activities that were performed during Year 4 to operate and monitor the HCS IM, which includes three extraction wells, seven injection wells, and conveyance piping to a modular structure containing the control panel and an air stripper. Influent and effluent sampling results from the air stripper show that the system is operating as designed and is reducing concentrations of contaminants of concern to below detection limits. In addition to HCS operation, this PMR also discusses performance monitoring that has been implemented to assess progress of the HCS IM and overall plume conditions through scheduled groundwater (quarterly and semi-annual) and sub-slab soil gas (quarterly) sampling and analysis. Two ambient air samples were also collected on a quarterly basis in the vicinity of the modular structure and the paved driveway east of the Solvent Reclamation Area during routine operation and maintenance (O&M) activities to ensure safe breathing zone air quality for on-site personnel. All sub-slab soil gas and ambient air sampling conducted during the Year 4 operational period showed results below applicable regulatory air screening limits. Predictions made during the Year 2 groundwater model updates were in close correlation to post Year 4 plume conditions. A supplemental DPT study conducted in 2022 and 2023. This study indicated that low-concentration plume conditions, where concentrations exceed State of Florida Groundwater Cleanup Target Levels, expanded westward to Kennedy Parkway North and northward to the vicinity of the railroad tracks. Based on these results, recommendations were made to install 14 wells to monitor the downgradient and boundary conditions of the expanded LCP. The contents of this Year 4 PMR were presented during the November 2023 KSC Remediation Team meeting, where Team consensus was reached on several items including continued O&M of the HCS, and continued monitoring of groundwater, ambient air, and sub-slab soil gas. Sampling for per- and polyfluoroalkyl substances at CRCA is ongoing and will be submitted under separate cover.

K. Alex Murphy↗

Reactions Involving Calcium and Magnesium Sulfates as Potential Sources of Sulfur Dioxide During MSL SAM Evolved Gas Analyses

The Sample Analysis at Mars (SAM) and Chemistry and Mineralogy (CheMin) instruments on the Mars Science Laboratory (MSL) have analyzed several subsamples of <150 micron fines from ten sites at Gale Crater. Three were in Yellowknife Bay: the Rocknest aeolian bedform (RN) and drilled Sheepbed mudstone from sites John Klein (JK) and Cumberland (CB). One was drilled from the Windjana (WJ) site on a sandstone of the Kimberly formation. Four were drilled from sites Confidence Hills (CH), Mojave (MJ), Telegraph Peak (TP) and Buckskin (BK) of the Murray Formation at the base of Mt. Sharp. Two were drilled from sandstones of the Stimson formation targeting relatively unaltered (Big Sky, BY) and then altered (Greenhorn, GH) material associated with a light colored fracture zone. CheMin analyses provided quantitative sample mineralogy. SAM's evolved gas analysis mass spectrometry (EGA-MS) detected H2O, CO2, O2, H2, SO2, H2S, HCl, NO, and other trace gases. This contribution will focus on evolved SO2. All samples evolved SO2 above 500 C. The shapes of the SO2 evolution traces with temperature vary between samples but most have at least two "peaks' within the wide high temperature evolution, from approx. 500-700 and approx. 700-860 C (Fig. 1). In many cases, the only sulfur minerals detected with CheMin were Ca sulfates (e.g., RN and GH), which should thermally decompose at temperatures above those obtainable by SAM (>860 C). Sulfides or Fe sulfates were detected by CheMin (e.g., CB, MJ, BK) and could contribute to the high temperature SO2 evolution, but in most cases they are not present in enough abundance to account for all of the SO2. This additional SO2 could be largely associated with x-ray amorphous material, which comprises a significant portion of all samples. It can also be attributed to trace S phases present below the CheMin detection limit, or to reactions which lower the temperatures of SO2 evolution from sulfates that are typically expected to thermally decompose at temperatures outside the SAM temperature range (e.g., Ca and Mg sulfates). Here we discuss the results of SAM-like laboratory analyses targeted at understanding this last possibility, focused on understanding if reactions of HCl or an HCl evolving phase (oxychlorine phases, chlorides, etc.) and Ca and Mg sulfates can result in SO2 evolution in the SAM temperature range.

McAdam, A. C.↗

Development of a modulator to measure water vapor selectively in a gaseous mixture

Selective thermal modulation (STM) is a technique which produces a concentration-dependent pulse by selectively modulating a sample in a gas stream. Several types of modulation techniques, both chemical and physical, using adsorption, decomposition, and catalytic and mechanical methods have been developed for use with multiplex gas chromatography. Two of these applications involve selective modulation of the components present in the sample gas stream. The selective modulation of the concentration of specific sample molecules or classes of molecules provides additional analytical selectivity which can lead to selective detection. For some specific applications, the column may even be eliminated. Chemical modulation by absorption of a substance from the sample stream by a stationary phase will also produce a change in the signal intensity. Removal of a substance from the sample stream results in a signal containing a vacancy peak. In the work reported here, a selective thermal modulation technique has been developed as a method for determination of water vapor for possible use in Mars' atmosphere.

NASA Center ARC↗

Preliminary results of investigations into the use of artificial neural networks for discriminating gas chromatograph mass spectra of remote samples

Neural networks trained using mass spectra data from the National Institute of Standards and Technology (NIST) are studied. The investigations also included sample data from the gas chromatograph mass spectrometer (GCMS) instrument aboard the Viking Lander, obtained from the National Space Science Data Center. The work performed to data and the preliminary results from the training and testing of neural networks are described. These preliminary results are presented for the purpose of determining the viability of applying artificial neural networks in discriminating mass spectra samples from remote instrumentation such as the Mars Rover Sample Return Mission and the Cassini Probe.

Geller, Harold A.↗

Ultraviolet atomic emission detector

A device and method are provided for performing qualitative and quantitative elemental analysis through the utilization of a vacuum UV chromatographic detector. The method involves the use of a carrier gas at low pressure. The gas carries a sample to a gas chromatograph column; the column output is directed to a microwave cavity. In this cavity, a low pressure microwave discharge produces fragmentation of the compounds present and generates intense atomic emissions in the vacuum ultraviolet. These emissions are isolated by a monochromator and measured by photometer to establish absolute concentration for the elements.

Braun, W.↗

Design, fabrication, and operation of capsules for the irradiation testing of candidate advanced space reactor fuel pins

Fuel irradiation experiments were designed, built, and operated to test uranium mononitride (UN) fuel clad in tungsten-lined T-111 and uranium dioxide fuel clad in both tungsten-lined T-111 and tungsten-lined Nb-1% Zr. A total of nine fuel pins was irradiated at average cladding temperatures ranging from 931 to 1015 C. The UN experiments, capsules UN-4 and -5, operated for 10,480 and 10,037 hr, respectively, at an average linear heat generation rate of 10 kW/ft. The UO2 experiment, capsule UN-6, operated for 8333 hr at an average linear heat generation rate of approximately 5 kW/ft. Following irradiation, the nine fuel pins were removed from their capsules, externally examined, and sent to the NASA Plum Brook Facility for more detailed postirradiation examination. During visual examination, it was discovered that the cladding of the fuel pin containing dense UN in each of capsules UN-4 and -5 had failed, exposing the UN fuel to the NaK in which the pins were submerged and permitting the release of fission gas from the failed pins. A rough analysis of the fission gas seen in samples of the gas in the fuel pin region indicated fission gas release-to-birth rates from these fuel pins in the range of .00001.

Thoms, K. R.↗