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Developing Mass Spectrometry for Water Quantitation and Volatiles Analysis from In-Situ Regolith

With a revived focus to create a sustainable hu-man presence on the moon, and in preparation for future Mars exploration, it is imperative that all resources are utilized to their fullest potential [1]. In-Situ Resource Utilization (ISRU) will be critical for future mission success as it would enable in-dependent operation of missions while reducing the dependence on the complex supply chain created between the Earth, the moon and Mars. One of the most critical resources that has been identified for ISRU on the lunar surface is water [2]. Water is a versatile resource that can be used in various space operations, such as ra-diation shielding and conversion to oxygen (O2) for propellant [3,4]. One of the most water rich resources is thought to be within the regolith lo-cated in the permanently shadowed regions (PSR) of the Moon; several upcoming missions, such as PRIME-1 and VIPER, are already sched-uled to confirm this hypothesis [5,6]. However, there are currently no missions planned to quanti-fy the abudance of water at these regions. The quantity of water contained in the ice will inform and help the development of future ISRU plants and operation. Water and other volatile gases can be detect-ed upon controlled heating of icy lunar regolith for an accurate quantification of water. This method is similar to thermogravimetric analysis, which was used to analyze Apollo lunar regolith sam-ples. However, losses via sublimation/evaporation or contamination may have occurred with the samples due to the transit and exposure to the terrestrial environment. Furthermore, water would not be expected for these samples since they were not collected from a PSR. Thus, for more accurate results, icy lunar regolith should be ana-lyzed in situ to provide the most representative composition of both water and other volatile gas-es. The Light Water Analysis and Volatile Extract (LightWAVE) project aims to address this knowledge gap. A system has been developed to collect, heat and analyze evolved gases from lu-nar regolith on the lunar surface. The gases will be analyzed by a modified commercial off the shelf (COTS) residual gas analyzer (RGA) quad-rupole mass spectrometer. Evolved gases from heated regolith samples can be identified by the observed mass-to-charge (m/z) ratios, and the peak intensities correlate to the abundances of the observed gases for quantitation. Therefore, our group is developing a calibration methodology utilizing a COTS RGA to quantitate water from in-situ regolith samples on the lunar surface. The partial pressure of water and ideal gas law will be used to quantify the total water evolved from a regolith sample. Here we present our methodol-ogy for the design and calibration for water quan-titation using a COTS RGA.

Nilab Azim↗

DOE OSTI2021

Electron energy distributions in the extended gas nebulae associated with high-z AGN: Maxwell–Boltzmann versus κ distributions

ABSTRACT Emission line observations together with photoionization models provide important information about the ionization mechanisms, densities, temperatures, and metallicities in active galactic nuclei (AGN)-ionized gas. Photoionization models usually assume Maxwell–Boltzmann (M–B) electron energy distributions (EED), but it has been suggested that using κ distributions may be more appropriate and could potentially solve the discrepancies in temperatures and abundances found in HII regions and planetary nebulae. We consider the impact of the presence of κ distributions in photoionized nebulae associated with AGN and study how this might affect spectral modelling and abundance analyses for such regions. Using the photoionization code MAPPINGS 1e, we compute models adopting M–B and κ distributions of electron energies and compare the behaviour of emission line ratios for different values of κ, gas metallicity, density, ionization parameter, and SED slope. We find that the choice of EED can have a large impact on some UV and optical emission lines emitted by photoionized nebulae associated with AGN, and that the impact of adopting a κ distribution is strongly dependent on gas metallicity and ionization parameter. We compile a sample of line ratios for 143 type 2 AGN and compare our models against the observed line ratios. We find that for 98 objects, κ distributions provide a better fit to the observed line ratios than M–B distributions. In addition, we find that adopting κ-distributed electron energies results in significant changes in the inferred gas metallicity and ionization parameter in a significant fraction of objects.

Morais, S. G. (ORCID:0000000200927813)↗

NASA NTRS1985

Multistage open-tube trap for enrichment of part-per-trillion trace components of low-pressure (below 27-kPa) air samples

A multistage open-tube trap for cryogenic collection of trace components in low-pressure air samples is described. The open-tube design allows higher volumetric flow rates than densely packed glass-bead traps commonly reported and is suitable for air samples at pressures below 27 kPa with liquid nitrogen as the cryogen. Gas blends containing 200 to 2500 parts per trillion by volume each of ethane and ethene were sampled and hydrocarbons were enriched with 100 + or - 4 percent trap efficiency. The multistage design is more efficient than equal-length open-tube traps under the conditions of the measurements.

Ohara, D.↗

NASA NTRS1990

Molecular gas and star formation in the centers of Virgo spirals

The CO and H alpha flux distributions for a sample of Virgo spirals were mapped out in an attempt to understand the coupling between gas dynamics and star formation in spiral galaxies. A broad range of morphological types were observed (types Sab through Scd) under the hypothesis that the gas dynamics is most influential in determining the overall appearance of a spiral galaxy. Only non-barred spirals were considered so that the well-studied but complicated properties of bars and their role in inducing star formation would not be a factor. All galaxies were chosen from the Virgo cluster to eliminate uncertainties due to distance errors. Since the dynamical seat of a spiral is at its center, it was expected that the dynamics of the central region would influence global properties of the rest of the disk. This could happen through the existence or absence of an inner Lindblad resonance (according to the degree of central concentration of mass) to modulate swing amplification of spiral waves, or the persistence of an oval distortion to initiate an instability which leads to spiral structure.

Canzian, Blaise↗

NASA NTRS1977

An experimental study of reactive turbulent mixing

An experimental study of two coaxial gas streams, which react very rapidly, was performed to investigate the mixing characteristics of turbulent flow fields. The center stream consisted of a CO-N2 mixture and the outer annular stream consisted of air vitiated by H2 combustion. The streams were at equal velocity (50 m/sec) and temperature (1280 K). Turbulence measurements were obtained using hot film anemometry. A sampling probe was used to obtain time averaged gas compositions. Six different turbulence generators were placed in the annular passage to alter the flow field mixing characteristics. The turbulence generators affected the bulk mixing of the streams and the extent of CO conversion to different degrees. The effects can be related to the average eddy size (integral scale) and the bulk mixing. Higher extents of conversion of CO to CO2 were found be increasing the bulk mixing and decreasing the average eddy size.

Cooper, L. P.↗

NASA NTRS2013

Application of CO2 Snow Jet Cleaning in Conjunction with Laboratory Based Total Reflection X-Ray Fluorescence

The Genesis mission was the first mission returning solar material to Earth since the Apollo program [1,2]. Unfortunately the return of the space craft on September 8, 2004 resulted in a crash landing, which shattered the samples into small fragments and exposed them to desert soil and other debris. Thus only small fragments of the original collectors are available, each having different degrees of surface contamination. Thorough surface cleaning is required to allow for subsequent analysis of solar wind material embedded within. An initial cleaning procedure was developed in coordination with Johnson Space Center which focused on removing larger sized particulates and a thin film organic contamination acquired during collection in space [3]. However, many of the samples have additional residues and more rigorous and/or innovative cleaning steps might be necessary. These cleaning steps must affect only the surface to avoid leaching and re-distribution of solar wind material from the bulk of the collectors. To aid in development and identification of the most appropriate cleaning procedures each sample has to be thoroughly inspected before and after each cleaning step. Laboratory based total reflection X-ray fluorescence (TXRF) spectrometry lends itself to this task as it is a non-destructive and surface sensitive analytical method permitting analysis of elements from aluminum onward present at and near the surface of a flat substrate [4]. The suitability of TXRF has been demonstrated for several Genesis solar wind samples before and after various cleaning methods including acid treatment, gas cluster ion beam, and CO2 snow jet [5 - 7]. The latter one is non-invasive and did show some promise on one sample [5]. To investigate the feasibility of CO2 snow jet cleaning further, several flown Genesis samples were selected to be characterized before and after CO2 snow application with sample 61052 being discussed below.

Schmeling, M.↗

NASA NTRS1999

Sample Acquisition Techniques for Exobiology Flight Experiments

Exobiology Flight Experiments involve complex analyses conducted in environments far different than those encountered in terrestrial applications. A major part of the analytical challenge is often the selection, acquisition, delivery and, in some cases, processing of a sample suitable for the analytical requirements of the mission. The added complications of severely limited resources and sometimes rigid time constraints combine to make sample acquisition potentially a major obstacle for successful analyses. Potential samples come in a wide range including planetary atmospheric gas and aerosols (from a wide variety of pressures), planetary soil or rocks, dust and ice particles streaming off of a comet, and cemetery surface ice and rocks. Methods to collect and process sample are often mission specific, requiring continual development of innovative concepts and mechanisms. These methods must also maintain the integrity of the sample for the experimental results to be meaningful. We present here sample acquisition systems employed from past missions and proposed for future missions.

Kojiro, Daniel R.↗

NASA NTRS2013

RESOLVE Project

The RESOLVE project is a lunar prospecting mission whose primary goal is to characterize water and other volatiles in lunar regolith. The Lunar Advanced Volatiles Analysis (LAVA) subsystem is comprised of a fluid subsystem that transports flow to the gas chromatograph - mass spectrometer (GC-MS) instruments that characterize volatiles and the Water Droplet Demonstration (WDD) that will capture and display water condensation in the gas stream. The LAVA Engineering Test Unit (ETU) is undergoing risk reduction testing this summer and fall within a vacuum chamber to understand and characterize component and integrated system performance. Testing of line heaters, printed circuit heaters, pressure transducers, temperature sensors, regulators, and valves in atmospheric and vacuum environments was done. Test procedures were developed to guide experimental tests and test reports to analyze and draw conclusions from the data. In addition, knowledge and experience was gained with preparing a vacuum chamber with fluid and electrical connections. Further testing will include integrated testing of the fluid subsystem with the gas supply system, near-infrared spectrometer, WDD, Sample Delivery System, and GC-MS in the vacuum chamber. This testing will provide hands-on exposure to a flight forward spaceflight subsystem, the processes associated with testing equipment in a vacuum chamber, and experience working in a laboratory setting. Examples of specific analysis conducted include: pneumatic analysis to calculate the WDD's efficiency at extracting water vapor from the gas stream to form condensation; thermal analysis of the conduction and radiation along a line connecting two thermal masses; and proportional-integral-derivative (PID) heater control analysis. Since LAVA is a scientific subsystem, the near-infrared spectrometer and GC-MS instruments will be tested during the ETU testing phase.

Parker, Ray↗

DOE OSTI2020

Reduced methane recovery at high pressure due to methane trapping in shale nanopores

By 2050, shale gas production is expected to exceed three-quarters of total US natural gas production. However, current unconventional hydrocarbon gas recovery rates are only around 20%. Maximizing production of this natural resource thus necessitates improved understanding of the fundamental mechanisms underlying hydrocarbon retention within the nanoporous shale matrix. In this study, we integrated molecular simulation with high-pressure small-angle neutron scattering (SANS), an experimental technique uniquely capable of characterizing methane behavior in situ within shale nanopores at elevated pressures. Samples were created using Marcellus shale, a gas-generative formation comprising the largest natural gas field in the United States. Our results demonstrate that, contrary to the conventional wisdom that elevated drawdown pressure increases methane recovery, a higher peak pressure led to the trapping of dense, liquid-like methane in sub-2 nm radius nanopores, which comprise more than 90% of the measured nanopore volume, due to irreversible deformation of the kerogen matrix. These findings have critical implications for pressure management strategies to maximize hydrocarbon recovery, as well as broad implications for fluid behavior under confinement.

58 GEOSCIENCES↗

NASA NTRS2012

RESOLVE Project

The RESOLVE project is a lunar prospecting mission whose primary goal is to characterize water and other volatiles in lunar regolith. The Lunar Advanced Volatiles Analysis (LAVA) subsystem is comprised of a fluid subsystem that transports flow to the gas chromatograph- mass spectrometer (GC-MS) instruments that characterize volatiles and the Water Droplet Demonstration (WDD) that will capture and display water condensation in the gas stream. The LAVA Engineering Test Unit (ETU) is undergoing risk reduction testing this summer and fall within a vacuum chamber to understand and characterize C!Jmponent and integrated system performance. Ray will be assisting with component testing of line heaters, printed circuit heaters, pressure transducers, temperature sensors, regulators, and valves in atmospheric and vacuum environments. He will be developing procedures to guide these tests and test reports to analyze and draw conclusions from the data. In addition, he will gain experience with preparing a vacuum chamber with fluid and electrical connections. Further testing will include integrated testing of the fluid subsystem with the gas supply system, near-infrared spectrometer, WDD, Sample Delivery System, and GC-MS in the vacuum chamber. This testing will provide hands-on exposure to a flight forward spaceflight subsystem, the processes associated with testing equipment in a vacuum chamber, and experience working in a laboratory setting. Examples of specific analysis Ray will conduct include: pneumatic analysis to calculate the WOO's efficiency at extracting water vapor from the gas stream to form condensation; thermal analysis of the conduction and radiation along a line connecting two thermal masses; and proportional-integral-derivative (PID) heater control analysis. In this Research and Technology environment, Ray will be asked to problem solve real-time as issues arise. Since LAVA is a scientific subsystem, Ray will be utilizing his chemical engineering background to operate the near-infrared spectrometer and GC-MS instruments during ETU testing. Ray will be working with Modified Commercial off the Shelf (MCOTS) instruments and characterizing their analytical behavior for optimization. Ray will be offered the opportunity to suggest testing modifications or configuration changes at any time to improve the experimental effectiveness. He will gain many skills needed for working in a technical team setting requiring flexibility and critical thinking.

Parker, Ray O.↗

NASA NTRS1977

An experimental study of reactive turbulent mixing

An experimental study of the turbulent mixing of two coaxial gas streams, which react very rapidly (pseudo-hypergolic chemical kinetics), was performed to investigate the mixing characteristics of turbulent flow fields. The center stream consisted of a CO-N2 mixture and the outer annular stream consisted of air vitiated by H2 combustion. The streams were at equal velocity (50 m/sec) and temperature (1280 K). Turbulence measurements were obtained using hot film anemometry. A sampling probe was used to obtain time averaged gas compositions. Six different turbulence generators were placed in the annular passage to alter the flow field mixing characteristics. The turbulence generators affected the bulk mixing of the streams and the extent of CO conversion to different degrees. The effects can be related to the average eddy size and the bulk mixing. Higher extents of conversion of CO to CO2 were found by increasing the bulk mixing and decreasing the average eddy size.

Cooper, L. P.↗

NASA NTRS2019

Correlation between SFR Surface Density and Thermal Pressure of Ionized Gas in Local Analogs of High-redshift Galaxies

We explore the relation between the star formation rate (SFR) surface density (integration of SFR) and the interstellar gas pressure for nearby compact starburst galaxies. The sample consists of 17 green peas and 19 Lyman break analogs (LBAs). Green peas are nearby analogs of Ly alpha emitters at high redshift and LBAs are nearby analogs of Lyman break galaxies at high redshift. We measure the sizes of green peas using Hubble Space Telescope Cosmic Origins Spectrograph near-UV images with a spatial resolution of approximately 0.05 arcsec. We estimate the gas thermal pressure in H II regions by P equals N (sub total)Tk (sub B) approximately or equal to 2n (sub e)Tk (sub B). The electron density is derived using the [S II] doublet at 6716,6731 Angstroms and the temperature is calculated from the [O III] lines. The correlation is characterized by the integration of SFR equals 2.40 times 10 (sup -3) times solar mass per year per square kiloparsec times ((P divided by k (sub B)) divided by (10 ( sup 4) per cubic centimeter times K)) times (sup 1.33). Green peas and LBAs have high integration of SFR up to 1.2 solar masses per year per square kiloparsec and high thermal pressure in the H II region up to P divided by k (sub B) approximating 10 (sup 7.2) K cubic centimeters. These values are at the highest end of the range seen in nearby starburst galaxies. The high gas pressure and the correlation are in agreement with those found instar-forming galaxies at redshift approximating 2.5. These extreme pressures are shown to be responsible for driving galactic winds in nearby starbursts. These outflows may be crucial in enabling Ly alpha and Lyman-continuum to escape.

Galaxies: Evolution↗

NASA NTRS2014

Reduced and Oxidized Sulfur Compounds Detected by Evolved Gas Analyses of Materials from Yellowknife Bay, Gale Crater, Mars

Sulfate minerals have been directly detected or strongly inferred from several Mars datasets and indicate that aqueous alteration of martian surface materials has occurred. Indications of reduced sulfur phases (e.g., sulfides) from orbital and in situ investigations of martian materials have been fewer in number, but these phases are observed in martian meteorites and are likely because they are common minor phases in basaltic rocks. Here we discuss potential sources for the S-bearing compounds detected by the Mars Science Laboratory (MSL) Sample Analysis at Mars (SAM) instrument’s evolved gas analysis (EGA) experiments.

McAdam, A. C.↗

NASA NTRS1978

Chemical alterations of the Holbrook chondrite resulting from terrestrial weathering

Major, minor and trace element analysis as well as noble gas measurements were performed on three Holbrook chondrite samples collected fresh in 1912, in 1931, and in 1968. Decreases in metallic iron and MgO and an increase in total iron were detected. Elemental concentrations of Ti, Ca, Al, P, Mn, Ni, and Cr did not change significantly during weathering. While sodium might have been lost, and K slightly enriched, the trace elements C, Rb, and Sr increased at least two-fold during weathering. Gas abundances decreased, and the concentration ratios of noble gas nuclides varied unpredictably.

Gibson, E. K., Jr.↗

NASA NTRS2004

Evaluation of the Paratrend Multi-Analyte Sensor for Potential Utilization in Long-Duration Automated Cell Culture Monitoring

BACKGROUND: Compact and automated sensors are desired for assessing the health of cell cultures in biotechnology experiments. While several single-analyte sensors exist to measure culture health, a multi-analyte sensor would simplify the cell culture system. One such multi-analyte sensor, the Paratrend 7 manufactured by Diametrics Medical, consists of three optical fibers for measuring pH, dissolved carbon dioxide (pCO(2)), dissolved oxygen (pO(2)), and a thermocouple to measure temperature. The sensor bundle was designed for intra-vascular measurements in clinical settings, and can be used in bioreactors operated both on the ground and in NASA's Space Shuttle and International Space Station (ISS) experiments. METHODS: A Paratrend 7 sensor was placed at the outlet of a bioreactor inoculated with BHK-21 (baby hamster kidney) cells. The pH, pCO(2), pO(2), and temperature data were transferred continuously to an external computer. Cell culture medium, manually extracted from the bioreactor through a sampling port, was also assayed using a bench top blood gas analyzer (BGA). RESULTS: Two Paratrend 7 sensors were used over a single cell culture experiment (64 days). When compared to the manually obtained BGA samples, the sensor had good agreement for pH, pCO(2), and pO(2) with bias (and precision) 0.005(0.024), 8.0 mmHg (4.4 mmHg), and 11 mmHg (17 mmHg), respectively for the first two sensors. A third Paratrend sensor (operated for 141 days) had similar agreement (0.02+/-0.15 for pH, -4+/-8 mm Hg for pCO(2), and 24+/-18 mmHg for pO(2)). CONCLUSION: The resulting biases and precisions are com- parable to Paratrend sensor clinical results. Although the pO(2) differences may be acceptable for clinically relevant measurement ranges, the O(2) sensor in this bundle may not be reliable enough for the ranges of pO(2) in these cell culture studies without periodic calibration.

Validation Studies↗

NASA NTRS1992

Huygens/ACP: An instrument for aerosols chemical composition measurements

The Aerosol Collector Pyrolyzer (ACP) which will be used aboard the Huygens probe is introduced. The scientific objectives, scientific rationale, and a technical description of the ACP are given. The ACP will sample the aerosols of the Titan's atmosphere in two regions, 160 to 60 and 60 to 25 km, respectively. In the first region, it will collect aerosol particles absorbed by a complex core (organic polymers) coated with absorbed or condensed molecules. The second collect will sample larger aerosols and the N2-CH4 droplets. In each sampling, the particles are collected on a metallic filter through which the atmospheric gas is pumped. The filter is then inserted into an oven connected to the Gas Chromatograph Mass Spectrometer (GCMS) Experiment which analyzes the gases produced during the heating of the samples. For each sample it will be possible to bring information on the nature and abundance of the volatile components contained in the particles and/or the composition of the photochemical core.

Israel, Guy↗

NASA NTRS2000

BUNDLE: A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

NASA Marshall Space Flight Center has developed a novel directional solidification furnace prototype for processing metals and alloys experiments in a microgravity environment. The BUNDLE (Bridgman Unidirectional Dendrite in Liquid Experiment) furnace is intended to accommodate the science requirements of Flight Definition Principle Investigators studying cellular/dendritic growth in aluminum and lead alloys at processing temperatures up to 1200 C. The furnace implements a number of innovative features to achieve high thermal gradients and quench rates in a low-power, light-weight design. These include a pyrolytic boron nitride/graphite composite heating element surrounded by layers of self-supporting refractory metal shielding, and a graphite fiber enhanced cold zone allowing high levels of heat extraction from the sample crucible. Novel to the BUNDLE design is an in-situ helium gas quench capability that ensures rapid freezing of the solidifying region (mushy zone) of the metal sample within the furnace without sample disturbance prior to quenching; this is a stringent requirement for subsequent analysis and understanding of microstructural development. The experiment hardware concept features multiple furnaces that may be "bundled" together so many samples, currently up to eight, can be processed at one time. The design of BUNDLE is flexible enough to be implemented on the Shuttle and Space Station in a number of locations (SpaceHab, Express Rack, MPESS, ISPR, etc). BUNDLE prototype furnaces have directionally solidified and quenched 1cm diameter lead - 5.8 weight percent antimony and aluminum - 4 weight percent copper alloys. Quenching of the mushy zone, as recorded by in-situ thermocouples, occurred on the order of 0.5 seconds or less, a rate within the PI's requirements. Subsequent metallographic examination revealed the solidified microstructure to be, as expected, unidirectional. Both the dendrite tips and the eutectic reaction were planar in nature indicating uniform axial heat flow. Delineation between the growing dendrites and eutectic structure with the "quenched-in" liquid was sharp, attesting to the efficacy of the helium quench. BUNDLE's conception, development, capability, and adaptability are presented (in view of Flight PI's needs and science requirements) through viewgraphs depicting actual hardware, generated thermal analysis, and micrographs prepared from BUNDLE processed, flight-like samples.

Carrasquillo, Edgar J.↗

NASA NTRS2001

BUNDLE - A Novel Furnace for Performing Controlled Directional Solidification Experiments in a Microgravity Environment

Carrasquillo, Edgar J.↗