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All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Optimizing Cryo-Focused Pyrolysis GC/MS for Tracing Soil Organic Matter Across Diverse Ecosystems

The cycling of organic matter in terrestrial soils and sediments is central to a range of biogeochemical processes that regulate nutrient cycling, crop productivity, trace gas emissions, and contaminant transport. Pyrolysis-gas chromatography/mass spectrometry (py-GC/MS) is a powerful tool for characterizing bulk soil organic matter (SOM) at the molecular level. In this study, we used a cryo-focused py-GC/MS system to analyze soil samples from seven diverse ecosystems: vernal pool, prairie pothole, temperate forest, tropical forest, tundra, wildfire-affected boreal forest, and grassland. We addressed a key bottleneck in molecular-level SOM characterization by developing an automated data analysis pipeline to optimize py-GC/MS and complementary evolved gas analysis/mass spectrometry (EGA/MS) methods, incorporating advanced tools for peak deconvolution, developing a custom compound class library, and implementing fragmentation spectrum-based molecular networking for the first time. This improved workflow was applied to soil samples from all seven ecosystems, including multiple depths and density fractions. Our findings demonstrate that ecosystem type plays a dominant role in shaping compositional differences in SOM. We also identified trends in the source of SOM compounds (e.g., microbial vs plantderived) across soil depth and density fractions, which are critical for understanding persistence and turnover of SOM. Our molecular networking analysis indicated that although many compounds are widespread across ecosystems, others are restricted to specific environments, such as wetlands. This underscores the utility of molecular-level data in elucidating the complexity of SOM composition and the environmental drivers that shape it. Such molecular-level insights can deepen our knowledge of biogeochemical SOM cycles.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2013

Evidence for Perchlorates and the Origin of Chlorinated Hydrocarbons Detected by SAM at the Rocknest Aeolian Deposit in Gale Crater

Four individual sample portions from a single scoop of the Rocknest aeolian deposit were sieved ( 150 m) and delivered to the Sample Analysis at Mars (SAM) instrument by the Mars Science Laboratory rover's sample acquisition system. The samples were analyzed separately by the SAM pyrolysis evolved gas and gas chromatography mass spectrometry analysis modes. Several chlorinated hydrocarbons including chloromethane, dichloromethane, trichloromethane, a chloromethylpropene, and chlorobenzene were identified by SAM above background levels with abundances of 0.01 to 2.3 nanomole.The evolution of the chloromethanes observed during pyrolysis is coincident with the increase in O2 released from the Rocknest sample and the decomposition of a product of N-methyl-N- (tert-butyldimethylsilyl)trifluoroacetamide (MTBSTFA), a chemical that leaked from a derivatization cup inside SAM.The best candidate for the oxychloride phase in Rocknest is a hydrated calcium perchlorate (Ca(ClO4)2nH2O), based on the temperature release of O2 that correlates with the release of the chlorinated species measured by SAM, although other chlorine bearing phases are being considered. Laboratory pyrolysis experiments suggest that reaction of martian chlorine with organic carbon from MTBSTFA can explain the presence of the chloromethanes and a chloromethylpropene also detected by SAM.However, we cannot exclude the possibility that traces of organic carbon of either martian or exogenous origin contributed to some of the chloromethanes measured by SAM. Although the alteration history and exposure age of the Rocknest deposit is unknown, it is possible that oxidative degradation of complex organic matter by ionizing radiation or other chemical processes in Rocknest has occurred.

Mars Rover↗
NASA NTRS2013

Evidence for Perchlorates and the Origin of Chlorinated Hydrocarbons Detected by SAM at the Rocknest Aeolian Deposit in Gale Crater

A single scoop of the Rocknest aeolian deposit was sieved (less than 150 micrometers), and four separate sample portions, each with a mass of approximately 50 mg, were delivered to individual cups inside the Sample Analysis at Mars (SAM) instrument by the Mars Science Laboratory rover's sample acquisition system. The samples were analyzed separately by the SAM pyrolysis evolved gas and gas chromatograph mass spectrometer analysis modes. Several chlorinated hydrocarbons including chloromethane, dichloromethane, trichloromethane, a chloromethylpropene, and chlorobenzene were identified by SAM above background levels with abundances of approximately 0.01 to 2.3 nmol. The evolution of the chloromethanes observed during pyrolysis is coincident with the increase in O2 released from the Rocknest sample and the decomposition of a product of N-methyl-N-(tert-butyldimethylsilyl)-trifluoroacetamide (MTBSTFA), a chemical whose vapors were released from a derivatization cup inside SAM. The best candidate for the oxychlorine compounds in Rocknest is a hydrated calcium perchlorate (Ca(ClO4)2·nH2O), based on the temperature release of O2 that correlates with the release of the chlorinated hydrocarbons measured by SAM, although other chlorine-bearing phases are being considered. Laboratory analog experiments suggest that the reaction of Martian chlorine from perchlorate decomposition with terrestrial organic carbon from MTBSTFA during pyrolysis can explain the presence of three chloromethanes and a chloromethylpropene detected by SAM. Chlorobenzene may be attributed to reactions of Martian chlorine released during pyrolysis with terrestrial benzene or toluene derived from 2,6-diphenylphenylene oxide (Tenax) on the SAM hydrocarbon trap. At this time we do not have definitive evidence to support a nonterrestrial carbon source for these chlorinated hydrocarbons, nor do we exclude the possibility that future SAM analyses will reveal the presence of organic compounds native to the Martian regolith.

sample analysis at mars↗
NASA NTRS1993

Differential Scanning Calorimetry (DSC) for planetary surface exploration

Differential Scanning Calorimetry (DSC) is the quantitative measurement of the enthalpic response of a material to a systematic change in temperature. In practice, the heat flow into or outward from a sample is measured as the sample is heated or cooled at a carefully controlled rate. DSC superficially resembles, but is not the same as differential thermal analysis (DTA), which is the measurement of temperature differences between a sample and reference material as the pair is heated or cooled. The fundamental properties measured by DSC are enthalpies and temperatures of phase transitions and constant-pressure heat capacities. Depending on instrument design and the nature of the sample, high-quality DSC analyses can be obtained on only a few milligrams of solid materials. DSC requires direct contact with the sample and generally degrades, if not destroys, the sample as a consequence of heating. In laboratory applications, it is common to subject the gaseous effluent from the DSC to analysis by a separate evolved-gas analyzer (EGA).

Gooding, James L.↗
NASA NTRS2019

Origin and Speciation of Sulfur Compounds in the Murray Formation, Gale Crater, Mars

The Mars Curiosity rover has traversed nearly 20 km and gained over 350 meters in elevation since landing in Gale crater in August 2012. Through 2250 sols of surface operations, Curiosity has spent approximately 60% of its time investigating the Murray formation, a unit of layered sediments. The occurrence of sulfur compounds in the Murray formation has been established by imaging of light-toned veins by MastCam and MAHLI, chemical compositions measured by the Alpha Particle X-ray Spectrometer (APXS) and ChemCam, crystalline phase identifications by the CheMin X-ray diffractometer, and evolved gas analyses from the Sample Analysis at Mars (SAM) instrument.

Yen, A. S.↗
NASA NTRSDate not supplied

Mineralogical Trends Over the Clay-Sulfate Transition in Gale Crater from the Mars Science Laboratory CheMin Instrument

The Mars Science Laboratory Curiosity rover landed in Gale crater in 2012 to explore a sedimentary sequence in lower Aeolis Mons (informally known as Mount Sharp)that shows changes in mineralogy from orbital visible/near-infrared reflectance spectroscopy[1]. Sedimentary layers with spectral signatures of hydrated Mg sulfate overly layers with signatures of Fe/Mg smectite, a mineralogical stratigraphy that is seen in other ancient sedimentary rocks across Mars[e.g., 2-4]. Curiosity recently completed its campaign in a valley with a strong orbital signature of smectite, named Glen Torridon. Mineralogical measurements by the CheMin X-ray diffractometer(XRD), complemented by evolved gas analyses by the Sample Analysis at Mars (SAM) instrument suite, allowed the identification of abundant Fe3+-bearing dioctahedral smectite (i.e., nontronite) in Glen Torridon [5-6]. Curiosity left Glen Torridon in February 2021 and began traversing through a “clay-sulfate transition” zone on the way to the pediment and the sulfate unit[e.g., 7]. This clay-sulfate transition is defined in orbital reflectance spectroscopy as having a weak signature of hydrated Mg sulfate. Curiosity has drilled five outcrops over the traverse through the clay-sulfate transition and delivered the rock powders to CheMin for mineralogical analysis. Here, we report on the mineral assemblages of those five targets derived from CheMin XRD patterns and discuss mineralogical trends as the rover approaches the sulfate unit.

Mars↗
NASA NTRS2012

Mass Spectrometers in Space!

Exploration of our solar system over several decades has benefitted greatly from the sensitive chemical analyses offered by spaceflight mass spectrometers. When dealing with an unknown environment, the broadband detection capabilities of mass analyzers have proven extremely valuable in determining the composition and thereby the basic nature of space environments, including the outer reaches of Earth s atmosphere, interplanetary space, the Moon, and the planets and their satellites. Numerous mass analyzer types, including quadrupole, monopole, sector, ion trap, and time-of-flight have been incorporated in flight instruments and delivered robotically to a variety of planetary environments. All such instruments went through a rigorous process of application-specific development, often including significant miniaturization, testing, and qualification for the space environment. Upcoming missions to Mars and opportunities for missions to Venus, Europa, Saturn, Titan, asteroids, and comets provide new challenges for flight mass spectrometers that push to state of the art in fundamental analytical technique. The Sample Analysis at Mars (SAM) investigation on the recently-launch Mars Science Laboratory (MSL) rover mission incorporates a quadrupole analyzer to support direct evolved gas as well as gas chromatograph-based analysis of martian rocks and atmosphere, seeking signs of a past or present habitable environment. A next-generation linear ion trap mass spectrometer, using both electron impact and laser ionization, is being incorporated into the Mars Organic Molecule Analyzer (MOMA) instrument, which will be flown to Mars in 2018. These and other mass spectrometers and mission concepts at various stages of development will be described.

Brinckerhoff, William B.↗
NASA NTRS1974

Effectiveness of solid lubricant coatings for friction in hard vacuum (10-9 tor)

A study was made of the efficiency of solid lubricating coatings, based on MoS2 with various binders, during friction and under highvacuum conditions. Mass spectrometry was used for an analysis of the composition of the gas evolved from the coatings in the friction process. It is shown that the vacuum level, loading, and sliding velocity influence coating effectiveness. In the friction process the solid lubricant coatings yield characteristic decay products associated with the chemical nature of the binders. The mechanism of coating breakdown during friction is associated with the binder breakdown mechanism.

Verkin, B. I.↗
NASA NTRS1996

Planetary Surface Instruments Workshop

This report on planetary surface investigations and planetary landers covers: (1) the precise chemical analysis of solids; (2) isotopes and evolved gas analyses; (3) planetary interiors; planetary atmospheres from within as measured by landers; (4) mineralogical examination of extraterrestrial bodies; (5) regoliths; and (6) field geology/processes.

Meyer, Charles↗
NASA NTRS2014

Characterizing the Phyllosilicate Component of the Sheepbed Mudstone in Gale Crater, Mars Using Laboratory XRD and EGA

The Curiosity rover investigated the mineralogy of the Sheepbed mudstone member of the Yellowknife Bay formation in Gale crater. Data from the Chemistry and Mineralogy (CheMin) X-ray diffractometer (XRD) helped identify phyllosilicates in the two drilled samples, John Klein and Cumberland. These patterns showed peaks at low angles, consistent with (001) peaks in 2:1 swelling phyllosilicates [1]. Evolved gas analyses (EGA) by the Sample Analysis at Mars (SAM) instrument of these samples confirmed the presence of phyllosilicates through the release of H2O at high temperatures, consistent with dehydroxylation of octahedral OH in phyllosilicates [2]. CheMin data for the phyllosilicates at John Klein and Cumberland show that they are structurally similar in that their (02l) peaks are near 22.5 deg 2theta, suggesting both samples contain trioctahedral 2:1 phyllosilicates [1]. However, the positions of the (001) peaks differ: the phyllosilicate at John Klein has its (001) peak at 10 Angstroms, whereas the phyllosilicate at Cumberland has an (001) peak at 14 Angstroms. Such differences in (001) dspacings can be ascribed to the type of cation in the interlayer site [3]. For example, large monovalent cations (e.g., K(+)) have low hydration energies and readily lose their H2O of hydration, whereas small divalent cations (e.g., Mg(2+)) have high energies of hydration and retain H2O in the phyllosilicate interlayers [3,4]. The goal of this study is to determine whether differences in the interlayer cation composition can explain the CheMin data from John Klein and Cumberland and to use this knowledge to better understand phyllosilicate formation mechanisms.

Rampe, E. B.↗
NASA NTRS2018

Amorphous Phase Characterization Through X-Ray Diffraction Profile Modeling: Implications for Amorphous Phases in Gale Crater Rocks and Soils

The CheMin X-ray diffraction instrument on the Mars Science Laboratory rover has analyzed 18 rock and soil samples in Gale crater. Diffraction data allow for the identification of major crystalline phases based on the positions and intensities of well-defined peaks and also provides information regarding amorphous and poorly-ordered materials based on the shape and positions of broad scattering humps. The combination of diffraction data, elemental chemistry from APXS (Alpha Particle X-ray Spectrometer) and evolved gas analyses (EGA) from SAM (Sample Analysis at Mars) help constrain possible amorphous materials present in each sample (e.g., glass, opal, iron oxides, sulfates) but are model dependent. We present a novel method to characterize amorphous material in diffraction data and, through this approach, aim to characterize the phases collectively producing the amorphous profiles in CheMin diffraction data. This method may be applied to any diffraction data from samples containing X-ray amorphous materials, not just CheMin datasets, but we re-strict our discussion to Martian-relevant amorphous phases and diffraction data measured by CheMin or CheMin-like instruments.

Achilles, C. N.↗
NASA NTRS2023

Hydrodynamics of bubble flow through a porous medium with applications to packed bed reactors

Gas-liquid flows through packed bed reactors (PBRs) are challenging to predict due to the tortuous flow paths that fluid interfaces must traverse. Experiments at the International Space Station showed that bubble and pulse flows are predominately observed under microgravity conditions, while the trickle and spray flows observed under terrestrial conditions are not present in microgravity. To understand the physics behind the former experiments, we simulate bubble flow through a PBR for different packing-particle-diameter-based Weber numbers and under different gravity conditions. We demonstrate different pore-scale mechanisms, such as capillary entrapment, buoyancy entrapment, and inertia-induced bubble displacement. Then, we perform a quantitative analysis by introducing new dynamic scales, dependent upon the evolving gas-liquid interfacial area, to understand the dynamic trade-offs between the inertia, capillary, and buoyancy forces on a bubble passing through a PBR. This analysis leads us to define new dimensionless Weber-like numbers that delineate bubble entrapment from bubble displacement.

Pranay P Nagrani↗
NASA NTRS2010

Thermal Properties of Lunar Regolith Simulants

Various high temperature chemical processes have been developed to extract oxygen and metals from lunar regolith. These processes are tested using terrestrial analogues of the regolith. But all practical terrestrial analogs contain H2O and/or OH(-), the presence of which has substantial impact on important system behaviors. We have undertaken studies of lunar regolith simulants to determine the limits of the simulants to validate key components for human survivability during sustained presence on the moon. Differential Thermal Analysis (DTA) yields information on phase transitions and melting temperatures. Themo-Gravimetric Analysis (TGA) with mass spectrometric (MS) determination of evolved gas species yields chemical information on various oxygenated volatiles (water, carbon dioxide, sulfur oxides, nitrogen oxides and phosphorus oxides) and their evolution temperature profiles. The DTA and TGAMS studies included JSC-1A fine, NU-LHT-2M and its proposed feed stocks: anorthosite; dunite; HQ (high quality) glass and the norite from which HQ glass is produced. Fig 1 is a data profile for anorthosite. The DTA (Fig 1a) indicates exothermic transitions at 355 and 490 C and endothermic transitions at 970 and 1235 C. Below the 355 C transition, water (Molecular Weight, MW, 18 in Fig 1c) is lost accounting for approximately 0.1% mass loss due to water removal (Fig 1b). Just above 490 C a second type of water is lost, presumably bound in lattices of secondary minerals. Between 490 and the 970 transition other volatile oxides are lost including those of hydrogen (third water type), carbon (MW = 44), sulfur (MW = 64 and 80), nitrogen (MW 30 and 46) and possibly phosphorus (MW = 79, 95 or 142). Peaks at MW = 35 and 19 may be attributable to loss of chlorine and fluorine respectively. Negative peaks in the NO (MW = 30) and oxygen (MW = 32) MS profiles may indicate the production of NO2 (MW = 46). Because so many compounds are volatilized in this temperature range quantification of the mass loss associated with individual species is difficult. Similar information will be presented for the other materials studied in this investigation.

Street, Kenneth↗
NASA NTRS2010

Performance Testing of Molten Regolith Electrolysis with Transfer of Molten Material for the Production of Oxygen and Metals on the Moon

Previously, we have demonstrated the production of oxygen by electrolysis of molten regolith simulants at temperatures near 1600 C. Using an inert anode and suitable cathode, direct electrolysis (no supporting electrolyte) of the molten silicate is carried out, resulting in the production of molten metallic products at the cathode and oxygen gas at the anode. Initial direct measurements of current efficiency have confirmed that the process offer potential advantages of high oxygen production rates in a smaller footprint facility landed on the moon, with a minimum of consumables brought from Earth. We now report the results of a scale-up effort toward the goal of achieving production rates equivalent to 1 metric ton O2/year, a benchmark established for the support of a lunar base. We previously reported on the electrochemical behavior of the molten electrolyte as dependent on anode material, sweep rate and electrolyte composition in batches of 20-200g and at currents of less than 0.5 A. In this paper, we present the results of experiments performed at currents up to 10 Amperes) and in larger volumes of regolith simulant (500 g - 1 kg) for longer durations of electrolysis. The technical development of critical design components is described, including: inert anodes capable of passing continuous currents of several Amperes, container materials selection, direct gas analysis capability to determine the gas components co-evolving with oxygen. To allow a continuous process, a system has been designed and tested to enable the withdrawal of cathodically-reduced molten metals and spent molten oxide electrolyte. The performance of the withdrawal system is presented and critiqued. The design of the electrolytic cell and the configuration of the furnace were supported by modeling the thermal environment of the system in an effort to realize a balance between external heating and internal joule heating. We will discuss the impact these simulations and experimental findings have on the design of a suitable prototype for lunar applications

Sibille, Laurent↗
NASA NTRS2010

Thermal Properties of Lunar Regolith Simulants

Various high temperature chemical processes have been developed to extract oxygen and metals from lunar regolith. These processes are tested using terrestrial analogues of the regolith. But all practical terrestrial analogs contain H2O and/or OH-, the presence of which has substantial impact on important system behaviors. We have undertaken studies of lunar regolith simulants to determine the limits of the simulants to validate key components for human survivability during sustained presence on the moon. Differential Thermal Analysis (DTA) yields information on phase transitions and melting temperatures. Themo-Gravimetric Analysis (TGA) with mass spectrometric (MS) determination of evolved gas species yields chemical information on various oxygenated volatiles (water, carbon dioxide, sulfur oxides, nitrogen oxides and phosphorus oxides) and their evolution temperature profiles. The DTA and TGAMS studies included JSC-1A fine, NU-LHT-2M and its proposed feed stocks: anorthosite; dunite; HQ (high quality) glass and the norite from which HQ glass is produced. Fig 1 is a data profile for anorthosite. The DTA (Fig 1a) indicates exothermic transitions at 355 and 490 C and endothermic transitions at 970 and 1235 C. Below the 355 C transition, water (Molecular Weight, MW, 18 in Fig 1c) is lost accounting for approximately 0.1% mass loss due to water removal (Fig 1b). Just above 490 C a second type of water is lost, presumably bound in lattices of secondary minerals. Between 490 and the 970 transition other volatile oxides are lost including those of hydrogen (third water type), carbon (MW = 44), sulfur (MW = 64 and 80), nitrogen (MW 30 and 46) and possibly phosphorus (MW = 79, 95 or 142). Peaks at MW = 35 and 19 may be attributable to loss of chlorine and fluorine respectively. Negative peaks in the NO (MW = 30) and oxygen (MW = 32) MS profiles may indicate the production of NO2 (MW = 46). Because so many compounds are volatilized in this temperature range quantification of the mass loss associated with individual species is difficult. Similar information will be presented for the other materials studied in this investigation.

Street, Kenneth↗
NASA NTRS1991

Combined Backscatter Moessbauer Spectrometer and X Ray Fluorescence analyzer (BaMS/XRF) for planetary surface materials

A backscatter Moessbauer spectrometer (BaMS) with included x ray fluorescence (XRF) capability for the Mars Environment Survey (MESUR) Mission, which has been proposed by NASA for 1998, is being developed. The instrument will also be suitable for other planetary missions such as those to the Moon, asteroids, and other solid solar-system objects. The BaMS would be unique for MESUR in providing information about iron mineralogy in rocks, clays, and other surface materials, including relative proportions of iron-bearing minerals. It requires no sample preparation and can identify all the normal oxidation states of iron (3+, 2+, 0). Thus, BaMS is diagnostic for weathering and other soil-forming processes. Backscatter design allows the addition of XRF elemental analysis with little or no modification. The BaMS/XRF instrument complements the thermal analyzer with evolved gas analyzer (TA-EGA) and the alpha-proton x-ray spectrometer (APXS) proposed (along with BaMS) for geochemical analysis on MESUR.

Agresti, D. G.↗
NASA NTRS2002

Glenn-HT: The NASA Glenn Research Center General Multi-Block Navier Stokes Heat Transfer Code

For the last several years, Glenn-HT, a three-dimensional (3D) Computational Fluid Dynamics (CFD) computer code for the analysis of gas turbine flow and convective heat transfer has been evolving at the NASA Glenn Research Center. The code is unique in the ability to give a highly detailed representation of the flow field very close to solid surfaces in order to get accurate representation of fluid beat transfer and viscous shear stresses. The code has been validated and used extensively for both internal cooling passage flow and for hot gas path flows, including detailed film cooling calculations and complex tip clearance gap flow and heat transfer. In its current form, this code has a multiblock grid capability and has been validated for a number of turbine configurations. The code has been developed and used primarily as a research tool, but it can be useful for detailed design analysis. In this presentation, the code is described and examples of its validation and use for complex flow calculations are presented, emphasizing the applicability to turbomachinery.

Gaugler, Raymond E.↗
NASA NTRS2001

Glenn-HT: The NASA Glenn Research Center General Multi-Block Navier-Stokes Heat Transfer Code

For the last several years, Glenn-HT, a three-dimensional (3D) Computational Fluid Dynamics (CFD) computer code for the analysis of gas turbine flow and convective heat transfer has been evolving at the NASA Glenn Research Center. The code is unique in the ability to give a highly detailed representation of the flow field very close to solid surfaces in order to get accurate representation of fluid heat transfer and viscous shear stresses. The code has been validated and used extensively for both internal cooling passage flow and for hot gas path flows, including detailed film cooling calculations and complex tip clearance gap flow and heat transfer. In its current form, this code has a multiblock grid capability and has been validated for a number of turbine configurations. The code has been developed and used primarily as a research tool, but it can be useful for detailed design analysis. In this paper, the code is described and examples of its validation and use for complex flow calculations are presented, emphasizing the applicability to turbomachinery for space launch vehicle propulsion systems.

Gaugler, Raymond E.↗