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NASA NTRS1998

Mars Volatiles and Climate Surveyor (MVACS) Integrated Payload for the Mars Polar Lander Mission

The Mars Volatiles and Climate Surveyor (MVACS) integrated payload for the Mars Polar Lander will be launched in January 1999, with a scheduled landing on Mars' south-polar layered deposits in December 1999. Over the course of its 90-day nominal mission during the martian southern spring and summer seasons, it will make in situ measurements that will provide new insights into the behavior and distribution of martian volatiles, MVACS consists of four major instrument systems: a surface stereo imager (SSI), which will acquire multispectral stereo images of the surface and atmosphere; a 2-m robotic arm (RA), which will dig a O.5-m deep trench and acquire surface and subsurface samples that will be imaged by a focusable robotic arm camera (RAC), which will take close-up images of surface and subsurface samples at a spatial resolution of 21 micron; a meteorology package (MET), which will make the first measurements of surface pressure, temperature, and winds in Mars' southern hemisphere and employ a tunable diode laser (TDL) spectrometer to measure the water-vapor concentration and isotopic composition of CO2 in the martian atmosphere; and a thermal and evolved gas analyzer (TEGA), which will use differential scanning calorimetry and TDL-evolved gas analysis to determine the concentrations of ices, adsorbed volatiles, and volatile-bearing minerals in surface and subsurface soil samples. The unique in situ measurements made by MVACS at its high-latitude landing site will define a number of important aspects of the physical, isotopic, and chemical nature of the martian near-surface and subsurface environment that will be valuable in better understanding Mars meteorites and returned samples, as well as in the search for martian resources that could be utilized by humans.

Paige, D. A.↗
NASA NTRS2000

The Search for Water and Other Volatiles in Martian Surface Materials: The Thermal Evolved Gas Analyzer (TEGA)

Volatile-bearing minerals and phases (e.g., Fe-oxyhydroxides, phyllosilicates, carbonates, sulfates, palagonites, glasses) may be important components of the Martian regolith. However, essentially no information exists on the mineralogical composition of volatile-bearing phases in the regolith. The Thermal Evolved Gas Analyzer (TEGA), which was part of the Mars Polar Lander payload, was to determine the abundances of two of the most important volatile compounds (i.e., water and carbon dioxide) in the martian soil and to identify the minerals or phases that harbor these volatiles. The TEGA instrument was composed of a differential scanning calorimeter (DSC) interfaced with evolved gas analysis (EGA). The EGA consisted of a Herriott cell of a tunable-diode laser (TDL) spectrometer that determines CO2 and H2O abundances. The sample chamber was to operate at about 100 mbar (-76 torr) with a N2 carrier gas flow of 0.4 sccm. Specifications of TEGA are described in detail elsewhere in this volume.

Ming, D. W.↗
NASA NTRS2002

A Review of Single Source Precursors for the Deposition of Ternary Chalcopyrite Materials

The development of thin-film solar cells on flexible, lightweight, space-qualified durable substrates (i.e. Kapton) provides an attractive solution to fabricating solar arrays with high specific power, (W/kg). The syntheses and thermal modulation of ternary single source precursors, based on the [{LR}2Cu(SR')2In(SR')2] architecture in good yields are described. Thermogravimetric analyses (TGA) and Low temperature Differential Scanning Caloriometry, (DSC) demonstrate that controlled manipulation of the steric and electronic properties of either the group five-donor and/or chalcogenide moiety permits directed adjustment of the thermal stability and physical properties of the precursors. TGA-Evolved Gas Analysis, confirms that single precursors decompose by the initial extrusion of the sulphide moiety, followed by the loss of the neutral donor group, (L) to release the ternary chalcopyrite matrix. X-ray diffraction studies, EDS and SEM on the non-volatile pyrolized material demonstrate that these derivatives afford single-phase CuInS2/CuInSe2 materials at low temperature. Thin-film fabrication studies demonstrate that these single source precursors can be used in a spray chemical vapor deposition process, for depositing CuInS2 onto flexible polymer substrates at temperatures less than 400 C.

Banger, K. K.↗
NASA NTRS2004

Lunar and Planetary Science XXXV: Weird Martian Minerals: Complex Mars Surface Processes

The session "Complex Mars Surface" included the following reports:A Reappraisal of Adsorbed Superoxide Ion as the Cause Behind the Reactivity of the Martian Soils; Sub-Surface Deposits of Hydrous Silicates or Hydrated Magnesium Sulfates as Hydrogen Reservoirs near the Martian Equator: Plausible or Not?; Thermal and Evolved Gas Analysis of Smectites: The Search for Water on Mars; Aqueous Alteration Pathways for K, Th, and U on Mars; Temperature Dependence of the Moessbauer Fraction in Mars-Analog Minerals; Acid-Sulfate Vapor Reactions with Basaltic Tephra: An Analog for Martian Surface Processes; Iron Oxide Weathering in Sulfuric Acid: Implications for Mars; P/Fe as an Aquamarker for Mars; Stable Isotope Composition of Carbonates Formed in Low-Temperature Terrestrial Environments as Martian Analogs; Can the Phosphate Sorption and Occlusion Properties Help to Elucidate the Genesis of Specular Hematite on the Mars Surface?; Sulfate Salts, Regolith Interactions, and Water Storage in Equatorial Martian Regolith; Potential Pathways to Maghemite in Mars Soils: The Key Role of Phosphate; and Mineralogy, Abundance, and Hydration State of Sulfates and Chlorides at the Mars Pathfinder Landing Site.

Source record↗
NASA NTRS2013

Hydrogen Isotopic Composition of Water in the Martian Atmosphere and Released from Rocknest Fines

The Mars Science Laboratory Curiosity rover sampled the aeolian bedform called Rocknest as its first solid samples to be analyzed by the analytical instruments CheMin and SAM. The instruments ingested aliquots from a sieved sample of less than 150 micrometer grains. As discussed in other reports at this conference [e.g., 1], CheMin discovered many crystalline phases, almost all of which are igneous minerals, plus some 10s of percent of x-ray amorphous material. The SAM instrument is focused on understanding volatiles and possible organics in the fines, performing evolved gas analysis (EGA) with the SAM quadrapole mass spectrometer (QMS), isotope measurements using both the QMS and the tunable laser spectrometer (TLS), which is sensitive to CO2, water and methane, and organics with the gas chromatograph mass spectrometer (GCMS). As discussed in the abstract by Franz et al. [2] and others, EGA of Rocknest fines revealed the presence of significant amounts of H2O as well as O-, C- and S-bearing materials. SAM has also tasted the martian atmosphere several times, analyzing the volatiles in both the TLS and QMS [e.g., 3,4]. This abstract will focus on presentation of initial hydrogen isotopic data from the TLS for Rocknest soils and the atmosphere, and their interpretation. Data for CO2 isotopes and O isotopes in water are still being reduced, but should be available by at the conference.

Leshin, L. A.↗
NASA NTRS2013

Coordinated Analyses of Antarctic Sediments as Mars Analog Materials Using Reflectance Spectroscopy and Current Flight-Like Instruments for CheMin, SAM and MOMA

Coordinated analyses of mineralogy and chemistry of sediments from the Antarctic Dry Valleys illustrate how data obtained using flight-ready technology of current NASA and ESA missions can be combined for greater understanding of the samples. Mineralogy was measured by X-ray diffraction (XRD) and visible/ near-infrared (VNIR) reflectance spectroscopy. Chemical analyses utilized a quadrupole mass spectrometer (QMS) to perform pyrolysis-evolved gas analysis (EGA) and gas chromatography-mass spectrometry (GC/MS) both with and without derivatization, as well as laser desorption-mass spectrometry (LD/MS) techniques. These analyses are designed to demonstrate some of the capabilities of near-term landed Mars missions, to provide ground truthing of VNIR reflectance data acquired from orbit by the Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) on MRO and to provide detection limits for surface- operated instruments: the Chemistry and Mineralogy (CheMin) and Sample Analysis at Mars (SAM) instrument suites onboard Mars Science Laboratory (MSL) and the Mars Organic Molecule Analyzer (MOMA) onboard ExoMars-2018. The new data from this study are compared with previous analyses of the sediments performed with other techniques. Tremolite was found in the oxic region samples for the first time using the CheMin-like XRD instrument. The NIR spectral features of tremolite are consistent with those observed in these samples. Although the tremolite bands are weak in spectra of these samples, spectral features near 2.32 and 2.39 micrometers could be detected by CRISM if tremolite is present on the martian surface. Allophane was found to be a good match to weak NIR features at 1.37-1.41, 1.92, and 2.19 micrometers in spectra of the oxic region sediments and is a common component of immature volcanic soils. Biogenic methane was found to be associated with calcite in the oxic region samples by the SAM/EGA instrument and a phosphoric acid derivative was found in the anoxic region sample using the SAM/MTBSTFA technique.

Mars↗
NASA NTRS2020

Detection of Siderite (FeCO3) in Glen Torridon Samples by the Mars Science Laboratory Rover

Siderite (FeCO3) has been detected in Gale Crater for the first time by the Mars Science Laboratory (MSL) Curiosity and is seen in multiple samples in the Glen Torridon (GT) region. The identification of siderite is based on evolved gas analysis (EGA) data from the Sample Analysis at Mars (SAM) instrument and X-ray diffraction (XRD) data from the Chemistry and Mineralogy (CheMin) instrument. Curiosity descended off of the Vera Rubin ridge (VRR) into the Glen Torridon region on Sol 2300. Glen Torridon is of particular interest because a strong clay mineral signature had been detected by orbital instruments [1]. To date, four drilled samples have been collected at two different drill locations: Kilmarie and Aberlady from adjacent blocks at the base of the south side of VRR in the Jura member and Glen Etive 1 and 2 on the same block in the Knockfarril member.

Archer, P. D.↗
NASA NTRS2020

Evidence for Adsorption of Chlorine Species on Iron(III) (hydr)oxides in the Sheepbed Mudstone, Gale Crater, Mars

Chlorine is a widespread element on Mars present in dust, soils and rocks, including the Sheepbed mudstone at Yellowknife Bay, Gale crater. Combined elemental and volatile analyses of two drilled samples, Cumberland and John Klein, indicated that chloride (Cl-) and perchlorate (ClO4 -) are likely present in the mudstone. The nature of chlorine species in Sheepbed mudstone is still not well constrained. It has been proposed that both are present as amorphous or crystalline salts physically mixed with mudstone minerals. We alternatively hypothesize that adsorbed perchlorate and chloride exist in the mudstone and adsorption could occur, in particular, on Fe(III) (hydr)oxide phases as supported by laboratory observations on terrestrial materials. Mineralogical and compositional analyses of the drilled Cumberland mudstone sample revealed the presence of ~30 wt% of a Fe-rich X-ray amorphous phase. Ferrihydrite has been proposed as a component of the Fe-rich X-ray amorphous material. The objectives of this work were to determine adsorption of perchlorate and chloride on ferrihydrite and to enable data comparison by characterizing adsorbed chloride and perchlorate with thermal and evolved gas analysis run under operating conditions similar to the SAM instrument onboard the Curiosity rover.

Peretyazhko, T. S.↗
NASA NTRS2021

Dissolution Rates of Allophane with Variable Fe Contents: Implications for Aqueous Alteration and the Preservation of X-ray Amorphous Materials on Mars

Recent measurements from Mars document X-ray amorphous/nano-crystalline materials in multiple locations across the planet. However, despite their prevalence, little is known about these materials or what their presence implies for the history of Mars. The X-ray amorphous component of the martian soil in Gale crater has an X-ray diffraction pattern that can be partially fit with allophane (approximately Al2O3•(SiO2)1.3-2•(H2O)2.5-3), and the low-temperature water release data are consistent with allophane. The chemical data from Gale crater suggest that other silicate materials similar to allophane, such as Fe-substituted allophane (approximately (Fe2O3)0.01-0.5(Al2O3)0.5-0.99•(SiO2)2•3H2O), may also be present. In order to investigate the properties of these potential poorly crystalline components of the martian soil, Fe-free allophane (Fe:Al = 0), Fe-poor allophane (Fe:Al = 1:99), and Fe-rich allophane (Fe:Al = 1:1) were synthesized and then characterized using electron microscopy and Mars-relevant techniques, including infrared spectroscopy, X-ray diffraction, and evolved gas analysis. Dissolution experiments were performed at acidic (initial pH values pH0 = 3.01, pH0 = 5.04), near-neutral (pH0 = 6.99), and alkaline (pH0 = 10.4) conditions in order to determine dissolution kinetics and alteration phases for these poorly crystalline materials. Dissolution rates (rdiss), based on the rate of Si release into solution, show that these poorly crystalline materials dissolve approximately an order of magnitude faster than crystalline phases with similar compositions at all pH conditions. For Fe-free allophane, logrdiss = -10.65 – 0.15 × pH; for Fe-poor allophane, logrdiss = -10.35 – 0.22 × pH; and for Fe-rich allophane, logrdiss = -11.46 – 0.042 × pH at 25°C, where rdiss has the units of mol m-2 s-1. The formation of incipient phyllosilicate-like phases was detected in Fe-free and Fe-rich allophane reacted in aqueous solutions with pH0 = 10.4 (steady-state pH ≈ 8). Mars-analog instrument analyses demonstrate that Fe-free allophane, Fe-poor allophane, and Fe-rich allophane are appropriate analogs for silicate phases in the martian amorphous soil component. Therefore, similar materials on Mars must have had limited interaction with liquid water since their formation. Combined with chemical changes expected from weathering, such as phyllosilicate formation, the rapid alteration of these poorly crystalline materials may be a useful tool for evaluating the extent of aqueous alteration in returned samples of martian soils.

S J Ralston↗
NASA NTRSDate not supplied

The Chemistry and Mineralogy of Mars Soils: A Tour of Landed Mission Results from the Last 45 years

Eight landed missions demonstrated that martian soils (defined as loose, unconsolidated surface material) consist of basaltic mineralogy, iron (hydr)oxides, amorphous material, sulfate, chloride, (per)chlorate, nitrate, carbonate, and possible organic C. The Viking Lander 1 and 2 (1976), Mars Pathfinder (1997), and Mars Exploration Rover (MER-A,B) (2004) missions determined that martian soil was similar at all landing sites by having mafic chemistry, high S (~ 7 wt.% SO3) and Cl (0.7 wt.%), and spectral detections of poorly crystalline and crystalline Fe-(hydr)oxide phases. The MER Mössbauer spectrometers detected Fe-bearing olivine and pyroxene along with magnetite, nano-phase Fe-oxides (npOx), hematite, and ferric sulfate. The 2008 Phoenix Lander instrumentation measured a soil pH of 7.7 and detected ~0.6 wt.% perchlorate, 3-5 wt.% Ca-rich carbonate and carbon (500 gC/g) consistent with oxidized organics and Fe-rich carbonate. The 2012 Mars Science Laboratory (MSL) rover (Gale Crater) through X-ray diffraction detected plagioclase feldspar, pyroxene, magnetite, hematite, anhydrite, and quartz, with the balance being composed of Si/Fe-containing amorphous (30 to 40 wt.%) material. MSL evolved gas analysis detected (per)chlorate (0.4 wt.% ClO4), nitrate (0.23 wt.%), along with minor Fe/Mg sulfate and oxidized organic C (~2000 gC/g). Limited pedogenesis may have occurred at the 2018 InSight landing site and in one Gusev Crater soil (MER-B) which have 3 to 10 cm-thick duricrust horizons consistent with atmospheric water vapor interactions with soil salts. Martian soil primary mineralogy was derived mostly from local rock (volcanic, sedimentary) that is largely basaltic planet wide. Secondary minerals [e.g., sulfate, chloride, perchlorate, nitrate, carbonate, Fe-(hydr)oxides] in martian soils formed from oxidative aqueous alteration processes and were likely derived from a combination of local sedimentary rock sources and the global bright dust. The Mars 2020 mission will collect soil for Earth return to enable a thorough assessment of the nature and origin of martian soil.

Mars↗
NASA NTRS2013

The Mineralogical and Chemical Case for Habitability at Yellowknife Bay, Gale Crater, Mars

Sediments of the Yellowknife Bay formation (Gale crater) include the Sheepbed member, a mudstone cut by light-toned veins. Two drill samples, John Klein and Cumberland, were collected and analyzed by the CheMin XRD/XRF instrument and the Sample Analysis at Mars (SAM) evolved gas and isotopic analysis suite of instruments. Drill cuttings were also analyzed by the Alpha Particle X-ray Spectrometer (APXS) for bulk composition. The CheMin XRD analysis shows that the mudstone contains basaltic minerals (Fe-forsterite, augite, pigeonite, plagioclase), as well as Fe-oxide/hydroxides, Fe-sulfides, amorphous materials, and trioctahedral phyllosilicates. SAM evolved gas analysis of higher-temperature OH matches the CheMin XRD estimate of ~20% clay minerals in the mudstone. The light-toned veins contain Ca-sulfates; anhydrite and bassanite are detected by XRD but gypsum is also indicated from Mastcam spectral mapping. These sulfates appear to be almost entirely restricted to late-diagenetic veins. The sulfate content of the mudstone matrix itself is lower than other sediments analyzed on Mars. The presence of phyllosilicates indicates that the activity of water was high during their formation and/or transport and deposition (should they have been detrital). Lack of chlorite places limits on the maximum temperature of alteration (likely <100 C). The presence of Ca-sulfates rather than Mg- or Fe-sulfates suggests that the pore water pH was near-neutral and of relatively low ionic strength (although x-ray amorphous Mg-and Fe- sulfates could be present and undetectable by CheMin). The presence of Fe and S in both reduced and oxidized states represents chemical disequilibria that could have been utilized by chemolithoautotrophic biota, if present. When compared to the nearby Rocknest sand shadow mineralogy or the normative mineralogy of Martian soil, both John Klein and Cumberland exhibit a near-absence of olivine and a surplus of magnetite (7-9% of the crystalline component). The magnetite is interpreted as an authigenic product formed when olivine was altered to phyllosilicate. Saponitization of olivine (a process analogous to serpentinization) could have produced H2 in situ. Indeed, early diagenetic hollow nodules ("minibowls") present in the Cumberland mudstone are interpreted by some as forming when gas bubbles accumulated in the unconsolidated mudstone. Lastly, all of these early diagenetic features appear to have been preserved with minimal alteration since their formation, as indicated by the ease of drilling (weak lithification, lack of cementing phases), the presence of 20-30% amorphous material, and the late-stage fracturing with emplacement of calcium sulfate veins and minibowl infills, where they were intersected by veins. A rough estimate of the minimum duration of the lacustrine environment is provided by the minimum thickness of the Sheepbed member. Given 1.5 meters, and applying a mean sediment accumulation rate for lacustrine strata of 1 m/1000 yrs yields a duration of 1,500 years. If the aqueous environments represented by overlying strata are considered, such as Gillespie Lake and Shaler, then this duration increases. The Sheepbed mudstone meets all the requirements of a habitable environment: Aqueous deposition at clement conditions of P, T, pH, Eh and ionic strength, plus the availability of sources of chemical energy.

Blake, David Frederick↗
NASA NTRS2011

delta C-13 Analysis of Mars Analog Carbonates Using Evolved Gas Cavity - Ringdown Spectrometry on the 2010 Arctic Mars Analog Svalbard Expedition (AMASE)

The 2010 Arctic Mars Analog Svalbard Expedition (AMASE) investigated two distinct geologic settings on Svalbard, using instrumentation and techniques in development for future Mars missions, such as the Mars Science Laboratory (MSL), ExoMars, and Mars Sample Return (MSR). The Sample Analysis at Mars (SAM) instrument suite, which will fly on MSL, was developed at Goddard Space Flight Center (GSFC), together with several partners. SAM consists of a quadrupole mass spectrometer (QMS), a gas chromatograph CGC), and a tunable laser spectrometer (TLS), which all analyze gases created by evolved gas analysis (EGA). The two sites studied represent "biotic" and "abiotic" analogs; the "biotic" site being the Knorringfjell fossil methane seep, and the "abiotic" site being the basaltic Sigurdfjell vent complex. The data presented here represent experiments to measure the carbon isotopic composition of carbonates from these two analogs using evolved gas analysis coupled with a commercial cavity ringdown CO2 isotopic analyzer (Picarro) as a proxy for the TLS on SAM.

Stern, J. C.↗
NASA NTRS2019

Mineralogical and Geochemical Trends of the Murray Mudstones, Gale Crater: A Combined Sample Analysis at Mars-Evolved Gas Analyzer and Chemistry and Mineralogy Instrument Assessment

The Murray formation is predominantly composed of lacustrine mudstone that forms the basal layer of Aeolis Mons (informally Mt. Sharp) in Gale Crater, Mars. The Murray formation has distinct iron and sulfur mineralogical variation within its stratigraphy detectable by the Chemistry Mineralogy (Che-Min) instrument consisting of magnetite/hematite in the lower Murray and higher hematite, CaSO4, and smectite content in the upper Murray. The objectives of this work were to evaluate the Sample Analysis at Mars Evolved Gas Analyzer (SAM-EGA) data to 1) Determine what SAM-EGA-detectable phases correlate or do not correlate with the Murray mineralogical composition detected by CheMin and 2) Utilize CheMin/SAM results to propose possible formation scenarios for the observed Murray mudstone mineralogy.

Sutter, B.↗
NASA NTRS2016

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.↗
NASA NTRS2022

Evolved Gas Analyses of Sedimentary Rocks from the Glen Torridon Clay-Bearing Unit, Gale Crater, Mars: Results From the Mars Science Laboratory Sample Analysis at Mars Instrument Suite

Evolved gas analysis (EGA) data from the Sample Analysis at Mars (SAM) instrument suite indicated Fe-rich smectite, carbonate, oxidized organics, Fe/Mg sulfate, and chloride in sedimentary rocks from the Glen Torridon (GT) region of Gale crater that displayed phyllosilicate spectral signatures from orbit. SAM evolved H2O data indicated that the primary phyllosilicate in all GT samples was an Fe-rich dioctahedral smectite (e.g., nontronite) with lesser amounts of a phyllosilicate such as mixed layer talc-serpentine or greenalite-minnesotaite. CO(2) data supported the identification of siderite in several samples, and CO(2) and CO data was also consistent with trace oxidized organic compounds such as oxalate salts. SO(2) data indicated trace and/or amorphous Fe sulfates in all samples and one sample may contain Fe sulfides. SO(2) data points to significant Mg sulfates in two samples, and lesser amounts in several other samples. A lack of evolved O(2) indicated the absence of oxychlorine salts and Mn3+/Mn4+ oxides. The lack of, or very minor, evolved NO revealed absent or very trace nitrate/nitrite salts. HCl data suggested chloride salts in GT samples. Constraints from EGA data on mineralogy and chemistry indicated that the environmental history of GT involved alteration with fluids of variable redox potential, chemistry and pH under a range of fluid-to-rock ratio conditions. Several of the fluid episodes could have provided habitable environmental conditions and carbon would have been available to any past microbes though the lack of significant N could have been a limiting factor for microbial habitability in the GT region.

A. C. McAdam↗
NASA NTRS2013

Detection and Quantification of Nitrogen Compounds in Martian Solid Samples by the Sample Analysis at Mars (SAM) Instrument Suite

The Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) Curiosity Rover detected both reduced and oxidized nitrogen-bearing compounds during the pyrolysis of surface materials from three sites at Gale Crater. Preliminary detections of nitrogen species include NO, HCN, ClCN, CH3CN, and TFMA (trifluoro-Nmethyl-acetamide). On Earth, nitrogen is a crucial bio-element, and nitrogen availability controls productivity in many environments. Nitrogen has also recently been detected in the form of CN in inclusions in the Martian meteorite Tissint, and isotopically heavy nitrogen (delta N-15 approx +100per mille) has been measured during stepped combustion experiments in several SNC meteorites. The detection of nitrogen-bearing compounds in Martian regolith would have important implications for the habitability of ancient Mars. However, confirmation of indigenous Martian nitrogen bearing compounds will require ruling out their formation from the terrestrial derivatization reagents (e.g. N-methyl-N-tert-butyldimethylsilyl-trifluoroacetamide, MTBSTFA and dimethylformamide, DMF) carried for SAM's wet chemistry experiment that contribute to the SAM background. The nitrogen species we detect in the SAM solid sample analyses can also be produced during laboratory pyrolysis experiments where these reagents are heated in the presence of perchlorate, a compound that has also been identified by SAM in Mars solid samples. However, this does not preclude a Martian origin for some of these compounds, which are present in nanomolar concentrations in SAM evolved gas analyses. Analysis of SAM data and laboratory breadboard tests are underway to determine whether nitrogen species are present at higher concentrations than can be accounted for by maximum estimates of nitrogen contribution from MTBSTFA and DMF. In addition, methods are currently being developed to use GC Column 6, (functionally similar to a commercial Q-Bond column), to separate and identify unretained compounds such as NO, N2O, and NO2, which are difficult to detect by EGA-MS due to mass interferences at 30, 44 and 46, respectively. Here we present evolved gas analysis-mass spectrometry (EGA-MS) and gas chromatography mass spectrometry (GC-MS) data on the identification and quantification of these nitrogen-bearing compounds, and suggestions for their origins

Stern, Jennifer C.↗
NASA NTRS2020

JSC-Rocknest: A Large-Scale Mojave Mars Simulant (MMS) Based Soil Simulant for In-Situ Resource Utilization Water-Extraction Studies

The Johnson Space Center-Rocknest (JSC-RN) simulant was developed in response to a need by NASA's Advanced Exploration Systems (AES) In-Situ Resource Utilization (ISRU) project for a simulant to be used in component and system testing for water extraction from Mars regolith. JSC-RN was designed to be chemically and mineralogically similar to material from the aeolian sand shadow named Rocknest in Gale Crater, particularly the 1-3 wt.% low temperature (<450 ºC) water release as measured by the Sample Analysis at Mars (SAM) instrument on the Curiosity rover. Sodium perchlorate, goethite, pyrite, ferric sulfate, regular and high capacity granular ferric oxide, and forsterite were added to a Mojave Mars Simulant (MMS) base in order to match the mineralogy, evolved gases, and elemental chemistry of Rocknest. Mineral and rock components were sent to the United States Geological Survey (USGS) in Denver for mixing. Approximately 800 kg of JSC-RN was sent back to NASA in 5 gallon buckets, which were subsampled and characterized. All samples of the USGS-produced simulants had similar evolved gas profiles as a small prototype batch of JSC-RN made in JSC laboratories, with the exception of HCl, and were similar in terms of mineralogy and total chemistry. Also, all JSC-RN subsamples were homogenous and had similar mineralogy, total chemistry, and low-temperature evolved gas profiles as the Rocknest aeolian sand shadow examined with Curiosity’s instrument suite on Mars. In particular, the low temperature water releases were similar and the amount of water evolved from JSC-RN at <450 ºC was similar to the water content of Rocknest based on SAM water peak integrations. Overall, JSC-RN is ideally suited for ISRU studies of water extraction of global martian soil due to its excellent agreement with measured properties of martian soils and its proven feasibility for large-scale production.

Simulant↗
NASA NTRS2009

Evolved Gas Measurements Planned for the Lower Layers of the Gale Crater Mound with the Sample Analysis at Mars Instrument Suite

The lower mound strata of Gale Crater provide a diverse set of chemical environments for exploration by the varied tools of the Curiosity Rover of the Mars Science Laboratory (MSL) Mission. Orbital imaging and spectroscopy clearly reveal distinct layers of hydrated minerals, sulfates, and clays with abundant evidence of a variety of fluvial processes. The three instruments of the MSL Sample Analysis at aMars (SAM) investigation, the Quadrupole Mass Spectrometer (QMS), the Tunable Laser Spectrometer (TLS), and the Gas Chromatograph (GC) are designed to analyze either atmospheric gases or volatiles thermally evolved or chemically extracted from powdered rock or soil. The presence or absence of organic compounds in these layers is of great interest since such an in situ search for this type of record has not been successfully implemented since the mid-60s Viking GCMS experiments. However, regardless of the outcome of the analysis for organics, the abundance and isotopic composition of thermally evolved inorganic compounds should also provide a rich data set to complement the mineralogical and elemental information provided by other MSL instruments. In addition, these evolved gas analysis (EGA) experiments will help test sedimentary models proposed by Malin and Edgett (2000) and then further developed by Milliken et al (2010) for Gale Crater. In the SAM EGA experiments the evolution temperatures of H2O, CO2, SO2, O2, or other simple compounds as the samples are heated in a helium stream to 1000 C provides information on mineral types and their associations. The isotopic composition of O, H, C, and S can be precisely determined in several evolved compounds and compared with the present day atmosphere. Such SAM results might be able to test mineralogical evidence of changing sedimentary and alteration processes over an extended period of time. For example, Bibring et al (2006) have suggested such a major shift from early nonacidic to later acidic alteration. We will illustrate through a variety of evolved gas experiments implemented under SAM-like gas flow and temperature ramp conditions on terrestrial analog minerals on high fidelity Sam breadboards the type of chemical information we expect SAM to provide.

Mahaffy, Paul↗