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NASA NTRS1992

Oxidation of the N-terminal methionine of lens alpha-A crystallin

Antiserum against the N-terminal peptide of bovine alpha-A crystallin has been used to monitor purification of two different seropositive peptides (i.e. T1a and T1b) from a tryptic digest of bovine lens proteins. Both these peptides have similar amino acid compositions, but peptide T1b has a molecular weight 16 atomic mass units larger than T1a, suggesting posttranslational modification. Analysis of ionization fragments of the T1b peptide by mass spectrometry demonstrates that this difference in molecular weight is due to the in vivo oxidation of the N-terminal met residue of the alpha-A crystallin molecule.

NASA Discipline Cell Biology↗

NASA NTRS2013

Water in Nominally Anhydrous Minerals from Nakhlites and Shergottites

Estimating the amount of water in the interior of terrestrial planets has tremendous implications on our understanding of solar nebula evolution, planet formation and geological history, and extraterrestrial volcanism. Mars has been a recent focus of such enquiry with complementary datasets from spacecrafts, rovers and martian meteorite studies. In planetary interiors, water can be dissolved in fluids or melts and hydrous phases, but can also be locked as protons attached to structural oxygen in lattice defects in nominally anhydrous minerals (NAM) such as olivine, pyroxene, or feldspar [1-3]. Measuring water in Martian meteorite NAM is challenging because the minerals are fragile and riddled with fractures from impact processes that makes them break apart during sample processing. Moreover, curing the sample in epoxy causes problems for the two main water analysis techniques, Fourier transform infrared spectrometry (FTIR) and secondary ionization mass spectrometry (SIMS). Measurements to date have resulted in a heated debate on how much water the mantle of Mars contains. SIMS studies of NAM [4], amphiboles [5], and apatites [6-8] from Martian meteorites report finding enough water in these phases to infer that the martian mantle is as hydrous as that of the Earth. On the other hand, a SIMS study of glass in olivine melt inclusions from shergottites concludes that the Martian mantle is much drier [9]. The latter interpretation is also supported by the fact that most martian hydrous minerals generally have the relevant sites filled with Cl and F instead of H [10,11]. As for experimental results, martian basalt compositions can be reproduced using water as well as Cl in the parent melts [12,13]. Here FTIR is used to measure water in martian meteorite minerals in order to constrain the origin of the distribution of water in martian meteorite phases.

Peslier, Anne H.↗

NASA NTRSDate not supplied

Surface Exposure History of Asteroid Bennu Based on Cosmogenic Radionuclides in OSIRIS-Rex Samples

The surface of asteroid Bennu changes over time because of impacts, mass movement, and particle ejections [1-4]. The OSIRIS-REx samples were collected from a 20-m-diameter crater on Bennu called Hokioi. One of the driving hypotheses of the mission is that Hokioi is part of a population of small (<25 m) craters that are less than 0.1 Myr old and contain relatively unweathered material [1,4]. Our goal is to understand the recent surface exposure history of Bennu, utilizing radionuclides (10Be, 26Al, 36Cl, 41Ca) produced by both galactic and solar cosmic rays. We received ~12 mg of aggregate sample OREX-803014-0. We picked five of the larger particles with masses ranging from 0.24 to 0.68 mg. We dissolved each particle, along with 0.15 mg Be and 1.0 mg Cl carrier, in HF/HNO3 mixture, and did the same for the remaining aggregate sample of 9.8 mg. After dissolution, we took a small aliquot for chemical analysis, added 0.7 mg of Al carrier, and separated Be, Al, and Cl for analysis of cosmogenic 10Be, 26Al, and 36Cl by accelerator mass spectrometry [5]. Preliminary 26Al results show concentrations of 21–27 dpm/kg for the Bennu samples, with an average of 22.5 ± 0.6 dpm/kg for the five particles and 21.1 ± 0.7 dpm/kg for the remaining aggregate. These values are close to the expected 26Al saturation values of 25–30 dpm/kg for the top 1 m of Bennu’s regolith, suggesting a minimum exposure age of 1.5–2.0 Myr near the surface. Our initial Bennu results also resemble those found for Ryugu samples [6,7]; thus, we can hypothesize that the two asteroids have had similar surface exposure histories.

K C Welten↗

NASA NTRS2017

Molecular Analyzer for Complex Refractory Organic-Rich Surfaces (MACROS)

The Molecular Analyzer for Complex Refractory Organic-rich Surfaces, MACROS, is a novel instrument package being developed at NASA Goddard Space Flight Center. MACROS enables the in situ characterization of a sample's composition by coupling two powerful techniques into one compact instrument package: (1) laser desorption/ionization time-of-flight mass spectrometry (LDMS) for broad detection of inorganic mineral composition and non-volatile organics, and (2) liquid-phase extraction methods to gently isolate the soluble organic and inorganic fraction of a planetary powder for enrichment and detailed analysis by liquid chromatographic separation coupled to LDMS. The LDMS is capable of positive and negative ion detection, precision mass selection, and fragment analysis. Two modes are included for LDMS: single laser LDMS as the broad survey mode and two step laser mass spectrometry (L2MS). The liquid-phase extraction will be done in a newly designed extraction module (EM) prototype, providing selectivity in the analysis of a complex sample. For the sample collection, a diamond drill front end will be used to collect rock/icy powder. With all these components and capabilities together, MACROS offers a versatile analytical instrument for a mission targeting an icy moon, carbonaceous asteroid, or comet, to fully characterize the surface composition and advance our understanding of the chemical inventory present on that body.

Getty, Stephanie A.↗

NASA NTRS2005

Mass Spectrometry for Planetary Probes: Past, Present and Future

Atmospheric entry probes present a unique opportunity for performing quantitative analysis of extra-terrestrial atmospheres in cases where remote sensing alone may not be sufficient and measurements with balloons or aircraft is not practical. An entry probe can provide a complete vertical profile of atmospheric parameters including chemical composition, which cannot be obtained with most other techniques. There are, however, unique challenges associated with building instruments for an entry probe, as compared to orbiters, landers, or rovers. Conditions during atmospheric entry are extreme, there are inherent time constraints due to the short duration of the experiment, and the instrument experiences rapid environmental changes in temperature and pressure as it descends. In addition, there are resource limitations, i.e. mass, power, size and bandwidth. Finally, the demands on the instrument design are determined in large part by conditions (pressure, temperature, composition) unique to the particular body under study, and as a result there is no one-size-fits-all instrument for an atmospheric probe. Many of these requirements can be more easily met by miniaturizing the probe instrument. Our experience building mass spectrometers for atmospheric entry probes leads us to believe that the time is right for a fundamental change in the way spaceflight mass spectrometers are built. The emergence over the past twenty years of Micro-electro- mechanical Systems (MEMS), utilizing lithographic semiconductor fabrication techniques to produce instrument systems in miniature, holds great promise for application to spaceflight mass spectrometry. A highly miniaturized, high performance and low-power mass spectrometer would be an enormous benefit to future entry probe missions, allowing, for example, parallel measurements (e.g., multiple simultaneous gas chromatographic analyses and direct atmospheric leaks.) Such an instrument would also enable mass spectrometry on board small multiple entry probes. In the development of a MEMS Mass Spectrometer, the challenge facing us is to move beyond the proof-of-concept, where research dollars tend to focus, and carry out the detailed work of developing a high performance mass spectrometer system on a chip which meets the unique technical requirements for an atmospheric entry probe described above.

Niemann, Hasso B.↗

NASA NTRS2017

Method for the Collection, Gravimetric and Chemical Analysis of Nonvolatile Residue (NVR) on Surfaces

Nonvolatile residue (NVR), sometimes referred to as molecular contamination is the term used for the total composition of the inorganic and high boiling point organic components in particulates and molecular films deposited on critical surfaces surrounding space structures, with the particulate and NVR contamination originating primarily from pre-launch operations. The "nonvolatile" suggestion from the terminology NVR implies that the collected residue will not experience much loss under ambient conditions. NVR has been shown to have a dramatic impact on the ability to perform optical measurements from platforms based in space. Such contaminants can be detected early by the controlled application of various detection techniques and contamination analyses. Contamination analyses are the techniques used to determine if materials, components, and subsystems can be expected to meet the performance requirements of a system. Of particular concern is the quantity of NVR contaminants that might be deposited on critical payload surfaces from these sources. Subsequent chemical analysis of the contaminant samples by infrared spectroscopy and gas chromatography mass spectrometry identifies the components, gives semi-quantitative estimates of contaminant thickness, indicates possible sources of the NVR, and provides guidance for effective cleanup procedures. In this report, a method for the collection and determination of the mass of NVR was generated by the authors at NASA Langley Research Center. This report describes the method developed and implemented for collecting NVR contaminants, and procedures for gravimetric and chemical analysis of the residue obtained. The result of this NVR analysis collaboration will help pave the way for Langley's ability to certify flight hardware outgassing requirements in support of flight projects such as Stratospheric Aerosol and Gas Experiment III (SAGE III), Clouds and the Earth's Radiant Energy System (CERES), Materials International Space Station Experiment - X (MISSE-X), and Doppler Aerosol Wind Lidar (DAWN).

Gordon, Keith↗

NASA NTRS1986

Radionuclide measurements by accelerator mass spectrometry at Arizona

Over the past years, Tandem Accelerator Mass Spectrometry (TAMS) has become established as an important method for radionuclide analysis. In the Arizona system the accelerator is operated at a thermal voltage of 1.8MV for C-14 analysis, and 1.6 to 2MV for Be-10. Samples are inserted into a cesium sputter ion source in solid form. Negative ions sputtered from the target are accelerated to about 25kV, and the injection magnet selects ions of a particular mass. Ions of the 3+ charge state, having an energy of about 9MeV are selected by an electrostatic deflector, surviving ions pass through two magnets, where only ions of the desired mass-energy product are selected. The final detector is a combination ionization chamber to measure energy loss (and hence, Z), and a silicon surface-barrier detector which measures residual energy. After counting the trace iosotope for a fixed time, the injected ions are switched to the major isotope used for normalization. These ions are deflected into a Faraday cup after the first high-energy magnet. Repeated measurements of the isotope ratio of both sample and standards results in a measurement of the concentration of the radionuclide. Recent improvements in sample preparation for C-14 make preparation of high-beam current graphite targets directly from CO2 feasible. Except for some measurements of standards and backgrounds for Be-10 measurements to date have been on C-14. Although most results have been in archaeology and quaternary geology, studies have been expanded to include cosmogenic C-14 in meteorites. The data obtained so far tend to confirm the antiquity of Antarctic meteorites from the Allan Hills site. Data on three samples of Yamato meteorites gave terrestrial ages of between about 3 and 22 thousand years.

Jull, A. J. T.↗

NASA NTRS1979

Lipids of aquatic sediments, recent and ancient

Computerized gas chromatography-mass spectrometry (GC-MS) is now an essential tool in the analysis of the complex mixtures of lipids (geolipids) encountered in aquatic sediments, both 'recent' (less than 1 million years old) and ancient. The application of MS, and particularly GC-MS, has been instrumental in the rapid development of organic geochemistry and environmental organic chemistry in recent years. The techniques used have resulted in the identification of numerous compounds of a variety of types in sediments. Most attention has been concentrated on molecules of limited size, mainly below 500 molecular mass, and of limited functionality, for examples, hydrocarbons, fatty acids and alcohols. Examples from recent studies (at Bristol) of contemporary, 'recent' and ancient sediments are presented and discussed.

Eglinton, G.↗

NASA NTRS1981

Comparison of Michigan Basin crude oils

Michigan Basin oils from the Ordovician Trenton, Silurian Niagaran, and Devonian Dundee formations have been geochemically compared by GC, GC-MS, and carbon isotope mass spectrometry. One oil from each formation was selected for detailed analysis which included measurement of individual n-alkane delta 13 C values. The Ordovician and Devonian oils are strikingly similar to one another, yet clearly different from the Silurian oil. This pattern is unexpected because Ordovician and Devonian reservoirs are physically separated by the Silurian strata. From time-temperature considerations, the Devonian oil probably was formed in older strata and has migrated to its present location. Our analyses suggest a common source for the Devonian and Ordovician oils.

Vogler, E. A.↗

NASA NTRS1985

Characterization methodology for PMR-15

Characterization of model compounds, monomers, resin solutions and cure cycles of PMR-15 polyimide are performed. Successful separation of various reaction products is also accomplished by liquid chromatography. The PMR-15 cure analysis is performed by fourier transform spectroscopy and gas chromatograph - mass spectrometry. Characterization receiving inspection tests for Quality Control are recommended.

Hunter, A. B.↗

NASA NTRS1994

Computer-Controlled, Motorized Positioning System

Computer-controlled, motorized positioning system developed for use in robotic manipulation of samples in custom-built secondary-ion mass spectrometry (SIMS) system. Positions sample repeatably and accurately, even during analysis in three linear orthogonal coordinates and one angular coordinate under manual local control, or microprocessor-based local control or remote control by computer via general-purpose interface bus (GPIB).

Vargas-Aburto, Carlos↗

NASA NTRS2003

Experimental Determination of Spinel/Melt, Olivine/Melt, and Pyroxene/Melt Partition Coefficients for Re, Ru, Pd, Au, and Pt

Experimental studies have identified spinels as important hosts phases for many of the highly siderophile elements (HSE). Yet experimental studies involving chromite or Cr-rich spinel have been lacking. Experimental studies of partitioning of HSEs between silicate, oxides and silicate melt are plagued by low solubilities and the presence of small metallic nuggets at oxygen fugacities relevant to magmas, which interfere with analysis of the phases of interest. We have circumvented these problems in two ways: 1) performing experiments at oxidized conditions, which are still relevant to natural systems but in which nuggets are not observed, and 2) analysis of run products with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS), allowing a combination of high sensitivity and good spatial resolution.

Righter, K.↗

NASA NTRS2015

Thermochemistry of Silicates

The thermodynamic properties of vapor and condensed phases of silicates are crucial in many fields of science. These quantities address fundamental questions on the formation, stability, transformation, and physical properties of silicate minerals and silicate coating compositions. Here the thermodynamic activities of silica and other species in solid solution have been measured by the analysis of the corresponding high temperature vapors using Knudsen Effusion Mass Spectrometry (KEMS). In first set of experiments KEMS has been used to examine the volatility sequence of species (Fe, SiO, Mg, O2 and O) present in the vapor phase during heating of fosterite-rich olivine (Fo93Fa7) up to 2400 C and to measure the Fe, SiO and Mg activities in its solid solution. The data of fosterite-rich olivine are essential for thermochemical equilibrium models to predict the atmospheric and surface composition of hot, rocky exoplanets (Lava Planets). In the second set of experiments the measured thermodynamic activities of the silica in Y2O3-SiO2 and Yb2O3-SiO2 systems are used to assess their reactivity and degradation recession as environmental barrier coatings (EBCs) in combustion environments (e.g. non-moveable parts of gas turbine engine).

Silicates↗

NASA NTRS2016

Conversion and Extraction of Insoluble Organic Materials in Meteorites

We endeavor to develop and implement methods in our laboratory to convert and extract insoluble organic materials (IOM) from low car-bon bearing meteorites (such as ordinary chondrites) and Precambrian terrestrial rocks for the purpose of determining IOM structure and prebiotic chemistries preserved in these types of samples. The general scheme of converting and extracting IOM in samples is summarized in Figure 1. First, powdered samples are solvent extracted in a micro-Soxhlet apparatus multiple times using solvents ranging from non-polar to polar (hexane - non-polar, dichloromethane - non-polar to polar, methanol - polar protic, and acetonitrile - polar aprotic). Second, solid residue from solvent extractions is processed using strong acids, hydrochloric and hydrofluoric, to dissolve minerals and isolate IOM. Third, the isolated IOM is subjected to both thermal (pyrolysis) and chemical (oxidation) degradation to release compounds from the macromolecular material. Finally, products from oxidation and pyrolysis are analyzed by gas chromatography - mass spectrometry (GCMS). We are working toward an integrated method and analysis scheme that will allow us to determine prebiotic chemistries in ordinary chondrites and Precambrian terrestrial rocks. Powerful techniques that we are including are stepwise, flash, and gradual pyrolysis and ruthenium tetroxide oxidation. More details of the integrated scheme will be presented.

Locke, Darren R.↗

NASA NTRS2016

Advanced Laser Architecture for Two-Step Laser Tandem Mass Spectrometer

Future astrobiology missions will focus on planets with significant astrochemical or potential astrobiological features, such as small, primitive bodies and the icy moons of the outer planets that may host diverse organic compounds. These missions require advanced instrument techniques to fully and unambiguously characterize the composition of surface and dust materials. Laser desorptionionization mass spectrometry (LDMS) is an emerging instrument technology for in situ mass analysis of non-volatile sample composition. A recent Goddard LDMS advancement is the two-step laser tandem mass spectrometer (L2MS) instrument to address the need for future flight instrumentation to deconvolve complex organic signatures. The L2MS prototype uses a resonance enhanced multi-photon laser ionization mechanism to selectively detect aromatic species from a more complex sample. By neglecting the aliphatic and inorganic mineral signatures in the two-step mass spectrum, the L2MS approach can provide both mass assignments and clues to structural information for an in situ investigation of non-volatile sample composition. In this paper we will describe our development effort on a new laser architecture that is based on the previously flown Lunar Orbiter Laser Altimeter (LOLA) laser transmitter for the L2MS instrument. The laser provides two discrete midinfrared wavelengths (2.8 m and 3.4 m) using monolithic optical parametric oscillators and ultraviolet (UV) wavelength (266 nm) on a single laser bench with a straightforward development path toward flight readiness.

Laser↗

NASA NTRS2019

Microbial Monitoring of Astromaterials Curation Labs Reveals Inter-Lab Diversity

The Astromaterials Curation Division at NASA’s Johnson Space Center houses seven sample collections stored in separate clean rooms to avoid cross-contamination. Prior to receiving new sample collections from carbon rich asteroids, we instituted a monitoring program to characterize the microbial ecology of these labs and to understand how organisms could interact with and potentially contaminate current and future collections. Methods: Beginning in Oct. 2017 we sampled the Meteorite (ISO 7 equivalent) and Pristine Lunar (ISO 5 equivalent) labs on a monthly basis. Surface samples were collected using dry swabs. Air samples were collected using an impactor style air sampler. Cultivable organisms were identified and characterized. Aliquots of each sample were also preserved for DNA sequencing. For each sampling event recovery rate was calculated as the percentage of samples showing microbial growth1. Fungal colonies were selected for amino acid extraction and analysis via Ultra- Performance Liquid Chromatography with Fluorescence Detection and Mass Spectrometry.

Regberg, A. B.↗

NASA NTRS1987

Research relative to an advanced rod control system for quadrupole mass spectrometry applications

The design of a suitable amplifier output stage using available transistors and passive components is summarized. All of the analysis and calculation confirm that it is feasible to design the amplifier and quadrupole coupling circuit needed for the Advanced Rod Control System. The progress obtained so far concerning the three frequency tank circuits to be used in the oscillator for the mass spectrometer of the Cometary Rendezvous Asteroid Flyby (CRAF) project is presented. Results from this study look promising. However, it is not known what minimum impedance levels are required to make it possible for the oscillator to work properly. Therefore, it is necessary to construct a prototype circuit in the laboratory which can be measured and tested in an oscillator circuit. Continued attempts will be made to develop a useful inductor motor with better characteristics than the one being used at the moment. It is important that such a model be found if computer simulation is to reflect reality more closely.

Carignan, George R.↗

NASA NTRSDate not supplied

Squeezing Every Last 'Bit' of Information from Enceladus Mass Spectrometry

Potential opportunities to return to Enceladus in Discovery and Flagship class missions inspire development of next-generation instruments and creative approaches to sample collection, sample analysis, and data analysis and transmission strategies. Mass spectrometers (MS) are ideally suited to future Enceladus missions due to their analytical power in identifying a range of molecular and ionic compositions – including complex organics – and potentially astrobiologically-important features such as isotope ratios, chirality, and enantiomeric excess. However, long communication delays from Enceladus and limited bandwidth limits the data transmission from these higher-data-volume instruments, likely delaying mission-related response to new data. We explore the utility of data science and machine learning (ML) on isotope ratio (IR)MS data collected from laboratory analogs of Enceladus to: 1) process data quickly for rapid ground-based analyses, 2) understand if compositional and biosignature information could be extracted from IRMS data, and 3) evaluate whether onboard ML techniques could improve sample analysis, cadence, and transmission prioritization. Laboratory analogs analyzed isotopes of volatile CO2 that interacted with seawaters of varying composition, and include both abiotic and biotic (microbially-influenced) experiments. Enceladus’s alkaline oceans promote speciation of carbon into multiple forms (e.g., H2CO3 / CO2, HCO3-, and CO32-), each of which could be isotopically fractionated by abiotic or biotic reactions. Large (>2‰) changes in carbon isotopes (δ13C) are observed from some biotic experiments inoculated with complex microbial ecosystems relative to the abiotic seawaters. ML training and classification suggests that microbial samples can be distinguished from abiotic samples, yet that a broad range of microbial experiments are necessary to train ML models to cover a range of complexities including disequilibria, and isotopic and compositional fractionation.

geochemistry↗