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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS2010

Carbon Isotope Characterization of Organic Intermediaries in Hydrothermal Hydrocarbon Synthesis by Pyrolysis-GC-MS-C-IRMS

We report results of experiments designed to characterize the carbon isotope composition of intermediate organic compounds produced as a result of mineral surface catalyzed reactions. The impetus for this work stems from recently reported detection of methane in the Martian atmosphere coupled with evidence showing extensive water-rock interaction during Martian history. Abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions may be one possible process responsible for methane generation on Mars, and measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible isotope measurements. Our isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-Combustion-Isotope Ratio Mass Specrometry (Py-GC-MS-C-IRMS). Others have conducted similar pyrolysis-IRMS experiments on low molecular weight organic acids (Dias, et al, Organic Geochemistry, 33 [2002]). Our technique differs in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of the organic compounds. A sample of carboxylic acid (mixture of C1 through C6) was pyrolyzed at 100 XC and passed through the GC-MS-C-IRMS (combusted at 940 XC). In order to test the reliability of our technique we compared the _13C composition of different molecular weight organic acids (from C1 through C6) extracted individually by the traditional sealed-tube cupric oxide combustion (940 XC) method with the _13C produced by our pyrolysis technique. Our data indicate that an average 4.3. +/-0.5. (V-PDB) apparent isotopic fractionation accompanies the pyrolysis extractions. We postulate that this isotope offset could be the result of incomplete thermal desorption during pyrolysis. We are continuing to investigate the reliability of this pyrolysis technique for correcting carbon isotope measurements of mineral surface catalyzed organic compounds.

Socki, Richard A.↗
NASA NTRS1985

The AMPTE IRM Science Data Center

The creation of artificial ion clouds is a major aspect of the AMPTE program. The IRM Science Data center supports real-time decision for a release with real-time scientific data processing and display including model calculations of ion trajectories. Additionally, survey plots and summary data records are generated in near real time thus allowing to start the data analysis as early as possible. For detailed analyses, interactive programs were developed so that physical parameters of all IRM experiments can be combined to produce common spectra or line plots.

Bauer, O. H.↗
NASA NTRS2013

Compound Specific Hydrogen Isotope Composition of Type II and III Kerogen Extracted by Pyrolysis-GC-MS-IRMS

The use of Hydrogen (H) isotopes in understanding oil and gas resource plays is in its infancy. Described here is a technique for H isotope analysis of organic compounds pyrolyzed from oil and gas shale-derived kerogen. Application of this technique will progress our understanding. This work complements that of Pernia et al. (2013, this meeting) by providing a novel method for the H isotope analysis of specific compounds in the characterization of kerogen extracted by analytically diverse techniques. Hydrogen isotope analyses were carried out entirely "on-line" utilizing a CDS 5000 Pyroprobe connected to a Thermo Trace GC Ultra interfaced with a Thermo MAT 253 IRMS. Also, a split of GC-separated products was sent to a DSQ II quadrupole MS to make semi-quantitative compositional measurements of the extracted compounds. Kerogen samples from five different basins (type II and III) were dehydrated (heated to 80 C overnight in vacuum) and analyzed for their H isotope compositions by Pyrolysis-GC-MS-TC-IRMS. This technique takes pyrolysis products separated via GC and reacts them in a high temperature conversion furnace (1450 C) which quantitatively forms H2, following a modified method of Burgoyne and Hayes, (1998, Anal. Chem., 70, 5136-5141). Samples ranging from approximately 0.5 to 1.0mg in size, were pyrolyzed at 800 C for 30s. Compounds were separated on a Poraplot Q GC column. Hydrogen isotope data from all kerogen samples typically show enrichment in D from low to high molecular weight compounds. Water (H2O) average deltaD = -215.2 (V-SMOW), ranging from -271.8 for the Marcellus Shale to -51.9 for the Polish Shale. Higher molecular weight compounds like toluene (C7H8) have an average deltaD of -89.7 0/00, ranging from -156.0 for the Barnett Shale to -50.0 for the Monterey Shale. We interpret these data as representative of potential H isotope exchange between hydrocarbons and sediment pore water during formation within each basin. Since hydrocarbon H isotopes readily exchange with water, these data may provide some useful information on gas-water or oil-water interaction in resource plays, and further as a possible indicator of paleo-environmental conditions. Alternatively, our data may be an indication of H isotope exchange with water and/or acid during the kerogen isolation process. Either of these interpretations will prove useful when deciphering H isotope data derived from kerogen analysis. More experiments are planned to discern these two or other possible scenarios.

Socki, Richard A.↗
NASA NTRS2014

Hydrogen (H) Isotope Composition of Type II Kerogen Extracted by Pyrolysis-GC-MS-IRMS: Terrestrial Shale Deposits as Martian Analogs

Described here is a technique for H isotope analysis of organic compounds pyrolyzed from kerogens isolated from gas‐ and liquids‐rich shales. Application of this technique will progress the understanding of the use of H isotopes not only in potential kerogen occurrences on Mars, but also in terrestrial oil and gas resource plays. H isotope extraction and analyses were carried out utilizing a CDS 5000 Pyroprobe connected to a Thermo Trace GC interfaced with a Thermo MAT 253 IRMS. Also, a split of GC‐separated products was sent to a DSQ II quadrupole MS to make qualitative and semi‐quantitative compositional measurements of these products. Kerogen samples from five different basins (type II and II‐S) were dehydrated (heated to 80 C overnight under vacuum) and analyzed for their H isotope compositions by Pyrolysis‐GC‐MS‐TC‐IRMS. This technique takes pyrolysis products separated via GC and reacts them in a high temperature conversion furnace (1450 C), which quantitatively forms H2. Samples ranging from ~0.5 to 1.0mg in size, were pyrolyzed at 800 C for 30s. and separated on a Poraplot Q GC column. H isotope data from all kerogen samples typically show enrichment in D from low to high molecular weight. H2O average delta D = ‐215.2 per mille (V‐SMOW), ranging from ‐ 271.8 per mille for the Marcellus Shale to ‐51.9 per mille for a Polish shale. Higher molecular weight compounds like toluene (C7H8) have an average delta D of ‐89.7 per mille, ranging from ‐156.0 per mille for the Barnett Shale to ‐50.0 per mille for the Monterey Shale. We interpret these data as representative of potential H isotope exchange between hydrocarbons and sediment pore water during basin formation. Since hydrocarbon H isotopes readily exchange with water, these data may provide some useful information on gas‐water or oil‐water interaction in resource plays, and further as a possible indicator of paleoenvironmental conditions. Alternatively, our data may be an indication of H isotope exchange with water and/or acid during the kerogen isolation process. Either of these interpretations will prove useful when deciphering H isotope data derived from kerogen analyses. Understanding the role that these H‐bearing compounds play in terrestrial shale paleo‐environmental reconstruction may also prove useful as analogs for understanding the interactions of water and potential kerogen/organic compounds on the planet Mars.

Socki, Richard A.↗
NASA NTRS1983

Nutation damper for the AMPTE-IRM satellite: Final Report

The design, computations, and testing of the nutation damper for the AMPTE-IRM satellite are described. The nutation motions of the satellite excite fluid oscillations in the closed tube system; kinetic energy is destroyed (converted to heat) through tube/fluid friction, constriction of the stream by cross sectional change, and formation of turbulence by stream enlargement. This energy is extracted from the satellite such that nutation is reduced. Tests were carried out in a pendulum testing device and the time constants were calculated. Findings showed that the damper remained within the originally specified values and provided for good dynamic behavior of the satellite.

Truckenbrodt, A.↗
NASA NTRS1985

The IRM fluxgate magnetometer

This report describes the three-axis fluxgate magnetometer instrument on board the AMPTE IRM spacecraft. Important features of the instrument are its wide dynamic range (0.1-60,000 nT), a high resolution (16-bit analog to digital conversion) and the capability to operate automatically or via telecommand in two gain states. In addition, the wave activity is monitored in all three components up to 50 Hz. Inflight checkout proved the nominal functioning of the instrument in all modes.

Luehr, H.↗
NASA NTRS1987

Electron cyclotron harmonic waves observed by the AMPTE-IRM plasma wave experiment following a lithium release in the solar wind

An unexpected occurrence following the second lithium release by the AMPTE-IRM spacecraft in the solar wind on September 20, 1984, was the appearance of electron cyclotron harmonic emissions. These emissions began about 50 s after the release and continued for several minutes. Narrow-band emissions polarized perpendicular to the magnetic field with amplitudes of approximately 0.00001 V/m were observed in each of the first five harmonic bands. The diffuse emissions extended from below the lowest measured frequency channel to above the highest narrow-band emission with a maximum below the electron cyclotron frequency. It will be shown that these observations are inconsistent with their generation by several ion beam instabilities.

Roeder, J. L.↗
NASA NTRS1987

AMPTE IRM observations of waves associated with flux transfer events in the magnetosphere

The AMPTE IRM wave instrument has been applied to the study of flux transfer events (FTE's). This initial investigation concentrates on FTE's observed in the magnetosphere during the fall of 1984. The wave morphology consists of four significant features: at frequencies below the ion gyrofrequency, magnetic fluctuations occur with amplitudes of the order of 1 nT; at frequencies from a few hertz to a few hundred hertz, electric field fluctuations are observed which have a broadband amplitude of a few millivolts per meter, which are perpendicularly polarized at the lowest frequencies, and which are partly electrostatic and partly electromagnetic; in the frequency range from 100 Hz to 10 kHz, broadband spikelike waves occur with a time-averaged amplitude of about 0.1 mV/m; and near the electron plasma frequency, bursts of waves occur at the boundaries of FTE's. In none of the 25 events surveyed does the total broadband amplitude of all the waves exceed a few millivolts per meter, an amplitude far too small to provide the dissipation required by 'traditional' reconnection models in which the dissipation region has a thickness the order of an ion gyroradius. Thus, either all of the FTE's are observed at some distance from the diffusion region, or the observable waves play no significant role in the diffusion process, or 'traditional' reconnection models do not apply to reconnection in FTE's.

Labelle, J.↗
NASA NTRS1987

Observation of nonlinear wave decay processes in the solar wind by the AMPTE IRM plasma wave experiment

Nonlinear wave decay processes have been detected in the solar wind by the plasma wave experiment aboard the Active Magnetospheric Particle Tracer Explorers (AMPTE) IRM spacecraft. The main process is the generation of ultralow-frequency ion acoustic waves from the decay of Langmuir waves near the electron plasma frequency. Frequently, this is accompanied by an enhancement of emissions near twice the plasma frequency. This enhancement is most likely due to the generation of electromagnetic waves from the coalescence of two Langmuir waves. These processes occur within the electron foreshock in front of the earth's bow shock.

Koons, H. C.↗
NASA NTRS1988

On the transport of ions released in the magnetotail by the AMPTE-IRM satellite

The Ba and Li ions releasd into the magnetotail in spring 1985 by the AMPTE-IRM satellite were not observed subsequently in the inner magnetosphere with the AMPTE-CCE satellite. These results were studied by using a Monte Carlo code to compute the transport of the ions. For each release several hundred ion guiding-center trajectories were computed under simulated magnetospheric conditions, using the Tsyganenko-Usmanov (1982) magnetic-field model and the Millstone Hill convection-electric-field model (Oliver et al., 1983). The corotation and convection electric fields were mapped to altitudes above the ionosphere, assuming the magnetic-field lines to be equipotentials. The initial conditions of the ions, at the times at which the ions were picked up by the electric field, were estimated by taking into consideration the release conditions and the early-time collective effects. The results indicate that the Ba(+) ions were not observed because the CCE satellite was not along the drift paths of the ions, and the Li(+) ions were not observed because their fluxes at the satellite were too low.

Cladis, J. B.↗
NASA NTRS1989

Isotope Ratio Monitoring Gas Chromatography Mass Spectrometry (IRM-GCMS)

On Earth, the C-13 content of organic compounds is depleted by roughly 13 to 23 permil from atmospheric carbon dioxide. This difference is largely due to isotope effects associated with the fixation of inorganic carbon by photosynthetic organisms. If life once existed on Mars, then it is reasonable to expect to observe a similar fractionation. Although the strongly oxidizing conditions on the surface of Mars make preservation of ancient organic material unlikely, carbon-isotope evidence for the existence of life on Mars may still be preserved. Carbon depleted in C-13 could be preserved either in organic compounds within buried sediments, or in carbonate minerals produced by the oxidation of organic material. A technique is introduced for rapid and precise measurement of the C-13 contents of individual organic compounds. A gas chromatograph is coupled to an isotope-ratio mass spectrometer through a combustion interface, enabling on-line isotopic analysis of isolated compounds. The isotope ratios are determined by integration of ion currents over the course of each chromatographic peak. Software incorporates automatic peak determination, corrections for background, and deconvolution of overlapped peaks. Overall performance of the instrument was evaluated by the analysis of a mixture of high purity n-alkanes of know isotopic composition. Isotopic values measured via IRM-GCMS averaged withing 0.55 permil of their conventionally measured values.

Freeman, K. H.↗
NASA NTRS1991

Propagation of perturbation energy fluxes in the subsolar magnetosheath - AMPTE IRM observations

The propagation properties of perturbation energy fluxes of subsolar magnetosheath fluctuations were studied. The Poynting flux, kinetic energy flux, and enthalpy flux are calculated using magnetic field and plasma measurements from the AMPTE IRM satellite during five intervals in 1984. The results are then compared with a disturbance indicator R of the magnetic field in the same magnetosheath region. It is shown that during disturbed periods with large transverse variations (low R level), the perturbation Poynting flux and the kinetic energy flux increase, and a significant portion of the fluxes consistently propagates toward the magnetopause. The Poynting flux of those fluctuations which consist of mainly compressional perturbations does not appear to propagate in any certain direction. The enthalpy flux of the perturbations does not propagate in any certain direction in any of the cases. The kinetic energy flux appears to be more important in exciting harmonic ULF waves in the dayside magnetosphere.

Lin, N.↗
NASA NTRS2011

Hydrogen Isotope Measurements of Organic Acids and Alcohols by Pyrolysis-GC-MS-TC-IRMS

One possible process responsible for methane generation on Mars is abiotic formation by Fischer-Tropsch-type (FTT) synthesis during serpentinization reactions. Measurement of carbon and hydrogen isotopes of intermediary organic compounds can help constrain the origin of this methane by tracing the geochemical pathway during formation. Of particular interest within the context of this work is the isotopic composition of organic intermediaries produced on the surfaces of mineral catalysts (i.e. magnetite) during hydrothermal experiments, and the ability to make meaningful and reproducible hydrogen isotope measurements. Reported here are results of experiments to characterize the hydrogen isotope composition of low molecular weight organic acids and alcohols. The presence of these organic compounds has been suggested by others as intermeadiary products made during mineral surface catalyzed reactions. This work compliments our previous study characterizing the carbon isotope composition of similar low molecular weight intermediary organic compounds (Socki, et al, American Geophysical Union Fall meeting, Abstr. #V51B-2189, Dec., 2010). Our hydrogen isotope measurements utilize a unique analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-High Temperature Conversion-Isotope Ratio Mass Spectrometry (Py-GC-MS-TC-IRMS). Our technique is unique in that it carries a split of the pyrolyzed GC-separated product to a Thermo DSQ-II? quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of separated organic compounds, therefore both chemical and isotopic measurements can be carried out simultaneously on the same sample.

Socki, Richard A.↗
NASA NTRS2012

Hydrogen Isotope Measurements of Organic Acids and Alcohols by Pyrolysis-GC-MS-TC-IRMS: Application to Analysis of Experimentally Derived Hydrothermal Mineral-Catalyzed Organic Products

We report results of experiments to measure the H isotope composition of organic acids and alcohols. These experiments make use of a pyroprobe interfaced with a GC and high temperature extraction furnace to make quantitative H isotope measurements. This work compliments our previous work that focused on the extraction and analysis of C isotopes from the same compounds [1]. Together with our carbon isotope analyses our experiments serve as a "proof of concept" for making C and H isotope measurements on more complex mixtures of organic compounds on mineral surfaces in abiotic hydrocarbon formation processes at elevated temperatures and pressures. Our motivation for undertaking this work stems from observations of methane detected within the Martian atmosphere [2-5], coupled with evidence showing extensive water-rock interaction during Mars history [6-8]. Methane production on Mars could be the result of synthesis by mineral surface-catalyzed reduction of CO2 and/or CO by Fischer-Tropsch Type (FTT) reactions during serpentization [9,10]. Others have conducted experimental studies to show that FTT reactions are plausible mechanisms for low-molecular weight hydrocarbon formation in hydrothermal systems at mid-ocean ridges [11-13]. Our H isotope measurements utilize an analytical technique combining Pyrolysis-Gas Chromatograph-Mass Spectrometry-High Temperature Conversion-Isotope Ratio Mass Spectrometry (Py-GC-MS-TC-IRMS). This technique is designed to carry a split of the pyrolyzed GC-separated product to a Thermo DSQII quadrupole mass spectrometer as a means of making qualitative and semi-quantitative compositional measurements of separated organic compounds, therefore both chemical and isotopic measurements can be carried out simultaneously on the same sample.

Socki, Richard A.↗
NASA NTRS1986

Plasma waves observed by the IRM and UKS spacecraft during the AMPTE solar wind lithium releases - Overview

The wave measurements from the Ion Release Module and the United Kingdom Satellite in the diamagnetic cavity, the transition region, and the upstream region are examined. Solar wind conditions during the releases on September 11 and 20, 1984 are described. The quasi-static electric field, wideband, high-frequency waves, and medium and VLF waves observations are analyzed. The data reveal that extremely low levels of wave activity are observed in the boundary between the diamagnetic cavity and external magnetic field, medium and VLF waves in the ion acoustic electrostatic cyclotron harmonic modes are detected in the transition region from the diamagnetic cavity to the solar wind, and decay in the magnetic field strength and density, and an increase in the quasi-static electric field is seen in the upstream edge of the transition region. The emissions observed are related to the different phases of the Li cloud development and different spatial regimes of the Li plasma-solar wind interaction.

Haeusler, B.↗
NASA NTRS1986

Lunar paleointensities via the IRMs normalization method and the early magnetic history of the moon

A method for determining a planetary body's magnetic field environment over time is proposed. This relative paleointensity method is based on the normalization of natural remanence to saturation remanence magnetization as measured after each sample is exposed to a strong magnetic field. It is shown that this method is well suited to delineating order-of-magnitude changes in magnetizing fields.

Cisowski, S. M.↗
NASA NTRS2012

Carbon and Hydrogen Isotope Measurements of Alcohols and Organic Acids by Online Pyroprobe-GC-IRMS

The detection of methane in the atmosphere of Mars, combined with evidence showing widespread water-rock interaction during martian history, suggests that the production of methane on Mars may be the result of mineral surface-catalyzed CO2 and or CO reduction during Fisher-Tropsch Type (FTT) reactions. A better understanding of these reaction pathways and corresponding C and H isotope fractionations is critical to deciphering the synthesis of organic compounds produced under abiotic hydrothermal conditions. Described here is a technique for the extraction and analysis of both C and H isotopes from alcohols (C1-C4) and organic acids (C1-C6). This work is meant to provide a "proof of concept" for making meaningful isotope measurements on complex mixtures of solid-phase hydrocarbons and other intermediary products produced during high-temperature and high-pressure synthesis on mineral-catalyzed surfaces. These analyses are conducted entirely "on-line" utilizing a CDS model 5000 Pyroprobe connected to a Thermo Trace GC Ultra that is interfaced with a Thermo MAT 253 isotope ratio mass spectrometer operating in continuous flow mode. Also, this technique is designed to carry a split of the GC-separated product to a DSQ II quadrupole mass spectrometer as a means of making semi-quantitative compositional measurements. Therefore, both chemical and isotopic measurements can be carried out on the same sample.

Socki, Richard A.↗
NASA NTRS2010

Stable Chlorine Isotope Study: Application to Early Solar System Materials

A significantly large mass fractionation between two stable chlorine isotopes is expected during planetary processes In addition, in view of the isotopic heterogeneity of other light elements, the chlorine isotopes can potentially be used as a tracer for the origins and evolutionary processes of early solar system materials. Due to analytical difficulties, however, current chlorine isotope studies on planetary materials are quite controversial among IRMS (gas source mass spectrometry) and/or TIMS (Thermal Ionization Mass Spectrometry) groups [i.e. 1-3]. Although a cross-calibration of IRMS and TIMS indicates that both techniques are sufficiently consistent with each other [4], some authors have claimed that the Cl-37/Cl-35 ratio of geological samples obtained by TIMS technique are, in general, misleadingly too high and variable compared to those of IRMS [3]. For example, almost no differences of Cl isotope composition were observed among mantle materials and carbonaceous meteorites by [3]. On the other hand, according to more recent IRMS work [2], significant Cl isotope variations are confirmed for mantle materials. Therefore, additional careful investigation of Cl isotope analyses are now required to confirm real chlorine isotope variations for planetary materials including carbonaceous chondrites [5]. A significantly large mass fractionation between two stable chlorine isotopes is expected during planetary processes In addition, in view of the isotopic heterogeneity of other light elements, the chlorine isotopes can potentially be used as a tracer for the origins and evolutionary processes of early solar system materials. Due to analytical difficulties, however, current chlorine isotope studies on planetary materials are quite controversial among IRMS (gas source mass spectrometry) and/or TIMS (Thermal Ionization Mass Spectrometry) groups [i.e. 1-3]. Although a cross-calibration of IRMS and TIMS indicates that both techniques are sufficiently consistent with each other [4], some authors have claimed that the 37Cl/35Cl ratio of geological samples obtained by TIMS technique are, in general, misleadingly too high and variable compared to those of IRMS [3]. For eample, almost no differences of Cl isotope composition were observed among mantle materials and carbonaceous meteorites by [3]. On the other hand, according to more recent IRMS work [2], significant Cl isotope variations are confirmed for mantle materials. Therefore, additional careful investigation of Cl isotope analyses are now required to confirm real chlorine isotope variations for planetary materials including carbonaceous chondrites [5]. In order to clarify the stable chlorine isotope features of early solar system materials, we have initiated development of the TIMS technique at NASA JSC applicable to analysis of small amounts of meteoritic and planetary materials. We report here the current status of chlorine isotope analysis at NASA JSC.

Mala,ira. M/↗