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At least 199 records · Page 11

Isotope-ratio-monitoring gas chromatography-mass spectrometry: methods for isotopic calibration

In trial analyses of a series of n-alkanes, precise determinations of 13C contents were based on isotopic standards introduced by five different techniques and results were compared. Specifically, organic-compound standards were coinjected with the analytes and carried through chromatography and combustion with them; or CO2 was supplied from a conventional inlet and mixed with the analyte in the ion source, or CO2 was supplied from an auxiliary mixing volume and transmitted to the source without interruption of the analyte stream. Additionally, two techniques were investigated in which the analyte stream was diverted and CO2 standards were placed on a near-zero background. All methods provided accurate results. Where applicable, methods not involving interruption of the analyte stream provided the highest performance (sigma = 0.00006 at.% 13C or 0.06% for 250 pmol C as CO2 reaching the ion source), but great care was required. Techniques involving diversion of the analyte stream were immune to interference from coeluting sample components and still provided high precision (0.0001 < or = sigma < or = 0.0002 at.% or 0.1 < or = sigma < or = 0.2%).

NASA Discipline Exobiology↗

Possible selective adsorption of enantiomers by Na-montmorillonite

Racemic amino acids including (D,L) alpha-alamine, (D,L) alpha-aminobutyric acid, (D,L) valine, and (D,L) norvaline were incubated with Na-montmorillonite at 100% CEC at three hydrogen ion concentrations, and amino acid adsorption was determined by ion exchange chromatography. Enantiomers were analyzed by gas chromatography. Differences in the quantities of D and L enantiomers in any of the fractions was no larger than a few percent. Although a large difference in the adsorption of the amino acid enantiomers was not observed, the analysis may indicate a small preferential adsorption (0.5-2%) of L-amino acids by Na-montmorillonite.

Friebele, E.↗

A Helium GC/IMS for the Analysis of Extraterrestrial Volatiles in Exobiology Flight Experiments

For exobiology experiments on board spacecraft or space probes, a wide range of chemical species often must be detected and identified. The limited amount of power and space available for flight instruments severely limits the number of instruments that can be flown on any given mission. It is important then, that these experiments utilize instrumentation with universal response, so that all species of interest can be analyzed. Instrumentation to fulfill the analytical requirements of exobiology experiments has been developed utilizing Gas Chromatography - Ion Mobility Spectrometry. The Gas Chromatograph (GC) combines columns developed specifically for the complex mixtures anticipated with highly sensitive Metastable Ionization Detectors (a type of Helium Ionization Detector). To satisfy the limitations placed on resources, the Ion Mobility Spectrometer (IMS) uses the same ultra high purity helium as the GC. This GC-MS provides the analytical capability to fulfill a wide range of exobiology flight experiment applications and has been included on a proposed Discovery Mission and proposals for both Lander and Orbiter of the European Space Agency's Rosetta Comet Mission. A data base of helium IMS spectra is now being built for these future applications.

Kojiro, Daniel R.↗

Detecting Organic Compounds Released from Iron Oxidizing Bacteria using Sample Analysis at Mars (SAM) Like Instrument Protocols

Mars is a planet of great interest for Astrobiology since its past environmental conditions are thought to have been favourable for the emergence life. At present, the Red Planet is extremely cold and dry and the surface is exposed to intense UV and ionizing radiation, conditions generally considered to be incompatible with life as we know it on Earth. It was proposed that the shallow subsurface of Mars, where temperatures can be above freezing and liquid water can exist on rock surfaces, could harbor chemolithoautotrophic bacteria such as the iron oxidizing microorganism Pseudomonas sp. HerB. The Mars Science Laboratory (MSL) mission will provide the next opportunity to carry out in situ measurements for organic compounds of possible biological origin on Mars. One instrument onboard MSL, called the Sample Analysis at Mars (SAM) instrument suite, will carry out a broad and sensitive search for organic compounds in surface samples using either high temperature pyrolysis or chemical extraction followed by gas chromatography mass spectrometry. We present gas chromatograph mass spectrometer (GC/MS) data on crushed olivine rock powders that have been inoculated with Pseudomonas sp. HerB at different concentrations ranging from approx 10(exp 2) to 10(exp 7) cells per gram. The inoculated olivine samples were heated under helium carrier gas flow at 500 C and the pyrolysis products concentrated using a SAM-like hydrocarbon trap set at -20 C followed by trap heating and analysis by GC/Ms. In addition, the samples were also extracted using a low temperature "one-pot" chemical extraction technique using N-methyl, N-(tert-butyldimethylsilyl) trifluoroacetamide (MTBSTFA) as the silylating agent prior to GC/MS analysis. We identified several aldehydes, thiols, and alkene nitriles after pyrolysis GC/MS analysis of the bacteria that were not found in the olivine control samples that had not been inoculated with bacteria. The distribution of pyrolysis products extracted from the bacteria was clearly distinct from similar GC/MS analyses of the carbonaceous meteorite Murchison that was dominated by sulfur containing aromatic compounds. A similar comparison, if organic compounds are detected by SAM on Mars, could be useful to help discriminate between meteoritic or biological origins.

Glavin, D. P.↗

Aliphatic hydrocarbons in meteorites.

Aliphatic hydrocarbons in meteorites, examining distribution of isoprenoid and other compounds via gas chromatography and mass spectrometry

METEORITIC COMPOSITION↗

Collection and analysis of NASA clean room air samples

The environment of the HALOE assembly clean room at NASA Langley Research Center is analyzed to determine the background levels of airborne organic compounds. Sampling is accomplished by pumping the clean room air through absorbing cartridges. For volatile organics, cartridges are thermally desorbed and then analyzed by gas chromatography and mass spectrometry, compounds are identified by searching the EPA/NIH data base using an interactive operator INCOS computer search algorithm. For semivolatile organics, cartridges are solvent entracted and concentrated extracts are analyzed by gas chromatography-electron capture detection, compound identification is made by matching gas chromatogram retention times with known standards. The detection limits for the semivolatile organics are; 0.89 ng cu m for dioctylphlhalate (DOP) and 1.6 ng cu m for polychlorinated biphenyls (PCB). The detection limit for volatile organics ranges from 1 to 50 parts per trillion. Only trace quantities of organics are detected, the DOP levels do not exceed 2.5 ng cu m and the PCB levels do not exceed 454 ng cu m.

Sheldon, L. S.↗

Gas chromatographic instrumentation for the analysis of aerosols and gases in Titan's atmosphere

Instrumentation presently being developed by NASA for the collection and analysis of organic gases and aerosols in Titan's atmosphere is described together with the results of the preliminary experiments. For the aerosols, stepwise pyrolysis was shown to be a suitable method for preparing complex organic material for gas chromatography (GC), and a pyrolysis-gas chromatograph was developed and successfully used to analyze a simulated Titan aerosol. Atmospheric gases will be collected by a low-pressure gas sampling system using large-volume sample loops and analyzed by GC. The results of preliminary studies using a 20 cu cm sampling system and a very sensitive metastable ionization detector showed that hydrocarbon components at the 10 ppb level can be detected. Studies are in progress on shortening the overall analysis time by improving the pyrolysis system, the gas sampling system, and the associated gas chromatograph. Further development of the gas sampling system is planned to ensure rapid collection of samples adequate for analysis by GC over the entire range of pressures to be encountered during the probe's descent.

Scattergood, T. W.↗

Biotransformation of an uncured composite material

The feasibility of biologically degrading prepreg wastes was studied. The work was conducted with the intention of obtaining baseline data that would facilitate the achievement of two long-range goals. These goals are: (1) the biological remediation of the hazardous components in the prepreg wastes, and (2) providing the potential for recycling the prepreg waste fibers. The experiments examined a prepreg that employs an bismaleimide resin system. Initial results demonstrated an obvious deterioration of the prepreg material when incubated with several bacterial strains. The most active cultures were identified as a mixture of 'Bacillus cereus' and 'Pseudomonas sp'. Gas chromatography analyses revealed seven primary compounds in the resin mixture. Biotransformation studies, using the complete prepreg material, demonstrated on obvious loss of all seven organic compounds. Gas chromatography-mass spectrometry analyses resulted in structure assignments for the two primary components of the resin. Both were analogs of Bisphenol A; one being bismaleimide, and the other being Bisphenol A containing a diglycidyl moiety. The 'diglycidyl analog' was purified using thin-layer chromatography and the biotransformation of this compound (at 27 ug/ml bacterial culture) was monitored. After a seven-day incubation, approximately 40% of the organic compound was biotransformed. These results demonstrate the biotransformation of the prepreg resin and indicate that biological remediation of the prepreg wastes is feasible.

Welsh, Clement J.↗