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Xenon and krypton as carrier gases in a highly sensitive ionization system, for detection of permanent gases and organic vapors, by gas chromatography
The Sample Analysis at Mars (SAM) instrument onboard the Curiosity rover, is specifically designed for in situ molecular and isotopic analyses of martian surface materials and atmosphere. It contributes to the Mars Science Laboratory (MSL) missions primary scientific goal to characterize the potential past, present or future habitability of Mars. In all of the analyses of solid samples delivered to SAM so far, chlorinated organic compounds have been detected above instrument background levels and identified by gas chromatography coupled to mass spectrometry (GC-MS) (Freissinet et al., 2015; Glavin et al., 2013). While some of these may originate from reactions between oxychlorines and terrestrial organic carbon present in the instrument background (Glavin et al., 2013), others have been demonstrated to originate from indigenous organic carbon present in samples (Freissinet et al., 2015). We present here laboratory calibrations that focused on the analyses performed with the MXT-CLP GC column (SAM GC-5 channel) used for nearly all of the GC-MS analyses of the martian soil samples carried out with SAM to date. Complementary to the mass spectrometric data, gas chromatography allows us to separate and identify the species analyzable in a nominal SAM-GC run time of about 21 min. To characterize the analytical capabilities of this channel within the SAM Flight Model (FM) operating conditions on Mars, and their implications on the detection of organic matter, it is required to perform laboratory experimental tests and calibrations on spare model components. This work assesses the SAM flight GC-5 column efficiency, confirms the identification of the molecules based on their retention time, and enables a better understanding of the behavior of the SAM injection trap (IT) and its release of organic molecules. This work will enable further optimization of the SAM-GC runs for additional samples to be analyzed during the MSL mission.
Gas liquid chromatography resolution of racemic hydroxy and beta-mercapto-amino acids involving suitable derivation of functional group
High sensitivity optical resolution of amine diastereoisomers by gas liquid chromatography
Reagent menthyl chloroformate use in optical analysis of asymmetric amino and hydroxyl compounds by gas chromatography
Gas chromatography and mass spectrometry applied to porphyrin microanalysis, studying homologous porphyrin series in ancient sediments and oils
Results are presented from a study in which a continuously changed gaseous sample was monitored by multiplex gas chromatography (MGC), using the exponential dilution (ED) technique of Ritter and Adams (1976) to change the composition and concentration of a gaseous mixture in such a way as to imitate changes in the atmospheric gases sampled by a descending aircraft. A calibration of the MGC system was performed with four different rates of sample dilution, and the errors resulting from various degrees of change in the sample concentration were determined.
Cold trap concentrates oxygen and argon to determine trace amounts /as low as 0.1 ppm/ in helium by gas chromatography.
Soil moisture content was determined by extracting soil with methanol and subsequently analyzing the extract for water by gas chromatography. With air-dried mineral soils, this method gave slightly higher moisture content values than those obtained by the oven-dry method. Moisture content was determined quantitatively in soils to which various amounts of water had been added. The complete procedure, including extraction and analysis, requires less than one hour and gives results that closely compare to the oven-dry method.
The elution behavior of low molecular weight probes on inverse gas chromatography (IGC) columns is simulated using a computer. The IGC model is based on a polymer stationary phase of uniform thickness with a nonnegligible resitance to probe penetration. Three characteristic numbers are found to determine the whole process: Z(p) characterizing the distribution of the probe between phases, Z(f) describing the diffusion in the polymer phase, and Z(g) related to diffusion in the gaseous phase. For situations when Z(p)/Z(f) is less than 2, the standard evaluation procedures are virtually useless. The actual behavior of such systems is described.
Life detection for space missions based on detecting optical asymmetry in biogenic molecules by gas chromatography involving diastereomeric esters synthesis
Life detection for space missions based on detecting optical asymmetry in biogenic molecules by gas chromatography involving diastereomeric esters synthesis
To determine moisture content of soils rapidly and conveniently extract moisture with methanol and determine water content of methanol extract by gas chromatography. Moisture content of sample is calculated from weight of water and methanol in aliquot and weight of methanol added to sample.
A sensitive primary amine assay, capable of detecting 10 to the minus 11th g and utilizing the determination of the amine N-2,4-dinitrophenyl derivative by electron-capture gas chromatography is described. The method is exemplified by the determination of cyclohexylamine in sodium cyclamate.
One of the primary objectives of the 1976 Viking missions was to determine whether organic compounds, possibly of biological origin, were present in the Martian surface soils. The Viking gas chromatography mass spectrometry (GCMS) instruments found no evidence for any organic compounds of Martian origin above a few parts per billion in the upper 10 cm of surface soil [l], suggesting the absence of a widely distributed Martian biota. However, Benner et d. have suggested that significant amounts of non-volatile organic compounds, possibly including oxidation products of bioorganic molecules (e.g. carboxylic acids) would not have been detected by the Viking GCMS [2]. Moreover, other key organic compounds important to biology, such as amino acids and nucleobases, would also likely have been missed by the Viking GCMS as these compounds require chemical derivatization to be stable in a GC column [3]. Recent pyrolysis experiments with a Mars soil analogue that had been innoculated with Escherichia coli bacteria have shown that amino acid decomposition products (amines) and nucleobases are among the most abundant products generated after pyrolysis of the bacterial cells [4,5]. At the part per billion level (Viking GCMS detection limit), these pyrolysis products generated from several million bacterial cells per gram of Martian soil would not have been detected by the Viking GCMS instruments [4]. Analytical protocols are under development for upcoming in situ lander opportunities to target several important biological compounds including amino acids and nucleobases. For example, extraction and chemical derivatization techniques [3] are being adapted for space flight use to transform reactive or fragile molecules that would not have been detected by the Viking GCMS instruments, into species that are sufficiently volatile to be detected by GCMS. Recent experiments carried out at NASA Goddard have shown that using this derivatization technique all of the targeted compounds mentioned above can be separated on a GC column and detected by MS at sub-picomole (< 10(exp -l2 mole) levels. With these methods, the detection limit for amino acids, carboxylic acids and nucleobases is several orders of magnitude more sensitive than the Viking GCMS instruments for these compounds. Preliminary results using this analytical technique on a variety of Martian soil analogues will be presented.
Optical scanning and resolution of D, L amino acids by gas-liquid chromatography and mass spectrometry
Fabrication of a miniature gas chromatograph column using integrated circuit technology was studied and found to be feasible. A bonding problem of forming a strong, gas tight seal between two wafers of silicon has prevented the completion of the column design. Continuing research using tin or a chromium-gold bond promises to overcome the problems of using the proposed gold-eutectic bond. Specifications for the miniature gas chromatograph column are: a spiral capillary column of semi-circular cross section, 30 micron radius, and a total length of 6.9 meters etched into a silicon structure 50 mm in diameter and 0.625 mm thick.
Chromatographic materials were developed to serve as the stationary phase of columns used in the separation of atmospheric gases. These materials consist of a crosslinked porous polymer matrix, e.g., a divinylbenzene polymer, into which has been embedded an inorganic complexed ion such as N,N'-ethylene-bis-(acetylacetoniminato)-cobalt (2). Organic nitrogenous bases, such as pyridine, may be incorporated into the chelate polymer complexes to increase their chromatographic utility. With such materials, the process of gas chromatography is greatly simplified, especially in terms of time and quantity of material needed for a gas separation.