The steric analysis of aliphatic amines with two asymmetric centres by gas-liquid chromatography of diastereoisomeric amides.
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System has been used for problems such as analysis of volatile metabolities in human blood and urine, analysis of air pollutants, and in tobacco smoke chemistry. Since adsorbent is reusable after porper reconditioning, method is both convenient and economical. System could be used for large scale on-site sampling programs in which sample is shipped to central location for analysis.
Experimental tests were made to determine whether analysis of volatile metabolic products, formed in situ, is a viable procedure for an extraterrestrial life detection system. Laboratory experiments, carried out under anaerobic conditions with addition of carbon source, extended to include a variety of soils and additional substrates. In situ experiments were conducted without amendment using a vacuum sampling system.
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A comparative study of the sterol components of slash pine (Pinus elliotti) callus tissue cultures, seeds, and seedlings was carried out using GC-MS techniques. Cholesterol, desmosterol, campesterol, stigmasterol, sitosterol and cycloeucalenol were identified in all tissues while lophenol and 24-methylenelophenol were identified in only the seed and seedlings. 24-Ethylidenelophenol was detected in trace concentrations in only the seedlings. Sitosterol was the predominant sterol component, i.e., 80.8, 38.1 and 47.8% of the tissue culture, seed and seedling sterols, respectively.
Fundamantal concepts are developed which are required to optimize a gas chromatograph-mass spectrometer chemical analysis system suitable for use on an unmanned roving vehicle for Mars exploration. Prior efforts have developed simulation models for the chromatograph which were compared with data obtained from a test facility. Representation of binary systems by superposition was shown to be a first-order approximation and in certain cases large discrepencies were noted. This subtask has as its objective generation of additional binary data and analysis of the observed nonlinear effects.
Results are presented on a computerized gas chromatograph-mass spectrometer analysis of methylene chloride and n-heptane extracts of a No. 2 fuel oil accommodated estuarine water sample. The analytical method is briefly described, and the limitations on the identifications are categorized. Some attempt was made to determine major and trace constituents in the water accommodate. Altogether 66 hydrocarbon compounds were identified specifically, and 75 compounds were partially identified. Seven compounds could be recognized as major constituents of the water accommodated oil and ten were present only as traces. The aromatic compounds found were alkyl benzenes, naphthalene, tetralin, indane, biphenyl, fluorene, anthracene, and some of their alkyl substituted isomers in the range of carbon numbers C7 to C15. Four n-alkanes, C10 to C13, were found along with four other assorted hydrocarbons.
The potential of commercially available pulse-modulated electron capture detector (ECD)-equipped gas chromatographs for direct measurement of ambient levels of N2O is assessed. Since the sensitivity of ECD to N2O is directly proportional to the detector operating temperature and detector standing current, it is necessary to use a 'hot' ECD (250-350 C). The method is shown to be very precise with a standard error not exceeding 1% for automated analysis of ambient air samples. The technology is available to permit highly accurate routine direct analysis of N2O in the troposphere and stratosphere. Both captured air samples or direct real-time measurement from research vessels or airborne platforms are possible.
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Analysis of the volatiles and sublimate produced when para-polyphenylene is pyrolyzed to constant weight under vacuum in the temperature range from 380 to 1000 C indicates that the polymer undergoes thermal degradation in two stages. The first stage involved dehydrohalogenation, which is essentially a curing reaction that produces crosslinking between polyphenylene chains resulting from the loss of chlorine from the polymer in the form of hydrogen chloride. The second stage of the thermal degradation is dehydrogenation because hydrogen is the major volatile species. Increasing amounts of polycyclic aromatic hydrocarbons (phenanthrene and 9, 10 benzphenanthrene) in the sublimate, concomitant with increasing C/H ratios of the polymeric residue with pyrolysis temperature, is consistent with the buildup of polynuclear structures in the polymer matrix.
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Analysis made on commercially available liquid chromatograph demonstrates high-pressure liquid chromatographic conditions for separation of approximately 50 aromatic amines ranging from simple aniline derivatives to complex multiring di- and tri-amines.
Porous polyaromatic packing beads have low polarity, high efficiency, short retention time, and may be synthesized in size range of 50 to 150 micrometers (100 to 270 mesh). Mechanically strong beads may be produced using various materials depending on elements and compounds to be identified.