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  • Humans  (53)
  • Analytical Chemistry and Spectroscopy  (42)
  • LUNAR AND PLANETARY EXPLORATION  (38)
  • Lunar and Planetary Science and Exploration  (38)
  • 1
    Electronic Resource
    Electronic Resource
    Identification of mustard related compounds in aqueous samples by gas chromatography/mass spectrometry (1989)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1989), S. 484-491 
    Details
    ISSN: 0887-6134
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Capillary column gas chromatography/mass spectrometry, under electron impact and chemical ionization conditions, was used for the detection and identification of mustard and other sulfur vesicant-related decomposition products in a number of aqueous sample extracts. Interpretation of the mass spectral, infrared, chromatographic and trimethylsilyl derivatization data acquired during this study enabled the identification of nineteen sulfur vesicant-related hydrolysis products. Many of the compounds characterized during these analyses, including a number of ether/thioether macrocycles and vinyl alcohols, have either not been previously reported or have not been previously associated with the decomposition of munitions-grade mustard.
    Additional Material: 6 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200180707
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  • 2
    Electronic Resource
    Electronic Resource
    Evaluation of solvent venting with a gas purge for the introduction of microliter sample volumes in supercritical fluid chromatography (1993)
    New York, NY [u.a.] : Wiley-Blackwell
    Journal of Microcolumn Separations 5 (1993), S. 505-510 
    Details
    ISSN: 1040-7685
    Keywords: supercritical fluid chromatography ; large volume injection ; solvent venting ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Peak broadening and sample recovery are important considerations when working with large sample volume injections in capillary SFC. To measure possible contribution to peak broadening in the venting valve, a tee coupling was inserted between the retention gap and the column. A standard sample containing glyceryl esters was injected. Based on time variance measurements, the venting valve did not lead to measurable band broadening. Recovery was found to be dependent on the length of the retention gap, the CO2/He ratio in the purge gas, and the temperature of the retention gap. Cryofocusing was needed to increase the recoveries of volatile n-alkanes. To increase the recoveries of glyceryl esters, an enhanced CO2/He ratio was needed.
    Additional Material: 10 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mcs.1220050603
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  • 3
    Electronic Resource
    Electronic Resource
    The characterization of synthetic by-products by B/E linked scanning and high-resolution thermospray mass spectrometry (1991)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 20 (1991), S. 268-274 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Characterization of unknown synthetic by-products from a test synthesis of the experimental inhibitor of HIV-1 reverse transcriptase, BI-RG-587, is presented. Seven impurities were separated and characterized by thermospray liquid chromatography/mass spectrometry using low-resolution, high-resolution, and B/E linked scanning methods. The high-resolution mass measurements which were obtained were accurate to within 10 ppm of structures proposed for synthetic by-products present at the 0.1% level. Linked scans produced daughter ion spectra for each impurity to further aid in the characterization.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200200506
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  • 4
    Electronic Resource
    Electronic Resource
    Peptide ladder sequencing by mass spectrometry using a novel, volatile degradation reagent (1994)
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 8 (1994), S. 737-742 
    Details
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A conceptually novel approach to protein sequencing involves the generation of ragged-end polypeptide chains followed by mass spectroscopic analysis of the resulting nested set of fragments. We report here on the synthesis and development of a volatile isothiocyanate (trifluoroethylisothiocyanate) that allows the identification of several consecutive residues starting with a few picomoles of peptide. The nested set of peptides is generated simply by adding equal aliquots of starting peptide each cycle and driving both the coupling and cleavage reactions to completion. No additional reagents are required to act as chain terminators and retention of the peptide terminal amine allows for subsequent modification with quaternary ammonium alkyl NHS esters to improve sensitivity. Complex washing procedures are not required each cycle, as reagents and by-products are efficiently removed under vacuum, eliminating extractive loss. Multiple peptide samples can be processed simultaneously, with each degradation cycle completed in 35-40 min. The inherent simplicity of the process should allow for easy automation and permit rapid processing of samples in parallel.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/rcm.1290080916
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  • 5
    Electronic Resource
    Electronic Resource
    Improved thermospray accurate mass measurement using a magnetic sector instrument (1991)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 20 (1991), S. 389-391 
    Details
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method permitting accurate mass measurement of full-scan thermospray mass spectra is presented. Improved resolution and sensitivity were achieved by the addition of source cryopumping. Ion beam stability was enhanced by adaptation of a vaporizer tip with a sapphire orifice. Large systematic errors, such as previously reported with current-controlled scanning and widely spaced reference ions, were greatly reduced by employing field-controlled magnetic scanning. The method permits measurements accurate to better than 10 ppm while employing a simple polyethylene glycol standard.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200200610
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  • 6
    Electronic Resource
    Electronic Resource
    Rayleigh instability of stationary phase films in capillary column chromatography (1987)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 10 (1987), S. 128-136 
    Details
    ISSN: 0935-6304
    Keywords: Gas chromatography ; Capillary columns ; Coating of capillaries, static and dynamic ; Rayleigh instability ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The film of stationary phase on the wall of a capillary column and that of the phase solution during both static and dynamic coating is subject to Rayleigh instability, which is quite independent of so-called wettability. A theory is developed which shows that the logarithmic growth rate of Rayleigh instabilities is proportional to the surface tension and to the third power of the film thickness, and inversely to the viscosity and to the fourth power of the capillary diameter. Determination of the variation of the viscosities of stationary phase solutions with concentration in coating solvents, and the variation of the viscosities of neat stationary phases with temperature, both revealed that heating and/or diluting changed the viscosities of phases with π-electron-containing, groups much more than for polydimethylsiloxanes. Rayleigh instability is therefore more important during coating of phenyl-containing phases such as OV-17, and later during column operation. The efficiencies of capillary columns of different diameters coated with a number of phases under different conditions of temperature and coating rate, and then operated at different temperatures were in good agreement with the predictions of the theory.
    Additional Material: 8 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240100305
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  • 7
    Electronic Resource
    Electronic Resource
    On-line enzymatic reaction, extraction, and chromatography of fatty acids and triglycerides with supercritical carbon dioxide (1993)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 16 (1993), S. 358-363 
    Details
    ISSN: 0935-6304
    Keywords: Capillary SFC ; Edible fat ; Enzyme reaction ; On-line SFE-SFC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Supercritical carbon dioxide can be utilized both as an introduction solvent in capillary SFC and as a reaction medium; both possibilities are illustrated in this study. An off-line SFE unit was modified for on-line SFE-SFC. To facilitate rapid depressurization of the extraction cell and to prevent memory effects, a 6-port valve was installed at the outlet line of the extraction unit. An increased background signal was obtained when PEEK polymer was used in the construction of the extraction vessel; when stainless steel was used, the blanks improved. The synthesis of methyl esters and butyl esters of fatty acids from triglycerides in edible fat was examined using an immobilized lipase as a catalyst in on-line SFE-SFC. As a result of 30 minutes reaction - extraction time, high yields of fatty acid esters were obtained at a pressure of 150 bar and a temperature of 50°C.
    Additional Material: 11 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/jhrc.1240160605
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  • 8
    Electronic Resource
    Electronic Resource
    Deuterium isotope effects on 13C nuclear shielding as a measure of tautomeric equilibria (1982)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 18 (1982), S. 58-61 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Large deuterium isotope effects of both signs have been observed on the 13C nuclear shielding in proton-chelating tautomeric forms of β-thioxoketones, and small isotope effects of both signs have been found in related forms of Schiff's bases of salicylaldehydes. These effects are interpreted in terms of shifts in the tautomeric equilibria on deuterium substitution of the enolic proton. The observation of deuterium isotope effects is suggested as a useful method for the detection of fast tautomeric equilibria in systems of the following type. .
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270180114
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  • 9
    Electronic Resource
    Electronic Resource
    The NMR spectrum of pentafluorothiophenol (1969)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 1 (1969), S. 295-303 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High-precision line measurements and tickling were shown to yield information, often not accessible, on the assignment and signs of spin coupling constants. For pentafluorothiophenol-d, this information was obtained for the three meta-JFF's. Relative to C6F5SH, the 19F resonances in C6F5SD experienced an upfield ‘isotope’ shift.
    Additional Material: 4 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270010403
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  • 10
    Electronic Resource
    Electronic Resource
    13C—13C coupling constants in derivatives of trans-stilbene and tetraphenylethylene. Determination of relative signs II (1976)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 8 (1976), S. 632-637 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Magnitudes and signs of 13C—13C coupling constants in compounds of the type Ph13CR1R2—13CR1R2Ph have been determined and the results are discussed in a broader context. Two types of coupling constants, J(C-i, C-α) and J(C-i, C-β), between aromatic carbon atoms and the benzylic carbons, probably with different coupling mechanisms, are considered. Whereas 2J(C-2, C-α) are always found positive, 2J(C-1, C-β) in the present compounds are found to be negative or about zero. 3J(C-3, C-α) has the same sign as 2J(C-2, C-α). A 4J and a 5J were observed in trans-stilbene.
    Additional Material: 2 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270081209
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