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  • Analytical Chemistry and Spectroscopy  (316)
  • 1975-1979  (316)
  • 1
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 8 (1976), S. 354-356 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: 77Se n.m.r. spectra of twenty-six organoselenium compounds, including some with an endocyclic selenium atom, have been recorded. Our measurements complete the scale of chemical shifts previously established by McFarlane. It seems difficult to define a range of chemical shifts which is characteristic of the valency state of selenium or of its endo- or exocyclic position. Some results are discussed qualitatively. In the case of selenolo[2,3-b]thiophene, evidence has been obtained for a 4J[Se, H] coupling across the sulphur atom.
    Notes: La résonance magnétique du 77Se a été observée dans vingt-six composés organiques dont certains contiennent un atome de sélénium endocyclique. Nous avons pu ainsi compléter l'échelle de déplacements chimiques établie par McFarlane. II apparaît difficile de définir une gamme de déplacement chimique du 77Se caractéristique de son état de valence ou de sa position endo- ou exocyclique. Certains résultats sont discutés qualitativement. Dans le cas du sélénolo [2,3-b]thiophène, des arguments en faveur d'un couplage 4J(Se, H) à travers l'atome de soufre ont été découverts.
    Additional Material: 4 Tab.
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  • 2
    ISSN: 0049-8246
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: A low-energy spectrometer for the X-ray analysis of plutonium and plutonium-containing materials has been built. We use ultra-thin window to maintain different pressures and contamination level in the spectrometers's sample and crystal chambers. Ultra-thin windows are also used on the X-ray tube and detector. Methods have been developed by which the spectrometer can analyze both metal and loose-powder samples. Representative calibration spectra are presented for the fluorine band in polyfluoroethylene, the oxygen band in α-Al2 O3, and the carbon band in graphite. Experimental spectra are presented for the fluorine band in PuF3 and for the oxygen ban in PuO2.
    Additional Material: 3 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 671-673 
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Combined gas chromatography mass spectrometry was used to separate and identify a carrageenan component suspected of being the acid ketal 4,6-O-(1-carboxyethylidene)-D-galactose. The mass spectral fragmentation pattern is presented as evidence for the presence of this component in the carrageenan from Petrocelis middendorfii (P. francisana).
    Additional Material: 3 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 6 (1979), S. 173-178 
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A study of the effect of crystal size on the bioavailability of benoxaprofen, 2-[4-chlorophenyl]-α-methyl-5-benzoxazoleacetic acid, in man is reported. The technique utilized comparison of either the plasma concentrations or urine levels, resulting from administration of deuterium labeled (2H7) drug in solution coadministered with a test capsule formulation. Drug concentrations were determined by gas chromatography, and the ratio of labeled to unlabeled drug was obtained by gas chromatography mass spectrometry. Measurements following coadministration of labeled and unlabeled drug in solution established the absence of an isotope effect due to the presence of deuterium. The dry formulations consisted of either a 3.17-100 micron fraction (mean = 18.5 microns) or a 32-1000 micron fraction (mean = 610 microns) formulated with starch powder. The results in three subjects indicate an almost complete availability (0.95-0.98) of the small crystals as measured by comparison of either area under the plasma level curves or urine excretion (0.94-0.97) of labeled versus unlabeled drug measured to 168 hours. The larger crystals exhibited a lower availability as shown by plasma levels (0.41-0.46) or urine recovery (0.39-0.43). A higher dose of the large crystal formulation resulted in decreased relative availability with a fourfold dose dropping availability to 0.22 in a single subject.
    Additional Material: 6 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 380-381 
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Gas phase carboxylate anions have been efficiently generated from the p-nitrobenzyl esters of nine fatty acids ranging in size from C6 to C22. The process involves the dissociative resonance capture of 2.9 eV electrons by the derivatives. The procedure is specific and gives the carboxylate anions as the base peak in all but two of the derivatives. The technique gives extremely simple spectra, with little additional fragmentation and no rearrangement ions.
    Additional Material: 1 Ill.
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  • 6
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The complete 1H and 13C NMR assignments for 3,6-epoxypentacyclo[6.2.2.02,7.04,10.05,9]dodecane and 3,6-epoxypentacyclo[6.2.1.02,7.04,10.05,9]undecane are reported. The difference between the 1H and 13C chemical shifts and one-bond proton-carbon coupling constants of these two compounds are adequately explained by the difference in the hybridization of the C—H bonds.
    Additional Material: 1 Ill.
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  • 7
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 11 (1978), S. 535-540 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A data base containing approximately 4000 13C nuclear magnetic resonance spectra has been assembled. The spectra have been evaluated and all the corresponding compounds have been registered by the Chemical Abstracts Service (CAS). The data base is available to the international scientific community on magnetic tape or microfiche and is also the basis of a search system operating upon an international computer network.
    Additional Material: 5 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1978), S. 163-166 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Chemical ionization mass spectra of exo- and endo-2-norbornanols and their phenylurethane derivatives have been obtained with several reactant ions. Small differences are noted in the abundances of norbornyl and [M+H]+ ions for the phenylurethane derivatives: more norbornyl ions with the exo compounds. Relative rate constants for decomposition of [M+H]+ ions, kexo/kendo ≅ 1-2. No evidence was found for s̰-participation in the decomposition of these ions. The i-C4H10 chemical ionization spectrum of endo-2-norbornanol contains a much greater abundance of [M-H]+ ions than the i-C4H10 chemical ionization spectrum of exo-2-norbornanol. This difference presumably results from steric hindrance toward attack of the endo hydrogen.
    Additional Material: 2 Tab.
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  • 9
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 12 (1977), S. 55-62 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In order to provide a comparison with the extensive research on the mechanism for elimination of water from various cyclohexanols, the mass spectra of 1-tetralol(1,2,3,4,-tetrahydro-1-naphthalenol) and 2-tetralol(1,2,3,4-tetrahydro-2-naphthalenol) have been investigated. Deuterium labeling experiments show that the 1-tetralol molecular ion expels water by a highly specific 1,4 elimination, whereas 2-tetralol undergoes a 1,3 elimination. Both of these processes are competitive with cycloreversion reactions. The ionization potentials and appearance potentials for the major fragments \documentclass{article}\pagestyle{empty}\begin{document}$ \left[{{\rm M - H}_{\rm 2} {\rm O}} \right]_{}^{_.^ + } $\end{document} and the cycloreversion products hae been measured using the Electron Distribution Difference method. In addition, the kinetic energy release in the metastable decompositions to lose water have been measured. It has been found that the 1,4 elimination for 1-tetralol releases over 50% of the available energy in the transition state, which is unexpected in view of the 6-membering ring transition state involved. This research also includes an investigation of the nature of the various \documentclass{article}\pagestyle{empty}\begin{document}$ \left[{{\rm C}_{{\rm 10}} {\rm H}_{{\rm 10}} } \right]_{}^{_.^ + } $\end{document} ions formed in the rearrangement reaction to lose water.
    Additional Material: 3 Ill.
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  • 10
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 13 (1978), S. 397-401 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The ion cyclotron resonance spectra of anisol, 3-methylanisol, phenetol, 3-methylphenetol and thioanisol at pressures of 10-6 Torr resemble the normal mass spectra. Above 10-5 Torr the spectra show signals due to product ions. As seen from double resonance measurements most product ions are formed by the reaction of a fragment ion with a neutral ether molecule under elimination of alkyl, alkoxy alkylthioradicals or of ethylene. Apart from the molecular ion radical ions do not participate in ion-molecule reactions.
    Notes: Die ICR-Spektren von Anisol, 3-Methylanisol, Phenetol, 3-Methylphenetol und Thioanisol, die bei 10-6 Torr weitgehend mit den normalen Massenspektren übereinstimmen, zeigen oberhalb von 10-5 Torr zahlreiche Signale von Produktionen. Doppelresonanzmessungen ergaben, daß die meisten Produktionen durch Reaktion eines Fragmentions mit einem Äthermolekül unter Abspaltung eines Alkyl-, Alkoxy- oder Thioalkylradikals bzw. von Äthylen entstanden sind. Daneben finden sich einzelene Produktionen (möglicher-weise Ion-Molekül-Komplexe), die durch Zusammentreten von Ionen mit Äthermolekülen ohne Eliminierung entstanden sind. Radikalionen, mit Ausnahme des Molekular ions, nehmen nicht an den Ionen-Molekül-Reaktionen teil.
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