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  • Analytical Chemistry and Spectroscopy  (201)
  • 1980-1984  (201)
  • 1982  (103)
  • 1981  (98)
  • 1
    Electronic Resource
    Electronic Resource
    NQR investigations of 35Cl in crystalline 2,5-dichloro-4-nitroaniline (1981)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 16 (1981), S. 123-125 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Two NQR lines were observed for 35Cl in 2,5-dichloro-4-nitroaniline at room temperature, using a self-quenched super-regenerative spectrometer. Analysis of the Zeeman effect on the two lines using a cylindrical single crystal reveals that the crystal belongs to the monoclinic system. The principal field gradient Z axes enclose an angle of 35° and 28° in the cases of the low and high frequency resonance lines, respectively. The b axis is parallel to 81°, 280°. The unit cell contains either two or a multiple of two molecules. The molecules in the crystal can be arranged into two sets, with the molecular planes in each set being parallel among each other. The angle subtended between the two planes is 159° and each of the planes is inclined to the b axis at an angle of 79.5°. There is an in-plane bending of the two C—Cl bonds by 5.5°. The ionic, single bond and double bond characters of the C—Cl bonds for both chlorines are almost equal, and are in the ratio 24:73:3.
    Additional Material: 3 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270160212
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  • 2
    Electronic Resource
    Electronic Resource
    Gas chromatographic mass spectrometric determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma using the nitrogen-15 labelled compound as internal standard (1982)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 9 (1982), S. 333-335 
    Details
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A method for the quantitative determination of 1,2,3-propanetrioltrinitrate (nitroglycerin) in human plasma by gas chromatography mass spectrometry has been developed. After addition of 1,2,3-propanetriol(15N)trinitrate as internal standard, plasma (1 ml) is extracted by a mixture of pentane and methyl acetate (90:10). The extracts are purified by partition between, first, the extraction solvent and a mixture of acetonitrile and water (60:40) and, secondly, the resultant aqueous phase and benzene. The solvent is evaporated to a small volume before injection. The fragment ions at m/z 46 and 47 are monitored for the measurement of the [NO2]+ and [15NO2]+ ions using electron impact ionization. The mean recovery (%) ±SD in blind plasma samples spiked with amounts in the concentration range 0.35-3.52 nmol I-1, was 97.4 ± 9.0 (n = 58). Within a day, recovery experiments gave rise to coefficients of variation of 9.6, 6.4 and 2.7% at the levels 0.44,0.88 and 11 nmol I-1, respectively. Concentrations in plasma down to about 0.2 nmol I-1 (50 pg mI-1) could be estimated. Percent recovery of duplicate determinations in the range 0.5-1.96 nmol I-1± SD was 99.4 ± 6.0 (n = 80).
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/bms.1200090805
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  • 3
    Electronic Resource
    Electronic Resource
    1H and 13C NMR study of 8-hydroxyquinoline and some of its 5-substituted analogues (1981)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 15 (1981), S. 280-284 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 1H and 13C NMR spectra of 8-hydroxyquinoline (oxine) and its 5-Me, 5-F, 5-Cl, 5-Br and 5-NO2 derivatives have been studied in DMSO-d6 solution. The 1H and 13C chemical shifts and proton-proton, proton-fluorine, carbon-proton and carbon-fluorine coupling constants have been determined. The 1H and 13C chemical shifts have been correlated with the charge densities on the hydrogen and carbon atoms calculated by the CNDO/2 method. The correlation of the 1H and 13C chemical shifts with the total charge densities on the carbon atoms is approximately linear (rH2 = 0.85, rC2 = 0.84). The proton in peri position to the nitro group in 5-NO2-oxine is an exception.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270150314
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  • 4
    Electronic Resource
    Electronic Resource
    Carbon-13 NMR studies of benzoquinones (1981)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 15 (1981), S. 311-316 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The assignment of all ring carbons of p-benzoquinones derived from perezone and from thymoquinone was completed using gated decoupled spectra. The long range proton-carbon couplings are discussed in terms of the degree of substitution of the quinone ring. The tautomeric interconversion of the two energetically equivalent forms of 2,5-dihydroxy-1,4-benzoquinones has been studied in various solvents and at several temperatures.
    Additional Material: 2 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270150321
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  • 5
    Electronic Resource
    Electronic Resource
    Half-chair conformations of unsaturated heterocyclic compounds (1982)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 18 (1982), S. 92-97 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The vicinal proton coupling constants were obtained for some 6-membered ring unsaturated heterocyclic compounds. The R values and ring dihedral angles were determined and found to be consistent with half-chair conformations. Relative to saturated heterocyclic compounds, the effect of the sulfur atom on ring puckering was attenuated. However, an increase in ring puckering resulted from the sulfone group and was attributed to torsional energy.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270180210
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  • 6
    Electronic Resource
    Electronic Resource
    Chemistry of 6H-pyrido [4, 3-b] carbazoles. Part 10For Part 9, see Ref. 1. - Carbon-13 nuclear magnetic resonance spectra of ellipticines and some model compounds (1982)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 18 (1982), S. 117-119 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 13C NMR spectrum of ellipticine has been re-interpreted by reference to model compounds, and correlated with the spectra of a number of new ellipticine derivatives.
    Additional Material: 3 Tab.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270180215
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  • 7
    Electronic Resource
    Electronic Resource
    Examination of the aspirin acetylation site of human serum albumin by 13C NMR spectroscopy (1981)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 15 (1981), S. 158-161 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Human serum albumin has been specifically acetylated using aspirin in which the methyl carbon of the acetyl group was enriched to 90% 13C. A single resonance at 23.13 ppm downfield from tetramethylsilane was observed in 13C differences spectra obtained at both 25.2 and 45.3 MHz. Chemical shift studies of several model compounds suggest that this is the resonance position to be expected for an acetamide group exposed to solvent. The line width observed for the enriched methyl resonance is consistent with free rotation of the methyl group.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270150210
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  • 8
    Electronic Resource
    Electronic Resource
    Carbon-13 NMR characterization of the bispyridinium oximes, toxogonin, HS-3, HS-6 and HI-6 (1981)
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 16 (1981), S. 7-10 
    Details
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The structure of the bispyridinium oximes, toxogonin, HS-3, HS-6 and HI-6, used as antidotes in organophosphorus poisoning, is confirmed by 13C NMR spectroscopy. The 13C NMR spectra of the corresponding monopyridinium precursors substantiate the signal assignment in the bispyridinium oxime spectra. In all oximes studied the hydroxyiminomethyl group (—CH=N—OH) exists in the syn configuration. The 13C signal differences also readily allow analysis of binary mixtures of the oximes and provide an easy method for monitoring their stability.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/mrc.1270160103
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  • 9
    Electronic Resource
    Electronic Resource
    The use of triple quadrupoles for sequential mass spectrometry: 1 - The instrument parameters (1982)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 205-211 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Triple quadrupoles are becoming widely used in sequential mass spectrometry. The observed spectra are very dependent upon the choice of instrument parameters such as the gas target density, the mode of operation of the central quadrupole, and the direct current levels of the quadrupoles (rod-offsets) which determine the collision energy and the maximum mass resolutions in each analysing quadrupole. The influence of each of the instrument parameters is discussed with examples of experimental measurements of performance, and the optimum choice of modes of operation is determined.
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210170503
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  • 10
    Electronic Resource
    Electronic Resource
    The use of triple quadrupoles for sequential mass spectrometry: 2 - A detailed case study (1982)
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 212-219 
    Details
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A detailed exploration of the application of triple quadrupoles in sequential mass spectrometry has been carried out using dimethylmorpholinophosphoramidate as a case study of an ion of relatively high mass and complex structure. Both metastable ion decomposition and dissociation by low energy collision were examined. Variation of the basic instrument parameters allowed the investigation of the cross-section for dissociation as a function of collision energy, the change in fragmentation patterns with collision energy, the kinetic energy distributions of daughter ions and the overall kinetics of dissociation in a succession of ion decomposition sequences giving daughter and granddaughter ions. The daughter ions could also be produced in the source region and examined separately so that a genealogical tree could be established.
    Additional Material: 12 Ill.
    Type of Medium: Electronic Resource
    URL: http://dx.doi.org/10.1002/oms.1210170504
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