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  • Articles  (21)
  • Analytical Chemistry and Spectroscopy  (21)
  • SPACECRAFT DESIGN, TESTING AND PERFORMANCE
  • 11
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 27 (1992), S. 609-610 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical ionization (CI) and electron impact (EI) mass spectra of eight symmetrical S-alkyl alkanesulfonothioates (thiosulfonates) are reported.
    Additional Material: 2 Ill.
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  • 12
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 27 (1992), S. 611-614 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical ionization (CI) and electron impact (El) mass spectra of six S-1-chloroalkyl alkanesulfonothioates (thiosulfonates) are reported.
    Additional Material: 2 Tab.
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  • 13
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 9 (1977), S. 75-79 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 13C and 15N n.m.r. results for a series of diazo compounds are reported. It is found that the diazo carbon is shielded by an extraordinary amount compared with normal sp2 hybridized carbons. The 15N chemical shifts reveal that the terminal nitrogen is deshielded relative to the central one. This is contrary to that expected from charge effects but support is found for this phenomenon in other systems. One-bond 13C—14N coupling in diazomethane is also reported for the first time. INDO MO calculations of the charges and finite perturbation calculations of 13C—14N and C—H couplings are compared with the experimental results.
    Additional Material: 4 Tab.
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  • 14
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 114-122 
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The chemical ionization and electron impact mass spectra of some thiosulfinates, thiosulfonates and sulfinyl sulfones have been studied. The electron impact mass spectra of four of the six thiosulfonates show molecular ions of less than 1%. Inconclusive evidence was obtained for sulfenyl sulfinate type intermediates in the electron impact spectra of thiosulfonates. The electron impact spectra of thiosulfonates were similar to those of thiosulfonates. The chemical ionization (isobutane) mass spectra of thiosulfinates and thiosulfonates generally show protonated molecular ions [MH]+ as base peaks and [MH+1]+ and [MH+2]+ peaks.
    Additional Material: 5 Tab.
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  • 15
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 21 (1983), S. 86-93 
    ISSN: 0030-4921
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: 13C NMR spectra of thiols, sulfinic acids, sulfinyl chlorides, sulfonic acids and sulfonic anhydrides have been obtained. The data are discussed in terms of the additivity of the deshielding effects exerted by the sulfur functionality at the α- or β-position, and the shielding effects produced by the sulfur function at the γ-position.
    Additional Material: 9 Tab.
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  • 16
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In general, ions corresponding to [M + H]+ and/or [M + NH4]+ are observed in thermospray mass spectrometry (TSMS) when using ammonium acetate in the liquid carrier. For several quinones investigated, unique thermospray mass spectra were detected with a mass spectral peak corresponding to an [M + 16]+ ion being observed in aqueous ammonium acetate solutions. Investigation of l,4-benzoquinone (BQU) and structurally analogous quinones indicated that amine conjugate formation with BQU and similar quinones was the origin of the unique [M + 16]+ ion in TSMS. When methanol was added to the liquid carrier, ions corresponding to methoxy conjugation were detected. High-performance liquid chromatography followed by TSMS or electrochemical detection gave evidence that this amine and methoxy conjugate formation was occurring in the thermospray source area.
    Additional Material: 6 Ill.
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  • 17
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 32 (1994), S. 134-137 
    ISSN: 0749-1581
    Keywords: NMR ; 13C,H long-range couplings ; Strychnine ; Hadamard spectroscopy ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Long-range 13C,H NMR coupling constants were measured in strychnine at 400 MHz by a method that employs selective excitation of individual 13C sites under decoupled conditions followed by polarization transfer to protons. The sensitivity was improved by performing eight simultaneous soft-pulse experiments coded (±) according to a Hadamard matrix and later separated by reference to the same matrix. The antiphase 13C,H splittings were measured by J-doubling performed in the frequency domain.
    Additional Material: 4 Ill.
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  • 18
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 903-910 
    ISSN: 0749-1581
    Keywords: Multi-dimensional spectroscopy ; Nuclear magnetic resonance ; NMR ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Multi-dimensional NMR spectroscopy must satisfy the Nyquist sampling condition in all frequency dimensions. This entails very long experiments and very large data arrays, and may mean that fine structure of cross-peaks cannot be adequately digitized. This sampling restriction can be sidestepped in an alternative approach which explores the new frequency dimensions by scanning selective radiofrequency pulses in small steps over narrow frequency ranges. A pulse envelope shaped according to the first half of a Gaussian curve is particularly well suited to this task. Thus a form of double resonance experiment can be used to generate two-dimensional correlation spectra that have all the features of the well known COSY experiment, with an additional ‘zoom’ capability that reveals the detailed fine structure information. For systems of three coupled spins the corresponding triple resonance experiment generates a three-dimensional correlation specrum, the frequency scans being restricted to the region of interest (the 3D cross-peak) based on information from the conventional NMR spectrum. For correlation spectroscopy of higher dimensionality no frequency search is employed, the selective pulses simply being set at predetermined chemical shift frequencies. A four-dimensional correlation experiment is described which uses population transfer to establish that four non-equivalent protons are coupled in a chain I—S—R—P. It employs an initial ‘ZZ-pulse’ applied at the I-spin frequency to excite longitudinal two-spin order (2IzSz) which is then propagated along the chain by the application of selective ‘ZZZ-pulses’ to the intermediate spins S and R, creating an antiphase intensity perturbation (2RzPz) on the P multiplet. The procedure is recursive and can in principle be extended to N spins coupled pairwise in a ‘linear’ chain. This is a powerful diagnostic tool for structure determination and can be adapted to recognize other topological features such as chain branching and ring closure.
    Additional Material: 12 Ill.
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  • 19
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 26 (1988), S. 813-816 
    ISSN: 0749-1581
    Keywords: 13C NMR ; 1H NMR ; Bis(1,1-dimethylethyl) disulfide ; Bis(1,1-dimethylethyl) trisulfide ; sulfinothioic acid S-esters ; sulfonothioic acid S-esters ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The 13C NMR and 1H NMR spectra of bis(1,1-dimethylethyl) disulfide and bis(1,1-dimethylethyl) trisulfide and their oxygenated derivatives, including sulfinothioic acid S-esters and sulfonothioic acid S-esters, have been studied. Deshielding βSO and βSO2 effects and shielding γSO and γSO2 effects are observed. The NMR spectra of tert-butyl polysulfides and the influences of sulfur atoms are also compared and discussed.
    Additional Material: 3 Tab.
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  • 20
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A mixture of hydroxypolychlorodibenzofurans was isolated from technical pentachlorophenol. The alkyl ethers were prepared, and analyzed by fused silica capillary column gas chromatography electron capture negative ion chemical ionization mass spectrometry. The appearance of intense molecular ion peaks for the alkyl ethers apparently depends on the ring position of alkoxy substitution. Loss of chlorine atoms from the ring, followed by protonation of the resultant anion as the alkyl group is eliminated, is postulated on the basis of deuterium labeling experlments. Evidence is also presented for the presence of a hydroxyheptachlorodibenzodioxin in technical pentáchlorophenol.
    Additional Material: 4 Ill.
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