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  • Analytical Chemistry and Spectroscopy  (4.318)
  • 1980-1984  (4.318)
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Verlag/Herausgeber
Erscheinungszeitraum
Jahr
  • 1
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1984), S. 573-576 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A detailed energy-resolved study of the fragmentation of CH2=CHCH(OH)CD2CD3 (1-d5) has been carried out using metastable ion studies and charge exchange techniques, combined with collision-induced dissociation studies to establish the structures of fragment ions. At low internal energies (metastable ions) the molecular ion of 1-d5 rearranges to the 3-pentanone structure and fragments by loss of C2H5 or C2D5 leading to the acyl structure, [CH3CH2C≡O]+ or [CD3CD2C≡O]+, for the fragment ion. However, with increasing internal energy of the molecular ion this rearrangement process decreases rapidly in importance and loss of C2D5 by direct cleavage, leading to [CH2=CHCH=OH]+, becomes the dominant fragmentation reaction. As a result the [C3H5O]+ ion seen in the electron impact mass spectrum of 1-penten-3-ol has predominantly the protonated acrolein structure.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 2
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 312-315 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: It is shown that under field desorption conditions some less volatile or non-volatile compounds such as oligosaccharides, sulphonic acids and fatty acids can be ionized below the threshold of field electron emission by clustering with anions. In all cases the sample, together with polyethylene oxide 4000, is dissolved in water. The source of the clustering anion is provided either by a small amount of a salt added to this solution (sugars) or by the compounds themselves (sulphonic and fatty acids). The solution is applied to unactivated and/or slightly activated 10 μm tungsten wire cathodes. Suitable clustering ions for the sugars appear to be [Cl]-, [NO3]- and to a lesser extent [Br]- and [I]-. Most of the sulphonic acids studied give rise to the formation of [Mn - H]- ions (n≤5), but their potassium salts yield only unclustered sulphonate anions. However, the addition of a small amount of LiCl to the mixture of benzene sulphonic acid and polyethylene oxide 4000 promotes the formation of clustered anions, [(M - H)2Li]- being by far the most abundant if activated cathodes are used. This addition of some LiCl is essential in the case of fatty acids: without LiCl no anions may be desorbed at all from activated wires, but with the presence of LiCl both [M - H]- and the most abundant [(M - H)2Li]- anions are easily generated.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 3
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 525-529 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The positive ion field desorption (FD) spectrum of arginine taken at the best anode temperature only contains a peak due to [M+H]+ ions. At higher emitter temperatures a considerable amount of fragmentation is induced and the [M+H—NH3]+ ions become most abundant. Specific 15N labelling reveals that the eliminated ammonia molecule, exclusively, contains one of the terminal nitrogen atoms of the guanidyl group. This also applies to the ammonia loss from metastably decomposing [M+H]+ ions. The positive ion fast atom bombardment (FAB) spectrum shows more fragmentation than the FD spectrum. In contrast with the FD results, the [M+H]+ ions generated upon FAB with ion lifetimes 〈10-6 s eliminate both ammonia containing one of the terminal nitrogen atoms of the guanidyl group and ammonia containing the α-amino group in the ratio of 1.35, as found by 15N labelling. The metastably decomposing [M+H]+ ions, however, eliminate only the former ammonia molecule. In the negative ion FD and FAB spectra no other peak than that corresponding to the [M—H]- ion is observed. Some attention has been paid to the thermal degradation of arginine on the basis of a few Curie-point pyrolysis experiments.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 4
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 169-171 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Glass capillary columns ; Trimethylsilyl derivatives ; Pregnant mares' urine estrogens ; Estrone-equilin separation ; OV-225, Silar 10C stationary phases ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Glass capillary columns coated with OV-225 and Silar 10C were used to analyze estrogens (as their trimethylsilyl derivatives) present in pregnant mares' urine. Such columns provide better resolution in a shorter time than the corresponding packed columns, as exemplified by the separation of estrone from equilin.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 5
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 21 (1983), S. 315-318 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The analysis of the 1H NMR spectra of 2,8-dithia-1,5-diphosphabicyclo[3.3.0]octane, 2,8-dithia-1-phospha-5-azabicyclo[3.3.0]octane and 2,8-dithia-1-arsa-5-phosphabicyclo[3.3.0]octane is supported by means of 2D- J-resolved NMR measurements. The spectra suggest a preferred conformer with strong puckering of the fused five membered rings.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 6-10 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Retention index calculation by correlation techniques ; Use of n-dialkyl sulphides as standards ; Use of selective detectors ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Retention indices were determined for a homologous series of n-dialkyl sulphides on three stationary phases (SE-30, OV-17 and XE-60) under isothermal and linear temperature programming conditions. Under these two different GC conditions, equations were derived for each of the three stationary phases which showed the dependence of retention index on the number of carbon atoms and the boiling points for a homologous series of n-dialkyl sulphides. The equation for the correlation isothermal retention index was shown to be applicable to the identification of n-dialkyl sulphides using linear temperature programming. It was found that the GC behaviour of n-dialkyl sulphides makes these compounds suitable for use as a standard series instead of n-alkanes for the calculation of retention indices in GC analysis in which detectors insensitive to n-alkanes are employed. The use of the homologous series of n-dialkyl sulphides for the calculation of sulphide retention indices can be great practical importance in the microanalysis of natural compounds. We have used this method successfully in the analysis of pesticides containing S-atoms.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 7
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 306-309 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, HPLC ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method is described for separation of low amounts of DHETX m. s. from human plasma, based on extraction and determination by high performance liquid chromatography with fluorimetric detection.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 8
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 370-374 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Trace analysis ; On-column injection ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Large sample volume on-column injection (up to 250 μL) of n-pentane solutions of halogenated hydrocarbons has been employed for the direct measurement of both low-boiling and high-boiling compounds in what is essentially a single run. Two-bonded phase, fused-silica capillary columns are joined in series, through which the low-boiling compounds are first chromatographed and detected with an electron capture detector. High-boiling compounds are then trapped in a section joining the two columns, and subsequently chromatographed in the second column, using the same detector. This procedure permits analysis at the ppt level.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 9
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 74-78 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The fragmentation pathways of RDX in chemical ionization mass spectrometry have been rationalized, using data from different reagent gases, including CD4 and iso-C4D10. The dependence of spectra taken with different gases on the acid strength of the reactant ions in the gases is accounted for.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 10
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 440-446 
    ISSN: 0935-6304
    Schlagwort(e): High performance thin-layer chromatography ; β-adrenoceptor blocking drugs ; Continuous development ; Multiple development ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: High performance thin-layer chromatography was used for the separation of nine therapeutically important and structurally similar β-adrenoceptor blocking drugs on silica gel plates. In situ scanning of the plate in the reflectance mode gave detection limits in the low nanogram range depending on the individual drug and the wavelength selected for its determination. Scanning the HPTLC plate at several wavelengths can be used to aid the identification of partially resolved components. Continuous development and continuous multiple development techniques are compared for the simultaneous separation of the drug mixture.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 11
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1984), S. 645-646 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 12
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 12 (1982), S. 165-172 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The temperature dependence of νi, Δν1/21 and the integrated band area for a few solid amides are studied for the γ(N—H) mode in the infra-red. A general theoretical discussion of these structureless broad γ(N—H) bands is presented. The bands are accounted for in terms of coupling of the γ(N—H) mode with longitudinal as well as transversal low-frequency phonons.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 13
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Packed and capillary columns ; Fungicides and insecticides ; Adsorption ; Length of column ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 14
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 614-616 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass fragmentation of three dinucleotide analogues in which D-ribose phosphodiester linkages were replaced by a three methylene unit chain has been investigated. The fragmentation pathways were proposed on the basis of high resolution data and metastable transitions. These compounds demonstrated a unique fragmentation with the formation of the fragment ion containing nitrogen at the end of the C3H6 chain.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 15
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 372-373 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 16
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The translational energy, T, released during CH3· loss from the molecular ions of epimeric steroid ketones and from both molecular and [M-H2O]+· ions of epimeric alcohols of the androstane, pregnane and cholestane series, differing in the mode of the A/B ring junction, has been measured. These data provide a simple and rapid method for identifying the configuration of the epimeric centres. Of the compounds studied, it is found in 3-hydroxy steroids that the 5β-isomers release the smaller amounts of translational energy for CH3· loss. In most of the 3-keto steroids investigated, the opposite is found, i.e. the larger T values are observed for the 5β-isomers. Exceptions occur when further keto groups are introduced at the 11- or 17-positions. A small range of epimeric pairs of 17-hydroxy, 17-keto and 4-keto steroids have also been studied, the 5β-isomer giving the lower T value in each case. The importance of hydroxy and keto groups at the various sites within the steroid structure in determining the T values is discussed.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 17
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 9 (1980), S. 263-265 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The Raman spectrum of a single crystal of monoclinic B-type (C2h3) gadolinium sesquioxide is presented. The low temperature polarization studies allowed the unambiguous attribution of 20 among the 21 normal modes expected according to the C2h factor group analysis predictions.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 18
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 328-329 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 19
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 52-52 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 20
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 375-375 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 21
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 3 (1984), S. 479-526 
    ISSN: 0277-7037
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 22
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 212-214 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The field ionization mass spectrum of diethylamine on a 5 μm activated wire at 300 K yields surface product ions like protonated molecular ions and doubly charged ions as well as gas phase ions like parent minus CH3 group. Variations of the reaction rate as a function of the decomposition times in the range 10-11-10-6 s for the elimination of a CH3 group are studied. The reaction rates are evaluated with the help of the retarding potential technique.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 23
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 18 (1982), S. 185-189 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The measurements of T1 relaxation times in 13C NMR spectroscopy are used to determine solute-solvent interactions. endo- and exo-Bicyclo[3.2.1]octan-3-ol and the corresponding bromohydrins are used as substrates. In a non-polar solvent, such as cyclohexane, solute-solvent interactions occur exclusively, whereas in the more polar acetone only solute-solvent interactions are observed. In chloroform, which is of intermediate polarity, the two types of interactions (solute-solute and solute-solvent) occur simultaneously.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 24
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1984), S. 464-466 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 25
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass spectra of 5,5-diphenylmonothiohydantoins and their N- and S-methyl derivatives have been investigated and interpreted in terms of structural correlations. All stable isomers can be easily distinguished by their fragmentation patterns.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 26
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The influence of functional group interaction on the intensity ratios (Q) of product ions from α-fission of ethyl-tert-alkylamines C2H5(C3H7)(HO(CH2)n)C —NHC2H5, in which one side chain of the tert-alkyl moiety is replaced by a hydroxyalkyl group of varying chain length, was investigated. It was found that only through-bond interaction between the functional groups has a major influence on these ratios. By substitution of a hydrogen by a halogen atom in one side chain it was shown that the so-called ‘ion mass effect’ is a degrees of freedom effect.
    Zusätzliches Material: 3 Ill.
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  • 27
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 253-260 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Interpretation of the metastable ion transitions found in normal electron impact mass spectra of appropriate compounds, shows that ions (C4 to C13) of structures \documentclass{article}\pagestyle{empty}\begin{document}${\rm R - CH = }\mathop {\rm O}\limits^{\rm + } {\rm H} $\end{document}, (a), \documentclass{article}\pagestyle{empty}\begin{document}${\rm R}^{\rm 1} ({\rm R}^{\rm 2} ){\rm C = }\mathop {\rm O}\limits^{\rm + } {\rm H}$\end{document} (b), and \documentclass{article}\pagestyle{empty}\begin{document}${\rm R}^{\rm 1} ({\rm R}^{\rm 2} ){\rm C = }\mathop {\rm O}\limits^{\rm + } {\rm R}^{\rm 3}$\end{document} (c) are clearly distinguishable from each other (R = alkyl). Within the latter series c those ions with R3 = methyl and R3〉methyl exhibit totally different behaviour. Low homologues are shown to behave exceptionally. Therefore, general conclusions drawn from their reactions must be regarded with caution. Except for these low homologues, ions b and c only isomerize within their groups, but not to each other or to other acyclic ‘oxonium’ ions. Ions a probably have a minor pathway to isomerize to b, and ions c with R3〉methyl were found not to isomerize at all prior to slow decompositions.
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  • 28
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 460-470 
    ISSN: 0935-6304
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 29
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 10 (1983), S. 633-640 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Combined high performance liquid chromatography mass spectrometry using a moving belt interface was used to investigate C-methylation artifacts arising from the permethylation reaction of peptides with methyl sulfinyl carbanion and methyl iodide. C-Methylation was not limited to glycine but, depending on the reaction conditions, other amino acids were also susceptible to it. In the absence of a glycine residue, preference for C-methylation of the C-terminus amino acid was observed. The use of on-line high performance liquid chromatography mass spectrometry allowed the separation of N, O, C-methylated from the N, O, S-permethylated derivatives, thus facilitating interpretation of the mass spectra.
    Zusätzliches Material: 6 Ill.
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  • 30
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 9 (1980), S. 166-171 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: We have designed and assembled a sensitive vidicon Raman spectrometer which is shown to be well suited for the studies of heme proteins in both Soret (near-ultraviolet) and Q (visible) band regions. This system, employing a dry ice-cooled silicon intensified target (SIT) detector and an additive dispersion double monochromator (two 600 g mm-1 gratings blazed at 400 nm), has excellent stray light rejection and optimum bandpass and resolution (5-12 cm-1) for biological applications. It is demonstrated that a 600 cm-1 wide section of the low frequency Raman spectrum of ferrocytochrome c excited at 413.1 nm (70 mW) can be obtained in 30 ms, which is ˜ 2×104 times faster than that required by the conventional scanning techniques. Our multichannel Raman system has an enhanced detection capability which enables us to identify at least 41 weak Raman lines below 850 cm-1 in the spectrum of ferrocytochrome c. Using the SIT detection system, the Raman excitation profile of a depolarized line at 750 cm-1 in Fe(II) cytochrome c has been constructed and compared with that reported for Ni etioporphyrin. Instead of strong 0-0 Raman intensity, the cytochrome c profile exhibits weaker 0-0 intensity, indicative of the absence of the Jahn-Teller effect. It is further demonstrated that the Soret-excited Raman spectrum of oxyhemoglobin can be readily obtained without photodissociation.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 31
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 11 (1981), S. 150-154 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Interactions of cobalt(III) ion with adenosine-5′-triphosphate in the presence of 1,10-phenanthroline and superoxide were studied by laser Raman spectroscopy. Striking intensity enhancement of two adenine ring vibrations at 734 and 1430 cm-1 was observed upon formation of the complex Co(III)-(phen)-ATP-O2-. The effect could be abolished by addition of cyanide ion to replace the superoxide ion. The spectral features were interpreted as indicating a direct binding of Co(III) to the C6-NH2 group of adenine. The interaction between Co(III) and 1,10-phenanthroline was manifested in the frequency and intensity changes near 436 and 1064 cm-1. Raman intensities at 734, 1312, 1055 and 1430 cm-1 were measured as a function of laser exciting wavelength. The gradual changes in Raman excitation profiles of ATP lines from 647.1 nm to 457.9 nm indicated the preresonance effect with a charge transfer transition between adenine and Co(III), which may lie between 300 and 400 nm as evidenced by the more dramatic enhancement of these lines with 406.7 nm excitation.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 32
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 22 (1984), S. 131-135 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 13C and 15N NMR chemical shift and spin-lattice relaxation data have been measured for both meso- and racemic-pentane-2,4-diamine. At high pH (12), relaxation is consistent with hindered rotation of the NH2 group due, in part, to the formation of intramolecular hydrogen bonds. At low pH (2), relaxation is consistent with relatively unhindered rotation of the NH3+ group. Rotational jump rates and barriers are reported, determined from the NT1 ratios between 15N and 13C nuclei. In all cases, the ratios for the racemic diastereomer are higher than those of the meso compounds; this is interpreted in terms of conformationally more stable intramolecular hydrogen bond formation in the meso compound. Chemical shifts for the diastereomeric amines show that 15N shifts move downfield on protonation along with methyl and methylene carbons, while the methine carbon resonances move upfield.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 33
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 15 (1984), S. 347-349 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Brillouin spectra of lithium potassium sulfate have been obtained in its hexagonal phase from room temperature to the orthorhombic phase transition temperature at 435°C. The ν11 longitudinal sound velocity corresponding to the C11 elastic coefficient undergoes a smooth decrease with increasing temperature; the maximum decrease is 6.0% at T0=435°C and the temperature dependence of ν11 satisfies an expression of form \documentclass{article}\pagestyle{empty}\begin{document}$$ \frac{{V_{11} (T)}}{{V_{11} (293\,{\rm K})}} = A - BT - \frac{C}{{T_c - T}} $$\end{document} with B=(1.13±0.04) × 10-4K-1, C = (0.9±0.1) K and Tc = (467±6)°C=(740±6)K.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 34
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 2 (1983), S. 1-45 
    ISSN: 0277-7037
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 35
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 171-175 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The fragmentation pathways for the ions generated by electron impact from nonan-4-one have been studied using low energy collision induced dissociation in a triple quadrupole mass spectrometer. Over 400 fragmentation pathways have been identified. These results are compared with data from earlier ion kinetic energy spectrometry studies of nonan-4-one which employed metastable decompositions.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 36
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 16-20 
    ISSN: 0935-6304
    Schlagwort(e): LC/MS interface ; Nebulizing interface ; Micro-LC ; CI-MS ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: An improved vacuum nebulizing interface with a very short counter nozzle was developed for direct coupling of a micro-LC and a quadrupole MS with CI-chamber. With the LC-MS system using the nebulizing interface, it became possible to take mass fragmentograms for various less volatile compounds such as glutamic acid, steroids, aromatic amines and chlorine-containing insecticides.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 37
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: An accurate and time-saving method for the determination of norepinephrine in human plasma is described. The whole device focused on an improvement in the pretreatment. One ml of human plasma was applied to a boric acid gel column without deproteinization and pH adjustment, and norepinephrine was eluted with 2 ml of a 1.3 M acetic acid in methanol solution. The pentafluoropropionic derivative of norepinephrine was analysed by gas chromatography mass spectrometry using deuterated norepinephrine as an internal standard. The level of plasma norepinephrine in healthy subjects at recumbency was 297 ± 95 pg ml-1 (mean ± SD). The lower limit of sensitivity was 25 pg ml-1 of norepinephrine in plasma.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 38
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, HPLC ; Post-column detection ; Amino acids ; NBD-CI ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 39
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 11 (1984), S. 594-600 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A series of metabolites of trinitrotoluene (TNT) have been synthesized and analysed by electron impact (EI) and chemical ionization (CI) mass spectrometry. Identification characteristics of these metabolites by their mass spectra have been determined. Differentiation of isomers is made possible by EI ions which are characteristic of the position of the methyl group with regard to the nitro groups.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 40
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 47-51 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Pressure dependence of several reversed phase liquid chromatographic solvents, including methanol, acetonitrile and mixtures of methanol: water and acetonitrile: water has been investigated. Typical ions, [MH]+, [2M+H]+ and [3M+H]+, were recorded as function of source pressure and as a function of the amount of water in the mixture. Ion formation processes in methanol: water and acetonitrile: water are discussed. The influence of liquid chromatographic mass spectrometric solvent pressure on the mass spectra of samples has been demonstrated on an amino acid sample.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
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  • 41
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1980), S. 637-639 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Mass spectra of explosives, including TNT, tetryl, nitroglycerin, PETN and RDX have been recorded by direct exposure chemical ionization with isobutane as reagent at source temperatures of 50-100°C. The mass spectra contain major [MH]+ ions, adduct ions and some fragment ions. The configuration of the relative abundances of these ions has been found to be a function of temperature and source pressure. Maximum [MH]+ ion abundance has been obtained at source pressures much lower than normal chemical ionization pressures.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 42
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 264-266 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A reduction process was found to occur in the ion source when observing the chemical ionization mass spectra of a series of trinitroaromatic compounds, using water as reagent. The [MH-30]+ ions in the CI mass spectra were due mainly to the reduction of the compounds to their corresponding amines. This was proved by using D2O as reagent: the [MH-30]+ ions were shifted to [MD-28]+ ions. The trinitroaromatic compounds investigated included 1,3,5-trinitrobenzene, 2,4,6-trinitrotoluene, 2,4,6-trinitro-m-cresol, 2,4,6-trinitroaniline (picramide) and 2,4,6-trinitrophenol (picric acid).
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
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  • 43
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 1 (1982), S. 257-307 
    ISSN: 0277-7037
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Zusätzliches Material: 20 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 44
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 321-326 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A collisional induced dissociation study of 1,3,5-trinitro-1,3,5 triazacyclohexane (RDX) and 1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane (HMX) was carried out using mass analyzed kinetic energy spectrometry. High resolution mass spectra and mass analyzed ion kinetic energy/collisional induced dissociation spectra of RDX and HMX were recorded in the electron impact, chemical ionization and negative ion chemical ionization modes. Fragmentation pathways of the compounds investigated were determined in all three modes of ionization. It was found that a major part of the fragment ions in RDX and HMX originate from formation of the aduct ions [M+NO]+ and [M+NO2]+ in electron impact and chemical ionization, and from [M+NO]- and [M+NO2]- in negative chemical ionization, followed by dissociation.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 45
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 8 (1981), S. 503-505 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Three physiologically important disaturated lecithins have been analyzed quantitatively as the acetate derivatives using a solids inlet probe and ammonia chemical ionization. Concentration independent response factors have been determined over a tenfold range that brackets human plasma levels. The results obtained serve as an independent corroboration of gas chromatographic analyses.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 46
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 9 (1982), S. 286-292 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Mass spectra of a series of alkyl, alkyl/aryl and biologically important quaternary ammonium and phosphonium compounds have been obtained by a direct thermal process. No means of ionization other than the heating of a salt coated filament is used. The spectra consist primarily of even electron ions for which decomposition schemes involving four-center reactions are proposed. These spectra are similar to those obtained in fission fragment induced desorption, laser induced desorption and field desorption/collisional activation, but they are produced by a far simpler means.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 47
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 15 (1984), S. 55-59 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Infrared spectra (4000-400 cm-1) of pentachlorocyclopropane have been recorded for all three of its physical states. A liquid-phase Raman spectrum of this molecule has also been observed. Based on the Raman depolarization data, gas-phase infrared band contours and expected group frequency correlations, it has been possible to propose an assignment for 20 of the 21 normal vibrations of pentachlorocyclopropane. This assignment agrees well with those proposed for hexachlorocyclopropane, the three isomeric tetrachlorocyclopropanes, 1,1-dichlorocyclopropane and chlorocyclopropane. Further, the vibrational assignment for pentachlorocyclopropane has identified characteristic vibrational frequencies for the three CH(X) modes: CH stretch, 3040 cm-1; in-plane CH bend, 1296 cm-1; and out-of-plane CH bend, 1088 cm-1.
    Zusätzliches Material: 3 Ill.
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  • 48
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Proton-coupled nitrogen-15 NMR spectra of urea, N-methylurea, N,-N′-dimethylurea, N-methyl-N′-benzylurea and N-phenylurea have been obtained at natural abundance level in neutral, basic and acidic solutions at 25°C. Base-catalyzed N—H proton exchange of the —NH2 group of N-methylurea in water was found to be 1.5 times faster than that for the -NH- group, while the corresponding acid-catalyzed exchange is 7.5 times faster. Comparison of urea and N,-N′-dimethylurea in water shows urea to be 10 times faster in base but 2 times slower in acid. The ratio of the base-catalyzed N—H proton exchanges of the two -NH- groups of N-methyl-N′-benzylurea in dimethyl sulfoxide is close to unity, whereas the CH3NH- group exchanges 4 times faster in acid. Similarly, the C6H5NH- group of N-methyl-N′-phenylurea exchanges 50 times faster than the CH3NH- group in base and about 3 orders of magnitude slower in acid. The results are rationalized by consideration of steric and electronic effects.
    Zusätzliches Material: 2 Ill.
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  • 49
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The proton-coupled nitrogen-15 NMR spectra of hydrazinecarbothioamide and 4-methylhydrazinecarbothioamide have been taken at the natural-abundance level in neutral, basic and acidic solutions at 25°C. The N—H proton-exchange reactions of the hydrazino-NH2 groups in both compounds were found to be very rapid in the presence of acid, but quite slow in the presence of base. The hydrazino-NH protons of hydrazinecarbothioamide exhange six times and 200 times faster than the amide protons in the presence of either base or acid, respectively. Similarly, acid- and base-catalyzed N—H proton exchanges of the hydrazino-NH group of 4-methylhydrazinecarbothioamide were found to be two to three orders of magnitude faster than those of N-methylamido protons. These results can be rationalized by consideration of the effect of the lone pair on the hydrazino—NH2 group on the reactivity of the adjacent —NH— group.
    Zusätzliches Material: 1 Ill.
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  • 50
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 14 (1980), S. 511-514 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 251 MHz 1H and the natural abundance 63.1 MHz 13C NMR spectra of 1,3-dioxepane (1) and 4,4,7,7-tetramethyl-1,3-dioxepane (2) have been investigated over the temperature range of 5 to -180 °C. While the spectra of 1 show no dynamic NMR effect, compound 2 exists in solution as a 1:1 mixture of a symmetrical (C2) twist-chair and its mirror image conformation. The free energy barrier for the conformational racemization of 2 is 43 kJ mol-1 (10.3 kcal mol-1). Interconversion paths between various conformations of 2 are discussed. Compound 1 is suggested to have a symmetrical (C2) twist-chair conformation which is rapidly pseudorotating via a chair conformation to achieve a time averaged symmetry of C2v, even at -180 °C.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 51
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 15N NMR spectra of several substances with nitrogen - nitrogen bonds have been obtained at the natural-abundance level by high-resolution NMR spectroscopy. Azo (—N=N—) nitrogens are 300-500 ppm deshielded compared with hydrazo (—NH—NH—) nitrogens. The sensitivity of the 15N shifts in these types of substances to substituent changes are reported, along with 15N-1H spin-spin couplings for some hydrazo compounds. Hydrogen-bonding effects arising from solvent changes on the 15N shifts of azoxybenzene are different for its two kinds of nitrogen. The 15N NMR spectrum of N,N'-dinitrosopiperazine in dimethyl sulfoxide at room temperature is consistent with the presence of two different conformations about the N—NO bonds.
    Zusätzliches Material: 1 Ill.
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  • 52
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 19 (1984), S. 250-252 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 53
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 14 (1980), S. 153-154 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The Ketonic 13C NMR signals of a series of 6-hydroxy-5-oxobicyclo[2.2.2]oct-7-ene-2-carboxylic acid lactones and of haplophytine and related N-substituted 3-piperidinones occur at exceptionally high field; the structural factors which are responsible have been elucidated by comparisons with related compounds.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 54
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 20 (1982), S. 199-200 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Earlier assignments of 13C NMR signals to C-6 and C-7 in 5,5-dimethyl-2-norbornanone (1) based on lanthanide-induced shifts are interchanged on the basis of studies of deuterium-labeled derivatives of 1. The revised assignments are in accord with predictions based on substituent parameters.
    Zusätzliches Material: 1 Tab.
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  • 55
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 10 (1983), S. 567-571 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In chemical ionization mass spectrometry, the use of a noble reagent gas mixed with a proton transfer reagent gas is known to produce mass spectra which contain both protonated molecules and fragment ions. We have used a mixture of isobutane and argon to improve the mass spectra of peptides which have been derivatized to O-TMS-polyamino alcohols. The molecular weight is deduced from a prominent [M+H]+ ion; the sequence of amino acids is deduced from the usual A- and Z-series fragment ions. This technique enhances the sequence ions for lysine and glycine-containing peptides, and retains the ability to distinguish C-terminal leucine and isoleucine.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 56
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    X-Ray Spectrometry 10 (1981), S. 85-90 
    ISSN: 0049-8246
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Physik
    Notizen: A systematic investigation of the chemical effects on the calcium X-ray K emission spectra from 32 chemical compounds was carried out using a two-crystal X-ray spectrometer. The observed chemical shifts of the Ca Kα1,2, Kα3,4, Kβ1,3 and Kβ5 lines relative to the respective lines from CaF2 varied in the range +0.06 to +0.30, +0.09 to +0.32, -0.06 and +1.1 to +3.2eV, respectively. A certain dependence on the nature of surrounding groups was found in these shifts. The profile changes in the Ca Kβ5 and Kβ5′ bands from all compounds were discussed by subdividing them roughly into three types, depending upon their characteristic features.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 57
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: We examine the difference between a linear and a non-linear model for the calculation of analyte concentration by interpolation between standards in isotope dilution/mass spectrometry. Equations are developed for calculating this difference for various increments of the bracketing intensity ratios and for various compositions of the sample; graphs are also presented to depict this difference for these various conditions. As an illustration, the result for a series of measurements on urea are presented and discussed.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
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  • 58
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 589-590 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, (HP)LC, CLC ; Capillary, fused silica with chemically bonded phases ; 30 μm i.d., split sampling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 59
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 83-85 
    ISSN: 0935-6304
    Schlagwort(e): HPLC ; Nanoliter volume detector ; 1.5 × 10-5 AU noise (0.1 μl 0.1% benzene in methanol) ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 60
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 348-358 
    ISSN: 0935-6304
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 61
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 6 (1983), S. 448-450 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Capillary column ; Solute focussing ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 62
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 14 (1980), S. 76-77 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Coupling constants between 11B and 13C, 13C and 1H, and 11B and 1H were obtained for LiB(CH3)4 in 1,2-dimethoxyethane, in which the anion B(CH3)4- is belived to exist as a separate ion pair. The correlations of the coupling constants with the effective nuclear charge of boron, and with the s character of the B—C bond, are discussed.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 63
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 12 (1982), S. 157-161 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Resonance Raman spectra of three types of reaction intermediates, blue, green and yellow species, formed from 1,1-diphenylethylene adsorbed on porous Vycor glass were measured by means of an improved experimental technique and with suitable excitations. The blue species, which is the least stable intermediate, is found to be a cation radical, , and the characteristic Raman bands of and 2 stretching vibrations are clearly observed. For the green and yellow species more detailed spectra were obtained than in previous experiments. The coverages of the three intermediates are θ≈10-3 for each, being in agreement with the values expected from the numbers of Lewis and Brönsted acid sites on porous Vycor glass. Resonance Raman spectrum of the blue species on silica-alumina, a catalyst, was also obtained by using the rotating sample technique.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 64
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 21 (1983), S. 570-572 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 13C NMR chemical shifts of m- and p-substituted benzyl N,N-dimethylcarbamates were measured in CDCl3. The meta and para 13C substituent chemical shifts were analysed by means of dual substituent parameter (DSP) equations. Good correlations were obtained, especially for the para-carbon substituent chemical shifts. The computed transmission coefficients, ρI and ρR, are consistent with the general features of the fitting parameters. It has been shown that no significant electron demand is imposed by the —CH2OCON(CH3)2 substituent.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 65
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 22 (1984), S. 439-445 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: 13C NMR spectra of p- and m-substituted phenyl N-methylcarbamates, phenyl N,N-dimethylcarbamates and p- and m-substituted phenyl propionates were recorded, and their para 13C SCS (substituent chemical shifts) were analysed by DSP (dual substituent parameters) and DSP-NLR (non-linear resonance) equations. It was found that the fixed substituent Y, —OCONHCH3, —OCON(CH3)2 and —OCOC2H5, were all mild in the sense that DSP analysis gave a good correlation, leaving little room for improvement by the DSP-NLR treatment. Further, the three series of compounds gave similar ρI and ρR values (para derivatives, 3.2-3.3 and 17.7-18.0; meta derivatives, 5.1-5.2 and 21.8-22.0). Examination of the corresponding analyses of similar compounds indicated that the ρI and ρR values and, hence, their ratio ρR/ρR = λ, depended primarily on the nature of the atom through which the fixed substituent Y (e.g. α-C, α-N and α-O) was bonded to the aromatic ring when the Y substituents are mild. The extent of this tendency for compounds with active fixed substituents is also discussed.
    Zusätzliches Material: 7 Tab.
    Materialart: Digitale Medien
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  • 66
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1980), S. 1-3 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The electron impact induced fragmentation of 1-benzoylbenzotriazole has been studied by 13C labelling experiments. It has been found that the loss of CO from the [M — N2]+· ions proceeds by two routes; about 78% of the ions decompose via the molecular ions of the corresponding thermal fragmentation product, 2-phenylbenzoxazole, and 22% via those of the corresponding photochemical fragmentation product, 6-phenanthridone.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 67
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 9 (1980), S. 401-402 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: By using optical fibres the sample surfaces can be illuminated widely and uniformly. This technique is useful for the Raman measurements of a small amount of surface species and also unstable surface species.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 68
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 14 (1983), S. 353-357 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The Raman spectrum of 1,2-diiodotetrafluorobenzene was recorded in the region 50-2000 cm-1 on a Jarrell-Ash Model 25-300 double monochromator spectrometer using 5145 Å radiation from an argon-ion laser. The depolarization ratios of the Raman lines were measured in CS2 and CHCl3 solutions. The infrared spectrum was recorded in CS2 and CHCl3 solutions in the region 180-200 cm-1 on a Perkin-Elmer 180 spectrometer using a CsI cell. The fundamental vibrations were assigned on the basis of the frequencies and relative intensities of the bands observed in the Raman and infrared spectra and the depolarization ratios of the Raman lines. A normal coordinate analysis was also performed to check the vibrational assignments.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 69
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 248-252 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Column loadability - overload phenomenon ; Non-classical approach to theory of loadability ; Effect on retention times, peak shape ; Effect of column length ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The usual concepts of the dynamics of an overloaded solute band fail to explain several phenomena such as the typical “leading-tail” shape and retention deviations exhibited by overloaded peaks, and why these defects are more commonly observed in short columns. These and other related deviations from theory can be rationalized by a non-classical approach to the overloading phenomenon.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 70
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 4 (1981), S. 569-576 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, HPLC ; Small bore columns ; Systematic performance studies with tabulated results ; Seven compounds separated in less than 10 s ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Using a specially designed column system, we have systematically investigated the effect of mobile phase velocity on column efficiency. The performance of small bore columns operated at different linear velocities of mobile phase was examined for three different types of injection system. Using the value of H∞/u or n∞/trº as a criterion of a high speed separation, we calculated values of n/trº for different solutes according to the equation \documentclass{article}\pagestyle{empty}\begin{document}$ {{\rm n}\mathord{\left/ {\vphantom {{\rm n} {{\rm t}_{\rm r}^ \circ }}}\right. \kern-\nulldelimiterspace} {{\rm t}_{\rm r}^ \circ }} = {{{\rm n}^\infty } \mathord{\left/ {\vphantom {{{\rm n}^\infty } {{\rm t}_{\rm r}^ \circ }}} \right. \kern-\nulldelimiterspace} {{\rm t}_{\rm r}^ \circ }}\left({\frac{{1 + {\rm k'}}}{{{\rm k' + }\beta }}} \right)^2 $\end{document}; the results obtained are in agreement with the experimentally determined values. These systematic investigations culminated in the separation of seven compounds in less than 10 s; the respective chromatogram is shown.
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 71
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 22 (1984), S. 272-273 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 13C NMR spectra of nine isomeric E-hydroxyazastilbenes (E-hydroxystyrylpyridines) have been fully assigned. The Ai and AiK empirical parameters of o-(m or p-)hydroxystyryl and 2-(3- or 4-)vinylpyridyl groups for the prediction, of chemical shifts of substituted styrylpyridines were calculated.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 72
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1980), S. 427-430 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass spectral fragmentation of the six 2′-, 3′- and 4′ -hydroxy substituted 4- and 2-azastilbenes is discussed and fragmentation pathways, elucidation of which were assisted by accurate mass measurements and metastable transitions, are proposed. It has been found that the position of the hydroxystyryl group in the pyridine ring may be deduced on the basis of mass spectral fragmentation patterns.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 73
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 17 (1982), S. 403-408 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass spectral fragmentation of twelve new 4-alkoxycarbonylakyithio substituted derivatives of uracils is discussed and fragmentation pathways. Elucidation of which assisted by accurate mass measurements and metastable transitions, are proposed. The comparison between the mass fragmentation of 2- and 4-alkoxycarbonylakylthiouracils have shown that the position of uracil ring thiation may be deduced on the basis of mass special fragmentation patterns.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 74
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 221-226 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass spectral fragmentation of twelve new 2-alkoxycarbonylalkylthio substituted derivatives of uracils is discussed and fragmentation pathways, elucidation of which were assisted by accurate mass measurements and metastable transitions are proposed. It has been found that the basic mass spectral fragmentation of these compounds is due to cleavage of S—Csp3, O—Csp2 and Csp2—Csp3 bonds of the alkoxycarbonylalkylthio group.
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 75
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 16 (1981), S. 153-158 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The mass fragmentation of twelve new 2- and 4-benzylthio substituted derivatives of uracils is discussed and fragmentation pathways, elucidation of which was assisted by accurate mass measurements and metastable transitions, are proposed. It has been found that the position of uracil ring thiation may be deduced on the basis of mass spectral fragmentation patterns.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
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  • 76
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 14 (1983), S. 87-92 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Fourier transform infrared spectra of bromocyclopropane at a resolution of 0.5 cm-1 have been recorded as well as liquid phase infrared spectra of this molecule from 4000-400 cm-1. For the first time, gas phase Raman spectra and solid phase infrared spectra of bromocyclopropane have been obtained. By combining all of the spectral data available it has been possible to assign all 21 normal modes of vibration of bromocyclopropane (as well as several overtones and combination bands) with a high degree of confidence. This proposed assignment is in excellent agreement with assignments for similar molecules and with anticipated cyclopropyl group frequencies.
    Zusätzliches Material: 5 Ill.
    Materialart: Digitale Medien
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  • 77
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 9 (1980), S. 334-338 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: For cyclopropyl isothiocyanate, the infrared (4000-200 cm-1) spectra in all three phases and the Raman spectra of the liquid and solid phases have been recorded. From Raman depolarization data and infrared gas phase band contours it has been concluded that cyclopropyl isothiocyanate exists in the cis conformation. No evidence for the existence of other conformations was found in the spectra. An assignment for 24 of the 27 fundamental vibrational modes has been proposed and this assignment has been shown to be in excellent agreement with vibrational assignments for other monosubstituted cyclopropanes and a number of isothiocyanate compounds.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 78
    Digitale Medien
    Digitale Medien
    Chichester [u.a.] : Wiley-Blackwell
    Journal of Raman Spectroscopy 12 (1982), S. 95-101 
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: Infrared and Raman spectra of (bromomethyl)cyclopropane and epibromohydrin have been recorded. Reversible spectral changes which accompany changes in temperature indicate the existence of an equilibrium mixture of gauche and cis conformers for (bromomethyl)cyclopropane. The gauche form is more stable, and from the variable temperature studies an enthalpy difference of 2.0±0.2 kcal mol-1 has been obtained for the liquid phase. For epibromohydrin, two non-equivalent gauche conformers have been identified, and the gauche-1 form is more stable than the gauche-2 by 0.80±0.20 kcal mol-1 in the liquid phase. Additionally there is evidence for a third conformer, presumably the cis form, but characterization of this conformer has been limited by the complexity of the spectra associated with the gauche-1 and gauche-2 forms. Consequently, only a lower limit can be given for the ΔH separating the cis and gauche-1 conformers. The results are consistent with previous observations for similar molecules.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 79
    ISSN: 0377-0486
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Notizen: The infrared spectra (4000-400 cm-1) of gaseous, liquid and solid (cyanomethyl) cyclopropane have been recorded for the first time. Additionally, the Raman spectra (3500-50 cm-1) of condensed phases of this substance have also been obtained. ‘Extra’ Q branches have been observed in the gas-phase infrared spectrum, and six liquid-phase Raman doublets (two of which are also seen in the infrared spectrum of the liquid) have also been observed, wherein one member of each doublet vanishes once the polycrystalline solid state spectrum is obtained. These data have been interpreted in terms of a two conformer (gauche/cis) fluid-phase equilibrium for (cyanomethyl)cyclopropane, with only the gauche conformer remaining in the solid phase. The temperature behavior of the 774/756 and 835/855 cm-1 liquid-phase Raman doublets yields an enthalpy difference between conformers of 0.72±0.10 kcal mol-1, with the gauche conformer the more stable. This ΔH value implies a room-temperature conformational equilibrium for (cyanomethyl)cyclopropane composed of 87% gauche and 13% cis rotamers in the liquid phase. In addition, a vibrational assignment for the 33 normal modes of (cyanomethyl)cyclopropane has been proposed, and it is in excellent agreement with the previously published vibrational assignments for three (halomethyl)cyclopropanes.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 80
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 15 (1980), S. 38-40 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The compounds Pt3(CO)3[P(C6H5)3]4 molecular weight 1717, Pt4(CO)5[P(C6H5)3]4 molecular weight 1968 and Pt5(CO)6[P(C2H5)3]4 molecular weight 1615 are thermally labile and are slowly solvolysed by tetrahydrofuran and acetone. They cannot be analysed by means of electron impact. Field desorption, however, shows the molecular ion and [M—xCO]+· peaks.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
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  • 81
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Seven desoxinojirimycin and three folic acid derivatives were investigated using the soft ionization techniques of desorption chemical ionization (DCI), laser desorption (LAMMA), field desorption (FD), secondary ion mass spectrometry (SIMS) and fast atom bombardment (FAB). The mass spectra were compared with electron impact (EI) spectra and interpreted in terms of their suitability for analytical purposes.
    Zusätzliches Material: 10 Ill.
    Materialart: Digitale Medien
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  • 82
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, HPLC ; General methods of nucleotide HPLC ; Molecular and ionic basis of separation ; Two-dimensional separation ; Stationary phase; selectivity to nucleotide size and composition, selectivity control ; Mobile phase (solvent, salt, pH), influence on retention and selectivity ; Guard-column functions ; Column loadability and packing, consolidation of bed particles ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In order to develop efficient separation methods for nucleotides according to their size and heterocyclic composition, the application of ion-exchange, reverse-phase, and normal-phase adsorption HPLC has been studied. The comparative investigation of retention power and selectivity of various packings (non-polar bonded-phase and amino silicas) in relation to nucleotide length and composition yields data which enable suitable packings to be selected and a method of preparing the new packing for a particular separation problem to be formulated. Thus a new anion exchanger with high selectivity and dynamic mass transfer has been prepared for fractionation of large oligonucleotides. The effect of the eluent pH and composition (organic modifier, salt) on retention, selectivity, and resolution in ion-exchange and reverse-phase HPLC has been studied. The optimum separation conditions comprise elution with oppositely directed gradients of the salt and the modifier, use of a precolumn packing that provides the best protection for the main column without loss of its efficiency, and the optimum gradient program for the desired retention of the component of interest. The relation between loading and sample concentration has been studied and the system for gradient elution improved. Our work shows that two-dimensional separation is the most reliable and informative method for preparation of homogeneous oligonucleotides. The hydrophobic-pair ion-exchange mechanism is proposed for ion-pair chromatography. Protected and partially deblocked oligonucleotides, chemically synthesized for genetic engineering studies, have been separated with high selectivity by adsorption (normal-phase) HPLC which is efficient for gradient elution with isohydric eluents. The analysis of a monomeric composition of nano-(pico-) molar amounts of oligonucleotides has been developed; the procedure involves microcolumn digestion of the oligonucleotides with immobilized enzymes followed by microcolumn separation of the nucleoside-mononucleotide mixture. Also, a new slurry method for packing stable HPLC columns with a tightly consolidated, nonshrinkable bed of particles has been developed.
    Zusätzliches Material: 31 Ill.
    Materialart: Digitale Medien
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  • 83
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method for the determination of underivatized chlorophenols in human urine samples by combined high performance liquid chromatography mass spectrometry is described. Results obtained on individual samples are reported and compared with data obtained by alternative chromatographic methods.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 84
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 83-88 
    ISSN: 0935-6304
    Schlagwort(e): High resolution gas chromatography ; Quantitative analysis ; Polycyclic aromatic hydrocarbons ; Nitrogen-containing polycyclic aromatic compounds ; SRC-II heavy distillate ; Shale oil process water ; Dual column analysis ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Complex organic mixtures, such as coal liquefaction and oil shale products and by-products, are comprised of hundreds or thousands of individual components. State-of-the-art high resolution gas chromatography does not always provide sufficient resolution to allow accurate quantitation or identification of many compounds of interest. The concept of dual capillary column chromatography combines the different resolving characteristics of two capillary columns coated with different stationary phases into a single chromatographic run. In this approach, both columns are connected to the same injection port. Analysis of complex mixtures in this fashion can confirm the identification and quantitation of components on two columns of different polarity with little increased analysis time, can provide a means of obtaining quantitative data for individual components which are known to coelute on any one column, and can alert one to unknown coelution problems that would be undetected by gas chromatographic analysis on a single capillary column.Simultaneous dual column analysis was applied to three samples, the neutral polycyclic aromatic hydrocarbon (PAH) fraction of a Solvent Refined Coal-II (SRC-II) heavy distillate, the nitrogen-containing polycyclic aromatic compound (N-PAC) fraction of an SRC-II heavy distillate, and the basic fraction from a shale oil process water. Fused silica capillary columns coated with SE-54 and Durawax 3 were used for the analyses of the heavy distillate, while SE-54 an Carbowax 20M capillary columns were used for the analysis of the process water.
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 85
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 3 (1980), S. 352-354 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Short capillary columns ; Rapid analysis ; Polycyclic aromatic hydrocarbons ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 86
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 5 (1982), S. 413-416 
    ISSN: 0935-6304
    Schlagwort(e): Capillary gas chromatography ; Stationary phase stability ; Stationary phase viscosity ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: With recent advances in column technology it is now possible to prepare highly efficient, very inert, and thermally stable capillary columns coated with nonpolar polysiloxane stationary phases. Unfortunately, the same degree of success has not been achieved for some of the more polar polysiloxane phases. A parameter that has been studied little in the past in relation to stationary phase film stability is the viscosity of the stationary phase. In this paper the efficiency and stability of coated columns are correlated to the viscosity of the phase. Due to their structure, the viscosity of the phenyl-containing polysiloxanes change rapidly with temperature and hence, thin-film coatings are not stable at elevated temperatures. By using high viscosity phenyl-containing methylphenylpolysiloxanes which were recently synthesized, efficient and stable columns have been prepared.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 87
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 329-332 
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Fused silica capillary columns ; Deactivation ; Polymethylhydrosiloxanes ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 88
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 10 (1983), S. 143-154 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The modification of alcoholic and phenolic compounds as their tert-butyldimethylsilyl ether derivatives has found wide use in the separation of complex mixtures by gas chromatography and in their quantification by gas chromatography mass spectrometry with selected ion monitoring. In comparison, the formation and use of the tert-butyldimethylsilyl ester derivatives has received little attention. This paper examines some of the factors involved in the esterification of fatty acids using a number of tert-butyldimethylsilyl reagents, delineating optimum conditions for derivative formation. In addition, using hydroxy fatty acids, differences in the selectivity of silylation between these tert-butyldimethylsilyl reagents and their trimethylsilyl analogues are demonstrated, which are manifested in the discrimination between silyl ester and silyl ether formation. The application and limitation of these techniques is discussed with reference to the quantification, by gas chromatography mass spectrometry selected ion monitoring of unsaturated fatty acids and hydroxy fatty acids as their tert-butyldimethylsilyl derivatives. The measurement of arachidonic acid obtained from human skin, where sample size is often limited, is illustrated using a stable isotope dilution assay. These results are compared to those obtained using the methyl ester.
    Zusätzliches Material: 9 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 89
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 466-472 
    ISSN: 0935-6304
    Schlagwort(e): Liquid chromatography, HPLC ; Normal phase ; Serum ; Retinol ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method for the quantitation of retinol in serum by normal phase high performance liquid chromatography is described. The mobile phase consists of a hexane/diethylether/methanol mixture with spectrophotometric detection. The sample preparation is similar to that described by other authors and involves protein precipitation followed by extraction and direct injection onto the chromatograph. Adequate sensitivity is achieved using 200 μl samples. The internal standard chosen is α-naphthol because of its spectral similarities to retinol and its greater stability than the commonly used retinyl esters. The method has been successfully applied to the clinical evaluation of a number of malabsorption syndromes for which it is preferred to the measurement of total carotenoids.
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 90
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 9 (1982), S. 302-306 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A 4 min gas chromatographic run on 3% SP-2250 allows for the simultaneous gas chromatographic selected ion monitoring assay of dopamine, homovanillic acid, dihydroxyphenylacetic acid and 3-methoxytyramine after a one-step derivatization with pentafluoropropionic anhydride and hexafluoroisopropanol. A comparison of electron impact, positive chemical ionization and negative chemical ionization conditions indicated dramatic increases in sensitivity with negative chemical ionization. This assay has wide applications for the measurement of monoamines and their metabolites in biological samples.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 91
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1980), S. 11-12 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Field desorption mass spectra of a homologous series of synthetic phosphatidylsulfocholines (dimyristoyl-, dipalmitoyl-, distearoyl- and dioleoyl-) are reported. Prominent ions related to the intact molecule ([M + 1]+, [M + 15]+, etc.) were detected, as well as characteristic fragmentation ions, and will be useful for the identification and analysis of these compounds isolated from natural sources.
    Zusätzliches Material: 1 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 92
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1980), S. 399-400 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Cationization of polyethyleneglycols with [Ca]2+ ions prior to field desorption mass spectrometry gives abundant [M + Ca]2+ ions in approximate proportion to the species present. Similar treatment with [Ba]2+ converts sucrose, raffinose and stachyose into doubly charged complex ions, including [M + Ba]2+. Such doubly charged ions extend the effective mass range of conventional mass spectrometers without the inherent loss of sensitivity associated with reduced accelerating voltage.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 93
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 18 (1983), S. 42-45 
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Intramolecular methyl transfer has been observed previously in pyrolysis electron impact mass spectra of complex ammonioalkanecarboxylates. We present here field desorption mass spectra results of more simple N,N,N-trimethylammoniocarboxylate hydrochloride salts and their N,N,N-perdeuterotrimethylammonium analogs in which we observe methyl transfer. We demonstrate that mechanisms for this and other fragmentation and rearrangement processes are dependent on anode heating current. Addition of the protonating agent p-toluenesulfonic acid suppresses most ions except the protonated molecular ion.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 94
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 9 (1982), S. 72-73 
    ISSN: 0306-042X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Field desorption (FD) mass spectra of alkali metal salts of organic acids are characterized by fluctuating ion current, high anode temperature, high abundance of metal ions and low abundance of structurally significant organic ions. As part of a continuing study of matrix effects on the FD process, we have now found that addition of pentaerythritol or cis-inositol results in a smoother desorption and a marked enhancement of intensity in a variety of such spectra. Results are presented for 12-hydroxystearic acid sodium salt; anthraquinone-2-sulfonic acid sodium salt.
    Zusätzliches Material: 2 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 95
    Digitale Medien
    Digitale Medien
    New York, NY [u.a.] : Wiley-Blackwell
    Mass Spectrometry Reviews 1 (1982), S. 63-102 
    ISSN: 0277-7037
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie , Physik
    Zusätzliches Material: 13 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 96
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Organic Magnetic Resonance 13 (1980), S. 384-386 
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 1H NMR spectra of phthalide in Merck Nematic Phase IV and in N-(p-ethoxybenzylidene)-p-n-butylaniline (EBBA) and of 2-coumaranone in Merck Nematic Phase IV were analyzed. Structural parameters were obtained. The planarity of the 5-membered ring and the molecular orientations were discussed.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 97
    Digitale Medien
    Digitale Medien
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 7 (1984), S. 473-476 
    ISSN: 0935-6304
    Schlagwort(e): Thin-layer chromatography, HPTLC ; Fluorimetric assay ; Mitochondria ; Phospholipids ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A method is described for quantitative determination of phospholipids of mitochondria following one-dimensional thin-layer chromatography without previous elution. Using high performance thin-layer chromatography (HPTLC) and an in situ fluorescence technique, the time needed for quantitative determination is relatively short. As the method is rather sensitive, small amounts of the extracts can be applied (about 200 ng of total phospholipids per spot). The reproducibility for the phospholipid fractions determined was in the range of 8-17%. The procedure was tested with lipid extracts of rat liver mitochondria. The method allows the determination of cardiolipin, phosphatidyl ethanolamine, phosphatidyl inositol, phosphatidyl choline, and sphingomyelin.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 98
    ISSN: 0030-493X
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The chemical ionization induced fragmentation behaviour of an open chain model compound, 5,7-undecanediol (meso and d,l stereoisomers), is studied and compared with that of previously studied alicyclic models, e.g. cyclohexanediols (cis and trans isomers). In close analogy to the latter, the major fragmentation processes are the one- and twofold loss of H2O from the protonated molecules [MH]+. As borne out by appropriately deuterium labelled analogues, the first loss of H2O is invariably a ‘clean’ heterolysis. The second loss is considerably more complex in that 1,3- and 1,4-elimination processes occur concurrently. While the 1,4-mode may be a direct elimination process in both types of compounds, the 1,3-mode is rearrangement induced in both. Whereas skeletal rearrangement (ring contraction) precedes this 1,3-elimination in the alicyclic models, hydrogen rearrangement (1,2-hydride shift) precedes it in the open chain model. No pronounced stereochemical effect is observed on the mechanistic course of the elimination processes, but is observed in their relative ease. The trimethylsilyl ethers of the stereoisomers of 5,7-undecanediol are also studied for analogous reactions, and are discussed in this context.
    Zusätzliches Material: 5 Tab.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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  • 99
    ISSN: 0030-4921
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The 29Si NMR subtituent chemical shifts of 14 meta-and para-substituted derivatives of phenyltrimethyl-and phenoxytrimethyl-silanes have been interpreted in a uniform manner. They are shown to depend not only on the local but also on the non-local parts of the charge distribution around the resonating nucleus. While the local part is taken into account by the paramagnetic screening constant, the influence of the non-local part can be described by the induced internal electric field and additional higher order terms.
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
    BibTip Andere fanden auch interessant ...
  • 100
    Digitale Medien
    Digitale Medien
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 7 (1980), S. 168-171 
    ISSN: 1052-9306
    Schlagwort(e): Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The measurement of plasma free fatty acid turnover and oxidation by means of the isotopic dilution technique using a radiolabeled free fatty acid has proven useful for the in vivo study of fat metabolism in animals. However, because of the ethical considerations regarding the administration of radioisotopes to humans, there is a lack of adequate information regarding the in vivo regulation of free fatty turnover and oxidation in humans, particularly children. Consequently, we have developed a technique using the stable, nonradioactive [1-13C]palmitic acid molecule as free fatty acid tracer to measure plasma free fatty acid metabolism in vivo. We have analysed the isotopic enrichment of plasma palmitate by selected ion monitoring on a gas chromatograph mass spectrometer and we have used an isotope ratio mass spectrometer to determine the much lower isotopic enrichment of the expired CO2. We have found this technique to be safe to administer, to have a high degree of analytical reproducibility, and to yield values in dogs comparable with those obtained using [1-14C]palmitic acid as the tracer.
    Zusätzliches Material: 2 Ill.
    Materialart: Digitale Medien
    Standort Signatur Erwartet Verfügbarkeit
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