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  • Analytical Chemistry and Spectroscopy  (1,210)
  • Inorganic Chemistry
  • 1990-1994  (1,501)
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Year
  • 1
    ISSN: 0749-1581
    Keywords: Penta-1,3-dien-5-ols ; 1H{1H} NOE ; 2D J-resolved 13C NMR ; 1H, 1H allylic coupling ; Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Established NMR criteria from 1H, 13C and 2D J-resolved 13C NMR spectra, and also 1H{1H} NOE experiments, were used to determine the constitution and configuration in a series of substituted penta-1,3-dien-5-ols.
    Additional Material: 5 Tab.
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  • 2
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Analytical pyrolysis-atmospberic pressure ionization (Py-API) tandem mass Spectrometry was used in the structure elucidation of the oxidalive and non-oxidative thermal decomposition products of cyclotetramethylenetetranitramine (HMX). The [15NO2]-, [15N8]- and [2H8]-HMX isotope preparations provided fundamental information in the determination of the identities of the various pyrolyzate species. All RDX pyrolysis product ions that were identified by Py-API tandem mass Spectrometry, i.e. m/z 44, 60, 74, 75, 85 and 98, were present in the pyrolyzate of HMX. In both RDX and HMX investigations, these ions provided identical mass spectral daughter ion analyses. HMX, however, provided additional ions at m/z 30, 58, 69, 71, 83 and 141. Of all thirteen ions identified in the Py-APJ mass spectrum of HMX, only that at m/z 75 contained a nitrogen atom that originated from the NO2 group. Standards analysis confirmed the identities of the ions at m/z 69, 71 and 141 as methyleneaminoacetonitrile, methylaminoacetonitrile and the caged compound hoxamethylenetetraamine, respectively. Isotopic analyses provided a high degree of confidence on the structural assignments of the ions at m/z 30 and 58 as methyleneimine and methyleneformamide; the ion at m/z 83, however, appeared to be a heterocyclic compound with daughter ion mass spectral elements similar to but not identical with that of 1-methylimidazole and 3-methylpyrazole.
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  • 3
    Electronic Resource
    Electronic Resource
    New York, NY : Wiley-Blackwell
    Rapid Communications in Mass Spectrometry 6 (1992), S. 197-202 
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The analysis of intact neutral oligosaccharides by on-line liquid chromatography/thermospray mass spectrometry is described. Molecular-weight information on oligomers up to a degree of polymerization of 10 is obtained using an aqueous mobile phase containing 10-4 mol/L sodium acetate, which was found to be compatible with thermospray interfacing and ionization. Ions due to sodiated and disodiated oligosaccharides are observed under these conditions without fragmentation. The aqueous 10-4 mol/L sodium acetate mobile phase is demonstated to be applicable in the separation of mixtures of oligosaccharides on a reversed-phase octadecyl-modified silica column.
    Additional Material: 6 Ill.
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  • 4
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The use of a laser-desorption mass spectrometer to examine a coal liquefaction extract known to contain high-molecular-mass material (from size-exclusion chromatography) has shown the presence of components of molecular mass in excess of 104Da for the first time. The molecules detected differ from each other in molecular mass by a few hundred or a few thousand Da. These preliminary results indicate that the basic coal-structure molecules probably consist of aromatic clusters on a chin, in reasonable agreement with current theories of coal structure.
    Additional Material: 2 Ill.
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  • 5
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: The on-line coupling of high-performance anion-exchange chromatography mass spectrometry is described. The system is applied to the analysis of neutral and acidic oligosaccharides obtained by (enzymic) degradation of plant-cell-wall polysaccharides. The features, potential and limitations of the method are discussed and exemplified with the analysis of some glucuronoxylan and xyloglycan digests. The system allows rapid molecular-mass determination of components in oligomer mixtures with 1-10 μg injected amounts.
    Additional Material: 5 Ill.
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  • 6
    ISSN: 0951-4198
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Physics
    Notes: Some synthetically obtained linear and cyclic phosphopeptides of low molecular weight have been studied by fast-atom bombardment and tandem mass spectrometry to verify the position of the phosphate group in these compounds. Based upon the occurrence/non-occurrence of loss of phosphoric acid from low abundance fragment ions induced by low- and high-energy collisions with target gases, it is shown that the position of the phosphate group in the phosphopeptides studied can be determined unequivocally.
    Additional Material: 7 Ill.
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  • 7
    ISSN: 0030-493X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The oxidative pyrolysis-atmospheric-pressure chemical ionization tandem mass Spectrometry (Py-APCI MS/MS) of Cyclotrimethylenetrinitramine (RDX) was investigated under various sample introduction conditions. Subambient (0.97 atm) as opposed to ambient (0.98 atm) pressure (1 atm = 101325 kPa) facilitated the appearance of new pyrolysis mass spectral ions, including m/z 44. Deuterated decomposition products from [2H]RDX contained amide groups and, depending on the ion source pressure, significant differences in the degree of proton-deuterium exchange occurred on the amide groups. The D2O Py-APCI MS/MS method also confirmed and extended the analogous H2O APCI information from RDX, [2H]RDX and pure standards. The m/z 44 decompositon species was identified as protonated dimethylimine, [H3CN=CH2]+ as opposed to its primary amine isomer, [H3CC(H)=NH]H+, which contains an acidic proton. It was determined that m/z 60 is due to protonated N-methylformamide and acetaldoxime, [H3CC(H)=NOH]H+.
    Additional Material: 2 Ill.
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  • 8
    ISSN: 0044-2313
    Keywords: Electrochemical synthesis ; Schiff bases metal complexes ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Elektrochemische Synthese von Metall(II)-Komplexen mit Schiffschen Basen: Kristallstruktur von Bis{2-[(4-methylphenyl)iminomethyl]pyrrolato}kupfer(II)Die elektrochemische Oxidation von anodischem Metall (Nickel, Kupfer, Zink, Cadmium) in einer Acetonitril-Lösung mit einer aus H-pyrrol-2-carbaldehyd abgeleiteten Schiffschen Base eines substitutierten Anilins (HL) liefert die gemischten Komplexe ML2. Die Kristallstruktur von Bis{2-[(4-methylphenyl)iminomethyl]pyrrolato}kupfer(II) wurde röntgenographisch bestimmt. Der Komplex kristallisiert monoklin in der Raumgruppe P21/n, a = 9,356(2), b = 16,697(2), c = 14,145(2) A, β = 108,47(2)°, Z = 4, und er besteht aus monomeren Molekülen, von denen die zentrale CuN4-Einheit eine verzerrt-tetraedrische Geometrie besitzt mit einem Diederwinkel der Flächen von 25,8(3)°. Die IR, 1H-NMR und UV-VIS Spektren werden im Zusammenhang mit der Struktur diskutiert.
    Notes: The electrochemical oxidation of anodic nickel, copper, zinc or cadmium in acetonitrile solutions of Schiff bases (HL) derived from H-pyrrole-2-carbaldehyde and substituted anilines gives compounds of general formula ML2. The crystal structure of bis{2-[(4-methylphenyl)iminomethyl]pyrrolato}copper(II) has been determined by X-ray diffraction. The compound crystallizes in the monoclinic space group P21/n with a = 9.356(2), b = 16.697(2), c = 14.145(2) Å and β = 108.47(2)°. The crystal structure consists of monomeric molecules in which the central CuN4 unit has distorted square-planar geometry with a dihedral angle of 25.8(3)° between the coordination planes. The IR, 1H NMR and UV-visible spectra of the complexes are discussed and related to the structure.
    Additional Material: 2 Ill.
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  • 9
    ISSN: 0044-2313
    Keywords: Electrochemical synthesis ; Schiff bases ; 2,2′-bipyridine bis{2-[(2-pyrrole)methylimino]5-methyl-phenolato}nickel (II) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Elektrochemische Synthese von Co, Ni und Zn Komplexen mit 2-Pyrrol-[N-(o-hydroxyphenyl)methylimin]: Kristallstruktur von 2,2′-Bipyridin-bis{2-[(2-pyrrol)methylimino]5-methylphenolato}nickel(II).Die elektrochemische Oxidation von anodischem Metall (Kupfer, Nickel und Zink) in einer Acetonitril-Lösung mit einer aus 2-Pyrrol-[N-(o-hydroxy-phenyl)methylimin] abgeleiteten Schiffschen Base (H2L) und einem Stickstoffliganden (1, 10-Phenanthrolin(phen) oder 2,2′-Bipyridin(bipy)) liefert die gemischten Komplexe ML2 phen und ML2 bipy. Die Kristallstruktur von 2,2′-Bipyridin-bis{2-[(2-pyrrol)methylimino]5-methyl-phenolato}nickel(II) wurde röntgenographisch bestimmt. Der Komplex kristallisiert orthorhombisch in der Raumgruppe Pccn, Z = 4, a ′ 19,430(2), b = 28,488(2), c = 17,567(1) Å. Die IR-, 1H NMR- und UV-Vis-Spektren werden im Zusammenhang mit der Struktur besprochen.
    Notes: The electrochemical oxidation of anodic cobalt, nickel, and zinc in acetonitrile containing both 2-pyrrole-[N-(o-hydroxyphenyl)methylimines] (H2L) and a bidentate ligand (1, 10-phenanthroline(phen) or 2,2′-bipyridine(bipy)) yielded compounds of general formula M(HL)2 · phen and M(HL)2 · bipy (M = Co, Ni, Zn). The crystal structure of 2,2′-bipyridine bis{2-[(2-pyrrole)methylimino]5-methylphenolato}nickel(II) was determined by X-ray diffraction. This compound crystallizes in the orthorhombic space group Pccn with a = 19.430(2), b = 28.488(2), c = 17.567(1) Å. The nickel atom has a distorted octahedral geometry, and the pyrrole nitrogen is not coordinated. The IR, 1H-NMR and UV-visible spectra of the complexes are discussed and related to the structure.
    Additional Material: 2 Ill.
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  • 10
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Direkte elektrochemische Synthese und Kristallstruktur des Zink(II)-carbamato-Komplexes{[N-methyl-N′-[(2-pyrrolyl)methylen]ethylendiamin][N-methyl-N-[2-[(2-pyrrolato)methylenamino]ethyl]carbamato]}zink(II)Die elektrochemische Oxidation von anodischem Zink in Acetonitril-Lösung einer Schiffschen Base, die aus Hpyrrol-2-carbaldehyd und N-methylethyldiamin dargestellt wurde, ergibt[Zn(C8H13N3)(C9H11N3O2)], dessen Kristallstruktur röntgenographisch bestimmt wurde. Die Verbindung kristallisiert im orthorhombischen Kristallsystem, mit der Raumgruppe Pbca und a = 13,757(2), b = 17,748(4), c = 14,808(4) Å, Z = 8. Die Verfeinerung führte bis zu einem R-Wert von 0,049 für 1407 unabhängige, beobachtete Reflexe. Die Kristallstruktur besteht aus monomeren Molekülen, in denen die zentrale ZnN4O-Einheit eine verzerrt trigonal bipyramidale Geometrie aufweist. Die Carbamatogruppe ist einzähnig gebunden.
    Notes: The electrochemical oxidation of anodic zinc in an acetonitrile solution of a Schiff base derived from Hpyrrole-2-carbaldehyde and N-methylethylenediamine gives [Zn(C8H13N3)-(C9H11N3O2)], whose crystal structure has been determined. The compound crystallizes in the orthorhombic space group Pbca (No. 61) with a = 13.757(2), b = 17.748(4), c = 14.808(4) Å and Z = 8. Refinement converged to R = 0.049 for 1407 independent observed reflections. The crystal structure consists of monomeric molecules in which the central ZnN4O unit has distorted trigonal bipyramidal geometry and the carbamato group is monodentate.
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