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  • 1
    Electronic Resource
    Electronic Resource
    Hoboken, NJ : Wiley-Blackwell
    AIChE Journal 33 (1987), S. 1698-1706 
    ISSN: 0001-1541
    Keywords: Chemistry ; Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Particulate expansion and minimum bubbling parameters (n, u′t, umB, εmB) are measured for fine carbon powders (dp = 44 and 112 μm) fluidized with synthesis gas (H2/CO = 0.8) at pressures within the range 2,070 〈 P 〈 12,420 kPa in an industrial, pilot-scale fluidized bed. Deviations between minimum bubbling (umB and εmB) and minimum fluidization (umf and εmf) conditions increase with increasing pressure, P. The expansion index, n, decreases with increasing P and always exceeds values recommended by Richardson and Zaki for solid/liquid systems. Particulate bed expansion for the fine powders is well characterized by the equations of Foscolo et al. and Abrahamsen and Geldart. The theory of Foscolo and Gibilaro adequately estimates the onset of bubbling for both powders at all P, provided that experimentally determined values of n and u′t, are applied. For the dp = 112 μm powder, the theory of Foscolo and Gibilaro is applicable with calculated values of ut and experimental values of n.
    Additional Material: 10 Ill.
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  • 2
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Numerous monofunctional amines have been reacted with dimethylthiophosphinic chloride to form stable derivatives. Their good gas chromatographic properties and abundant molecular ions afforded highly sensitive and specific detection by selected ion monitoring (SIM) down to the picogram level. Based upon this derivatization procedure, new methods for the determination of aniline in serum and urine by SIM were developed. The minimum detectable concentration of aniline was 500 pg ml-1. Linear response curves were obtained from 1.5 to 150 ng ml-1 using (2H5)aniline as the internal standard. Specific derivatization of a series of bifunctional amines was achieved with methyldichlorophosphine and sulfur resulting in the formation of stable phospholidine-thiones. These derivatives chromatograph well on nonpolar stationary phases, and their mass spectra exhibit abundant molecular ions. This derivatization reaction was applied to the quantification of ephedrine from urine and serum by SIM with (2H2)ephedrine as the internal standard. The detection limit of the method was 1 ng ml-1. The linearity was established in the range from 10 to 160 ng ml-1.
    Additional Material: 9 Ill.
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  • 3
    Electronic Resource
    Electronic Resource
    Chichester : Wiley-Blackwell
    Biological Mass Spectrometry 5 (1978), S. 302-311 
    ISSN: 0306-042X
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectra of 20 differently substituted dimethylthiophosphinic esters of aromatic hydroxy compounds are presented. Fragmentation routes were investigated using high resolution mass measurements, decoupled metastable determinations and deuterium labelling. All compounds exhibited abundant molecular ions and typical phosphorus-containing ions. Characteristic elimination processes strongly dependent upon the respective type of substitution were observed. Due to their high stability, their great ease of formation and their good gas chromatographic properties these new types of derivatives are of special interest for establishing gas chromatography mass spectrometry profiles of acidic catecholamine metabolites.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 425 (1976), S. 151-154 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. XX. On the Reaction of NiCl2 · 2 PR3 and CoCl2 · 2 PR3 with LiSn(CH2C6H5)3LiSn(CH2C6H5)3 reacts with NiCl2 · 2 P(n-C4H9)3 in tetrahydrofuran forming benzyl nickel chloride, which could be isolated in form of the bipyridyl complex C6H5CH2-NiCl · dipy. NiCl2 · 2 P(C6H5)3 and CoCl2 · 2 P(C6H5)3 are reduced to complexes of the formula MCl · 2 P(C6H5)3 · 3 THF (M = Ni, Co).
    Notes: LiSn(CH2C6H5)3 reagiert mit NiCl2 · 2 P(n-C4H9)3 in Tetrahydrofuran zu Benzylnickelchlorid, das als Dipyridylkomplex isoliert werden konnte. Bei Einsatz von NiCl2 · 2 P(C6H5)3 und CoCl2 · 2 P(C6H5)3 erfolgt dagegen eine Reduktion zu Komplexen der Zusammensetzung MCl · 2 P(C6H5)3 · 3 THF (M = Ni, Co).
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 455 (1979), S. 3-12 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXIX. Dibenzyl Manganese - Preparation and ReactionsManganese(II) acetylacetonate reacts with tribenzyl aluminium and dibenzyl magnesium forming the yellow complexes 3(C6H5CH2)2Mn · Al(acac)3 and (C6H5CH2)2Mn · Mg(acac)2 Dibenzyl manganese is also formed at the reaction of dibenzyl magnesium or benzyl magnesium chloride with MnCl2 · 1.5 THF and was separated as the dioxan complex (C6H5CH2)2Mn · 2C4H8O2, the ligands of which can be removed to a great extent in vacuum.Dibenzyl manganese reacts with CO2, CS2 and SO2 with insertion into the Mn-C-bonds. The corresponding manganese compounds were isolated and furtherly characterized.
    Notes: Mangan(II)-acetylacetonat reagiert mit Tribenzylaluminium bzw. Dibenzylmagnesium zu den gelben Komplexen 3(C6H5CH2)2Mn · Al(acac)3 bzw. (C6H5CH2)2Mn Mg(acac)2. Dibenzylmangan entsteht auch bei Einwirkung von Dibenzylmagnesium oder Benzyl magnesiumchlorid auf MnCl2 · 1,5 THF; eine Abtrennung von den Magnesiumsalzen gelingt in Form des 1,4-Dioxankomplexes (C6H5CH2)2Mn · 2C4H8O2, dessen Ligandenmoleküle im Vakuum weit gehend entfernt werden können.Dibenzylmangan reagiert mit CO2, CS2 und SO2 unter Insertion in die Mn-C-Bindungen. Die entsprechenden Mangansalze wurden isoliert und näher charakterisiert.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 508 (1984), S. 50-54 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. XXXVII. About the Existence of 1-Norbornyl Compounds of Tungsten and MolybdenumReactions of WCl6, WCl4, WO2Cl2, WOCl4, MoCl5, and MoO2(acac)2 with 1-Norbornyl lithium (1-NorLi1)) are described. From WCl6 and WCl4 [(1-Nor)2W]n is formed, whereas in dependence of the solvent WO2Cl2 and WOCl4 are transformed into the complexes Li2[1-NorWOCl4] · THF, Li[WOCl4], Li[WO2Cl2], and Li2[WO2Cl2]. MoCl5 and MoO2(acac)2 are reduced with formation of Li[MoCl5], Li[MoO2(acac)2] and Li2[MoO2(acac)2].  -  Stable (1-Nor)4M-derivatives of molybdenum and tungsten, comparable those of 3d-metals (M = Ti—Co) seem not to exist.
    Notes: Es wird über Reaktionen von WCl6, WCl4, WO2Cl2, WOCl4, MoCl5 und MoO2(acac)2) mit 1-Norbornyllithium (1-NorLi1)) berichtet. Ausgehend von WCl6 und WCl4 wird [(1-Nor)2W]n gebildet, während WO2Cl2 und WOCl4 je nach Lösungsmittel Komplexe der Formeln Li2[1-NorWOCl4] · THF, Li[WOCl4], Li[WO2Cl2] und Li2[WO2Cl2] ergeben. MoCl5 und MoO2(acac)2 werden zu Li[MoCl5], Li[MoO2(acac)2] und Li2[MoO2(acac)2] reduziert. - Den stabilen (1-Nor)4M-Derivaten der 3d-Metalle (M = Ti—Co) vergleichbare Verbindungen des Molybdäns und Wolframs scheinen nicht zu existieren.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 521 (1985), S. 57-60 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal alkyl Compounds. XXXIX. About 3(N,N-Dimethylamino) propyl Lanthanide CompoundsLaCl3, PrCl3, and ErCl3 react with dimethylaminopropyl lithium (RLi) in tetrahydro-furan as a solvent with formation of complexes of the type Li3[LnR3Cl3]. In a similar way the Li3[CeR6] derivative is formed from CeCl3.The organolanthanide complexes were characterized by elementary analysis, hydrolysis and thermolysis products, the effective magnetic moments and the i.r. spectra.
    Notes: LaCl3, PrCl3, und ErCl3 reagieren mit Dimethylaminopropyllithium (RLi) in Tetrahydrofuran als Lösungsmittel zu Komplexen des Typs Li3[LnR3Cl3]. Die entsprechende Reaktion mit CeCl3 führt dagegen zum Li3[CeR6]-Derivat.Eine nähere Charakterisierung der Verbindungen erfolgte durch Elementaranalysen, ihre Hydrolyse- und Thermolyseprodukte, die effektiven magnetischen Momente und ihre IR-Spektren.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 543 (1986), S. 192-198 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Organo Transition Metal Compounds. XLIX. Reactions of Cerium(IV) Acetylacetonate with Organolithium and Organomagnesium CompoundsReacting Ce(acac)4 with lithium organyls RLi (R = CH3 1-Nor1), ((CH3)2NCH2CH2CH2) in the molar ratio 1:1 the cerium compound is reduced with formation of Li[Ce(acac)4]. Using a molar ratio of Ce:Li = 1:4 organocerium complexes of the composition R3Ce · 3 Li(acac) or Li3[R3Ce(acac)3] are formed. From reactions with excess CH3Li (Ce: Li = 1:7) Li3[Ce(CH3)6] · 3 Li(acac) could be isolated.All cerium complexes are characterized by elementary analysis, hydrolysis products, i.r. spectra, and molecular weight determination.
    Notes: Ce(acac)4 reagiert mit Lithiumorganylen RLi (R = CH3, 1-Nor1), ((CH3)2NCH2CH2CH2) im Molverhältnis 1:1 unter Reduktion zum Cerium(III)-Komplex Li[Ce(acac)4]. Wählt man ein Molverhältnis von 1:4, so entstehen Organocerium(III)-Komplexe der Zusammensetzung R3Ce · 3 Li(acac) bzw. Li3[R3Ce(acac)3]. Donormoleküle bewirken keine Abspaltung des Li(acac), sondern werden zusätzlich addiert unter Bildung von Komplexen des Typs Li3[R3Ce(acac)3] · n D (D = THF, n = 2; D = DME, TMED2), n = 1. Bei Reaktionen mit überschüssigem CH3Li (Ce:Li = 1:7) wurde Li3[Ce(CH3)6] · 3 Li(acac) isoliert.Bei Umsetzungen von Ce(acac)4 mit Dibenzyl- und Bis(1-naphthylmethyl)magnesium wurden Cerium(III)-Komplexe der Zusammensetzung Ce(acac)3 · RMg(acac) gebildet.Alle erhaltenen Verbindungen wurden durch ihre Elementaranalysen, Hydrolyseprodukte, IR-Spektren und durch Molmassebestimmungen charakterisiert.Ce(acac)4 reacts with dibenzyl and bis (1-naphthylmethyl) magnesium with formation of complexes of the type Ce(acac)3 · RMg(acac).
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  • 9
    ISSN: 0044-2313
    Keywords: 2-(Dimethylaminomethyl)ferrocenyl 3 d metal compounds ; preparation ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Contributions to the Chemistry of Transition Metal Alkyl Compounds. 57. 2-(Dimethylaminomethyl)ferrocenyl Compounds of 3 d Elements[2-(Dimethylaminomethyl)ferrocenyl]lithium, (FcN)Li (I), reacts with MCl2 · xTHF to (FcN)2Mn (II), (FcN)2Co (III), Li2[Fe(FcN)2Cl2] (IV) as well as with FeCl3 to (FcN)3Fe (V). In the same way the complex (C5H5)2V(FcN) (VI) was obtained from (C5H5)2VCl. When I is reacted with M(acac)3 (M = Cr, Co) only a partial ligand exchange took place  -  independently from the molar ratio of the reactants  -  with formation of (FcN)Cr(acac)2 (VII) and (FcN)Co(acac) (VIII).An intensive characterization of II-VIII was achieved by elementary analysis, determination of molecular weights, IR-, UV-VIS- and 1H-NMR spectra as well as determination of effective magnetic moments.
    Notes: [2-(Dimethylaminomethyl)ferrocenyl]lithium, (FcN)Li (I), reagiert mit MCl2 · xTHF zu (FcN)2Mn (II), (FcN)2Co (III), Li2[Fe(FcN)2Cl2] (IV) sowie mit FeCl3 zu (FcN)3Fe (V). Auf gleiche Weise wurde aus (C5H5)2 VCl der Komplex (C5H5)2V(FcN) (VI) erhalten. Bei der Einwirkung von I auf M(acac)3 (M = Cr, Co) erfolgte unabhängig vom Molverhältnis der Reaktanten nur ein partieller Ligandenaustausch unter Bildung von (FcN)Cr(acac)2 (VII) und (FcN)Co(acac) (VIII).Eine eingehende Charakterisierung von II-VIII erfolgte durch Elementaranalysen, Molmassebestimmungen, IR-, UV-VIS- und 1H-NMR-Spektren sowie Bestimmung der effektiven magnetischen Momente.
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  • 10
    ISSN: 1052-9306
    Keywords: Chemistry ; Analytical Chemistry and Spectroscopy
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The mass spectra of the dimethylphosphinic, dimethylthiophosphinic and dimethylphosphinous ester derivatives of several monohydroxy steroids are reported. The fragmentations of the derivatized steroids largely depend on the nature of the the phosphorus-containing ester group. Phenolic ester derivatives exhibit the base peak at the molecular ion, whereas the spectra of the secondary phosphinic esters are dominated by very intense protonated phosphinic acid ions [Me2 P(XH)(OH)]+ at m/e 95 (X = O) or at m/e 111 (X = S). The present results also indicate the low ionization potential for the phosphinic ester group. Due to their good gas chromatographic properties, these steroid derivatives appear to be particularly suitable for gas chromatographic mass spectrometric analysis of biochemical materials.
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