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  • 1
    Electronic Resource
    Electronic Resource
    Springer
    Fresenius' journal of analytical chemistry 357 (1997), S. 508-513 
    ISSN: 1432-1130
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract The quantitative characterization of macro-porous materials with regard to pore width and pore width distribution was accomplished for the first time by using 1H-NMR microscopy in combination with suitable methods of digital image analysis. Here we present the newly developed algorithm and discuss the first experimental results. Large-pored glass filter systems filled with silicon oil as intrusion fluid were used as references. Silicates of unknown pore width were analyzed both with the new method and with Hg intrusion. NMR image data were recorded using a 3D spin echo sequence, which gave 128 slice images with a spatial resolution of 14.5 μm × 14.5 μm within each slice, with a slice-thickness of 37 μm or 48 μm. A quantitative evaluation of the 3D NMR data, with regard to pore width and pore width distribution, was done using the appropriate image processing function of the HORUS program. Individual slice evaluation was performed first, followed by an analysis of the binding elements between the slices. Pore widths of the glass filters determined using this analytical algorithm were in accordance with the manufacturer’s values, and silicate pore widths were in good agreement with the values determined by Hg intrusion.
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Experiments in fluids 11 (1991), S. 186-190 
    ISSN: 1432-1114
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract A cylindrical electrodiffusion probe for the measurement of liquid velocity vectors in the plane perpendicular to its axis was developed as an analogue to the triple-split film thermoanemometer. The geometry of the probe enables high directional resolution in the whole range of 360°. The total mass transfer of the probe was well correlated by the relation Sh = 0.76 Sc 0.33 Re 0.47.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Experiments in fluids 16 (1994), S. 368-374 
    ISSN: 1432-1114
    Source: Springer Online Journal Archives 1860-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The influence of eddy shedding on the instantaneous readings of a three-segment cylindrical electrodiffusion velocity probe was investigated in an immersed jet with a very low turbulence intensity, σ = 1.2%. The velocity fluctuations measured by the three-segment probe were smaller than 2.6%, and the maximum error in the flow angle estimation was 2∘. Vortices with the Strouhal frequency were detected by a simple electrodiffusion probe placed downstream of the three-segment probe, but no peaks with this frequency were found on the frequency spectra of the three-segment probe. From the probe response to a stepwise change of the polarization voltage the characteristic times of the transient process were estimated.
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  • 4
    Electronic Resource
    Electronic Resource
    Springer
    Naturwissenschaften 58 (1971), S. 321-322 
    ISSN: 1432-1904
    Source: Springer Online Journal Archives 1860-2000
    Topics: Biology , Chemistry and Pharmacology , Natural Sciences in General
    Type of Medium: Electronic Resource
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  • 5
    Electronic Resource
    Electronic Resource
    Springer
    Journal of applied electrochemistry 21 (1991), S. 1073-1076 
    ISSN: 1572-8838
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Electrical Engineering, Measurement and Control Technology
    Notes: Abstract A three-segment direction specific probe based on the electrodiffusion measuring technique was used to measure local liquid velocities in gas-liquid flow. Dissolved oxygen was employed as depolarizer instead of the usually applied redox system ferro-ferricyanide in water. The concentration of the auxiliary electrolyte K2SO4 was so low that coalescence behaviour of the gas-liquid system was not influenced. It was possible to measure liquid velocities up to ca 100cm s−1. The probe showed satisfying sensitivity to flow direction. Furthermore, unequivocal discrimination between signals from the liquid and gas phases was achieved.
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  • 6
    Electronic Resource
    Electronic Resource
    Springer
    Journal of applied electrochemistry 24 (1994), S. 666-669 
    ISSN: 1572-8838
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Electrical Engineering, Measurement and Control Technology
    Notes: Abstract An electrodiffusional three-segment probe was developed with which local axial and radial liquid velocities can be determined. Application of this probe in gas-liquid flow yields information on local gas hold-up. In coalescing media the commonly used redox-system Fe(CN) 6 3− /Fe(CN) 6 4 should be replaced by dissolved oxygen as depolarizer. Measurements of local axial and radial liquid velocity and turbulence intensity in different bubble columns (D = 150 and 600 mm) showed good agreement with data obtained by hotfilm anemometry.
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  • 7
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 865-870 
    ISSN: 0044-2313
    Keywords: Fluoridolysis ; N-Phosphoryl Phosphazenes ; Fluorophosphates ; Diazadiphosphetine ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoridolysis of N-Phosphoryl PhosphazenesIn the reaction of the N-phosphoryl phosphazenes X3P=N—P(Y)X2 (X = Cl, PhO, Et2N, CF3CH2O, PrS, Ph; Y = O, S) (1-18) with Et3N · nHF (n ≍ 3 or 0.6) fluoro derivatives of N-phosphoryl phosphazenes (see table 2) as well as N-phosphorylated imiddotetrafluorophosphates, [F4P=N—P(Y)Cl2]- (Y = O, S), and imidopentafluorophosphates, [F5P—N—P(Y)X2]2- or [F5P—NH—P(O)X2]- (see table 3), are formed. t-BuNHPCl2=N—POCl2 reacts in acetonitrile with Et3N or i-Pr2EtN to form a product, representing probably the diazadiphosphetine (5 b).
    Notes: Bei der Umsetzung der N-Phosphorylphosphazene X3P=N—P(Y)X2 (X = Cl, PhO, Et2N, CF3CH2O, PrS, Ph; Y = O, S) (1-18) mit Et3N · nHF (n ≍ 3 oder 0,6) werden durch den Austausch von Chlor sowie PhO-, Et2N- und CF3CH2O-Gruppen gegen Fluor Fluorderivate von N-Phosphorylphosphazenen (siehe Tab. 2) sowie N-phosphorylierte Imiddotetra- und -pentafluorophosphate, [F4P=N—P(Y)Cl2]- (Y = O, S) und [F5P—N—P(Y)X2]2- bzw. [F5P—NH—P(O)X2]- (siehe Tab. 3) gebildet. t-BuNHPCl2=N—POCl2 reagiert in Acetonitril mit Et3N oder i-Pr2EtN zu einem Produkt, bei dem es sich höchstwahrscheinlich um das Diazadiphosphetin (5 b) handelt.
    Additional Material: 5 Tab.
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  • 8
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 621 (1995), S. 894-900 
    ISSN: 0044-2313
    Keywords: Fluoridolysis ; Imidodiphosphoryl Compounds ; Methanediphosphonic Acid Derivatives ; Azadiphosphetidine ; Pentafluorophosphates ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Fluoridolysis of Diphosphoryl CompoundsThe behaviour of diphosphoryl compounds [X2(O)P]2Y in fluoridolysis reactions is decisively determined by the nature of the bridging group Y. In the cases of Y = NH and CH2 and X = Cl [F2P(O)]2N- and [F2P(O)]2CH2 are obtained quantitatively. For Y = NPh, O, and CH2 the formation of phosphorylated pentafluorophosphates [F5P—Y—POX2]- is observed. Amido and ester derivatives containing fluorine (see table 2) are obtained from the corresponding chloro compounds by Cl/F exchange. Fluoridolysis of the azadiphosphetidine 19 results in the formation of acyclic 19 a.
    Notes: Das Fluoridolyseverhalten von Diphosphorylverbindungen [X2(O)P]2Y wird maßgeblich durch die Brückengruppe Y bestimmt. Im Falle von Y = NH und CH2 sowie X = Cl werden quantitativ [F2P(O)]2N- und [F2P(O)]2CH2 erhalten. Für Y = NPh, O und CH2 wird die Bildung von phosphorylierten Pentafluorophosphaten [F5P—Y—POX2]- beobachtet. Aus chlorhaltigen Amido- und Esterderivaten werden durch Chlor-Fluor-Austausch die entsprechenden Fluorderivate erhalten (siehe Tab. 2). Die Fluoridolyse des Azadiphosphetidins 19 ergibt die acyclische Verbindung 19 a.
    Additional Material: 5 Tab.
    Type of Medium: Electronic Resource
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  • 9
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 563 (1988), S. 167-172 
    ISSN: 0044-2313
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Tetraphenyl Imidodiphosphate as Ligand in Fluoro Complexes. 1. Fluoro Complexes of TitaniumIn acetonitrile TiF4 reacts with tetraphenyl imidodiphosphate forming two tetrafluoro (I, II) and three trifluoro complexes (III, IV, V) as well as one difluorotitanium complex (VI). The difluoro complex VI is exclusively formed by sing an excess of the ligand. VI was isolated and analytically characterized. The constitution and configuration of the complexes are concluded from 19F and 31P n.m.r. data. The tetraphenyl imidodiphosphate is only bidentately bonded, i.e. as chelate or bridging ligand; in the substitution complexes III-VI it is coordinated as anion.
    Notes: TiF4 bildet mit Imidodiphosphorsäuretetraphenylester in CH3CN zwei Tetrafluoro- (I, II) und drei Trifluorokomplexe (III, IV, V) sowie einen Difluorotitan-Komplex (VI). Mit Ligandenüberschuß entsteht ausschließlich der Difluorokomplex, der isoliert und elementar-analytisch charakterisiert wurde. Die Konstitutions- und Konfigurationsaussagen zu den übrigen Komplexen basieren auf 19F- und 31P-NMR-Untersuchungen. Der Imidodiphosphorsäureestr ist in den Komplexen stets zweizähnig als Chelat- oder Brückenligand gebunden; in den Substitutions-komplexen III-VI ist er in seiner anionischen Form enthalten.
    Additional Material: 1 Tab.
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  • 10
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Zeitschrift für anorganische Chemie 614 (1992), S. 95-101 
    ISSN: 0044-2313
    Keywords: silicate solution ; water glass ; NMR spectroscopy ; dre adsorption ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: The Influence of Temperature and Impurities Addition on the Properties and the Constitution of Sodium Water Glass SolutionsSodium water glass (NaWG-)solutions of constant composition (SiO2/Na2O = 3,3; CSiO2 = 6,2 M) and different concentration of impurities (Fe, Al, Ti, Cu, chloride, sulfate) were investigated in dependence on temperature by means of the dye absorption method, 1H- and 23Na-NMR spectroscopy. It is shown, that the differences in the dye absorption spectra of normalized technical NaWG-solutions, mainly depend on the Fe-concentration in the solutions and their thermal history. From the results follow a crosslinking of polymeric silicate species by Fe—O—Si bonds and/or hydrogen bridges and a fully or partially degradation of these bonds at higher temperatures (150°C).
    Notes: Natriumwasserglas-(NaWG-)lösungen konstanter Zusammensetzung (SiO2/Na2O = 3,3; CSio2 = 6,2 M) und mit unterschiedlichen Fremdatomgehalten (Fe, Al, Ti, Cu, Chlorid, Sulfat) wurden in Abhängigkeit ihrer thermischen Vorbehandlung mit Hilfe der Farbstoffadsorptionsmethode sowie der 1H- und 23Na-NMR-Spektroskopie untersucht. Es zeigt sich, daß die Unterschiede in den Farbstoffspektren normierter technischer NaWG-Lösungen im wesentlichen von dem Fe-Gehalt der Lösungen und ihrer „thermischen Vergangenheit“ abhängen. Die Ergebnisse der Farbstoffmethode und NMR deuten darauf hin, daß in Fe-haltigen NaWG-Lösungen bei 80°C Vernetzungen der polymeren Silicatteilchen über Fe—O—Si-Bindungen und/oder Wasserstoffbrückenbindungen erfolgen, die bei höheren Temperaturen (150°C) wieder ganz oder teilweise gelöst werden.
    Additional Material: 5 Ill.
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