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  • 101
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 58-58 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 102
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 68-78 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper reviews the principle of the phase-Doppler particle sizer by means of examples of the effects of varying the various experimental parameters. The examples are computed by means of a comprehensive numerical model of a complete phase-Doppler system including many practical aspects such as aperture size, polarization filters and detector properties. First the phase-Doppler principle is explained as a logical development of an interferometric measurement of the phase of the light scattered from a particle. Then the standard phase-Doppler analyzer (PDA) is decribed followed by some newer or less known variations of the principle intended to measure, e.g., in the backscatter direction, to size very small particles or to determine the refractive index of a particle. Finally, the trajectory problem in PDA measurements is briefly discussed.
    Additional Material: 30 Ill.
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  • 103
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 89-96 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Light scattering by particles is often used to determine velocities or concentrations of particles in gaseous or liquid streams. Within the Lorenz-Mie theory, light scattering is well understood both for a single compact spherical particle and a single multilayered particle in a non-absorbing surrounding medium. However, in some cases of practical importance the Lorenz-Mie theory in its present form may fail to describe the scattering because the host medium is absorbing (e.g. water droplets in oil). In this case, a new treatment of the scattering theory is required. In previous work, solutions were obtained in the far-field of the scattering sphere. In this paper, a rigorous solution is derived from the calculation of the total absorption rate of the particle in the host medium, which is valid for all distances from the surface of the encapsulated particle. It is shown that it is necessary to consider finite sizes R of the integrating sphere when dealing with absorbing host media. Cross-sections are defined which are characteristic quantities not only for the particle, depending on the size of a conceptual sphere around the scatterer and the imaginary part of the refractive index of the host medium. The results obtained are discussed for the case of non-absorbing host media and in the far-field approximation. Some numerical examples are given which are also related to experimental results.
    Additional Material: 6 Ill.
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  • 104
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 104-111 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: After having recalled basic theoretical results concerning the extension of generalized Lorenz-Mie theory to the case of multilayered spheres, results connected with phase-Doppler anemometry are considered, showing the influence of Gaussian beam intensity profiles on the light scattering properties of these particles. Particular emphasis is placed on the case of water-coated carbon core particles, for which the possibility of obtaining simultaneous size measurements of the core and outer diameters is discussed. The sensitivity of the technique to particles with a refractive index profile is also considered, showing that this technique is more sensitive to changes in the average refractive index of the particles than to refractive index profiles, such as produced by high pressure and temperature stresses, at least for the studied geometry.
    Additional Material: 10 Ill.
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  • 105
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 34-40 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Microcontamination of product surfaces by deposited particles is an important problem in clean technologies. A most sensitive product to contamination by particles is a wafer during chip production. Therefore, methods for monitoring particle deposition on wafer surfaces have been developed in the last decade. A wafer with an unstructured and reflecting surface is inserted into the process equipment. After some time, depending on the process, this wafer is removed from the process equipment and is analysed with respect to the number of deposited particles using a wafer scanner. However, in situ particle detection in a process chamber is not possible with this technique. This would be possible if, instead of a monitor wafer, a transparent glass plate is mounted, e.g. in the housing of the process equipment. Then the illuminating and scattered light detection equipment can be mounted outside the process equipment. Since both the illuminating laser beam and the scattered light have to be transmitted through the glass plate, losses will occur, which will reduce the lower limit of detection with respect to particle size. In this article we estimate the detection possibilities theoretically and experimentally.A simple model based on Mie and vector scattering theory has been developed to describe the light-scattering behavior of a single spherical particle on a glass plate with random surface irregularities. The scattered light of individual particles of four particle sizes (1.03, 1.6, 2.92 and 4.23 μm) on the same glass surface and from the uncontaminated area of the glass plate was measured for unpolarized and normally incident light. The values of the scattered light from this model were compared with the experimental results. The comparison shows a reasonable agreement of the angular distribution of the scattered light. The developed model is used to predict the lower limit of detection for particles on a transparent surface. The theoretical estimations show that it should be possible to detect particles of a diameter down to 0.2 μm with the described measurement technique.
    Additional Material: 9 Ill.
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  • 106
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 59-67 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The ability to routinely make simultaneous measurements of the size and velocity of individual spherical particles is identified as a crucial component of advances in the science and technology of multiphase systems and processes. Since it is the dual beam interferometer identified here as the phase-Doppler particle-sizing velocimeter (PD) that has provided this capability, and since 1995 marks twenty years from a seminal paper by Durst and Zaré, a historical review is warranted and is presented. The roots and context of the development of PD are traced from the days of laser Doppler velocimetry (LDV) in the early 1970's through work culminating at several laboratories in the mid 1980's. A number of important contributions and the engineers and scientists responsible for those contributions are recognized.
    Additional Material: 12 Ill.
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  • 107
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 79-88 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The Scattering of focused laser beams by arbitrarily shaped dielectric bodies is investigated theoretically. The beam description is based on Davis third-order beam approximation for the field components. The scattering problem can be solved on a spherical basis by the extended boundary condition method or by the so-called modified version of the extended boundary condition method. For spheroidal particles with small eccentricities, a perturbation technique for the internal subproblem of the extended boundary condition method is described. This procedure is applied to analyse the influence of the particle shape and orientation on the response of a phase-Doppler system.
    Additional Material: 2 Ill.
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  • 108
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 97-103 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A new technique for the calculation of the optical properties of agglomerated spherical primary particles is presented. By means of the so-called virtual refractive index, the multiple scattering within the agglomerate is decribed by a modified Mie solution, thus avoiding restrictions with respect to the primary particle size. An additional benefit of the method is the small numerical expense required, permitting practical use for complex agglomerate structures such as real combustion aerosols. Utilizing this method, attention is focused on the calculation of the extinction cross-section of real combustion aerosols in order to discuss the results of multiple-wavelength extinction measurements within combustion systems. It is found that approximately the primary particle diameter is determined. Furthermore, the error that occurs can be avoided by means of the method presented without a detailed knowledge of the agglomerate size. Thus, the present work eliminates some current uncertainties inherent in optical combustion aerosol characterization.
    Additional Material: 8 Ill.
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  • 109
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The principle of the dual burst technique (DBT) based on phase-Doppler anemometry (PDA) is proposed for simultaneous particle refractive index, size and velocity measurements. This technique used the trajectory effects in PDA systems to separate the two contributions of the different scattering processes. In the case of forward scattering and refracting particles, it is shown that from the phase of the reflected contribution, the particle diameter can be deduced, whereas from the refracted contribution the particle refractive index and velocity can be obtained. Furthermore, the intensity ratio of these two scattering processes can be used for absorption measurements. Simulations based on generalized Lorenz-Mie theory and experimental tests using monodispersed droplets of different refractive indices and absorption coefficients have validated this technique.
    Additional Material: 19 Ill.
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  • 110
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 125-129 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Rainbow refractometry allows the determination of the refractive indices of droplets if a homogeneous refractive index can be assumed throughout the whole droplet. The influence of gradients on the angular position of the rainbow was examined for refractive index distributions with constant gradients and for distributions as they occur during cooling, heating and burning of droplets. Geometrical optics were used to determine rainbow positions. For a given value of refractive index at the surface, the rainbow position is in many cases a measure for the gradient itself. It was found that information obtained for constant gradients can often be used in cases with more complex distributions, which are found, for instance, for droplets undergoing heat-transfer processes. Significant errors may be obtained only for a very short initial phase of the process. Experimental results obtained with monosized droplet streams, which confirm theoretical predictions of the influence of gradients on the rainbow position, are presented.
    Additional Material: 9 Ill.
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  • 111
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 165-170 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The accurate measurement of mass flux is identified as being essential for the successful use of phase-Doppler anemometry (PDA) in many applications, in particular with sprays. Thus measured sizes of individual droplets and the cross-sectional area to which the flux measurement is referenced must be reliable. This paper investigates sources of measurement error in each of these quantities and provides means to eliminates or minimize these errors. A new PDA configuration, termed dual-mode PDA, is introduced as an implementation of these suggestions. Example measurements illustrate the advantages of the system over conventional arrangements.
    Additional Material: 9 Ill.
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  • 112
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 171-176 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: On the basis of the numerical solution of the radiative transfer equation (RTE), the influence of non-sphericity of oriented spheroidal particles on radiation intensity formation in a layer with a multiple scattering regime is considered. For solving the RTE with characteristics depending on the propagation direction of the radiation beam, an algorithm is developed based on the method of layer doubling. Calculations are presented of angle correlations for intensities of radiation in a layer with Fresnel reflection on the boundaries, and reflection and transmission coefficients.
    Additional Material: 8 Ill.
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  • 113
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    Electronic Resource
    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 114
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 263-271 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Catalyst surface characterizations have been carried out to investigate the role of dispersion on catalyst activity and to probe the occurrence of oscillations in coking levels with cycle number generally observed during multiple deactivation and regeneration schemes. The titrations were done, cycle by cycle, at 430°C after oxidation and at the same temperature (430°C) after reduction at 500°C. Results show the usually observed trend - that the dispersions after oxidation are higher than those after reduction. The average decline in dispersion from oxidation to reduction was calculated to be 39.25%. It was observed that the cycles with high toxic coke removal were characterised by high deactivation times. The deactivation times were still high even for cycles subsequent to those with low dispersion. At high dispersions the catalyst had short deactivation times, that is the small crystallites deactivate faster than large ones. The nature of reducebale coke and the efficiency of its removal is a much more determinant factor of catalyst activity than the level of metal disperision. Thus prolonged toxic coke reduction at the high temperature of 500°C, though resulting in an apparent lowering of dispersion, does not affect the quality of the catalyst. The dispersion before reduction could be retained on oxidation. Hence reduction at 500°C did not introduce sintering.
    Additional Material: 8 Ill.
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  • 115
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 291-298 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Reasons are given why the axial dispersion in a gas flowing through a packed bed may be influenced by the elasticity - or compressibility - of the fluid. To support this hypothesis, experiments have been done in a packed column at pressures from 0.13 to 2.0 MPa. The elasticity E of a gas is proportional to the pressure P and the compressibility to 1/P. The axial dispersion coefficients as determined were found to be a function of the pressure in the packed bed in the turbulent flow region of 3 〈 Rep 〈 150 if the Bodenstein number is plotted as a function of the particle Reynolds number. This is shown to be an artifact. The pressure influence is eliminated, if Bom, ax is plotted versus the ratio of the kinetic forces over the elastic forces ϱu2/E. Regrettably, Bom, ax seems to be independent of ϱu2/E. For the moment we only can conclude that Bom, ax in the turbulent region is a unique function of the velocity of the gas which flows through the packed bed. Although the fact that a constant Bo value is obtained when plotted against ϱu2/E, the experimental results are so intriguing we wanted to make them public already now. The experimental work proceeds.
    Additional Material: 15 Ill.
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  • 116
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 337-346 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A unified gas/ solid reaction model has been formulated for multi reactions with multi gas and solid species. The transient formulation has been followed by finite-difference method and subsequent solution via an iterative procedure. The simulation produces intermediate results for concentration profiles of various components and pressure and temperature distribution, in addition to various structural parameters within a reacting pellet. The effect of structural parameters is analysed. The general formulation allows homogeneous and heterogeneous reactions. Solid state processes can also be accommodated.
    Additional Material: 12 Ill.
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  • 117
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 364-372 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Calcination and carbonation behaviour of dolomite has been studied in a pressurised thermo balance at pressures in the range of 1.1 to 2.3 MPa and for temperatures ranging from 730 to 840°C. The atmosphere consisted of nitrogen containing up to 20 vol.-% carbon dioxide. The calcination of dolomite has been studied as a function of temperature, particle size, and Pco2. An investigation concerning possible mass transfer restrictions for the experimental system and a model investigation of the calcination rate in CO2 atmosphere has been made. Further, the effect of calcination on the BET surface and the BET surface including the surface structure due to successive temperature cycles has been studied. The temperature for the initialisation of calcination of dolomite in CO2 atmosphere was independent of both Pco2 and the particle size. No conclusive indications on mass transfer restrictions have been detected for the experimental system. A significant difference in calcination rate as a function of particle size existed for decomposition in CO2 atmosphere. A model for homogeneously progressing chemical reaction parallel with a shrinking core chemical reaction together with a mass transfer control mechanism was found to describe the calcination rate in CO2 atmosphere most accurately.
    Additional Material: 6 Ill.
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  • 118
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 410-419 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: General simple criteria to predict and analyze the influence on trickle-bed reactors behavior of three phenomena, namely, plug flow deviations, external wetting efficiency and external mass transfer resistance, are developed. Criteria predictions are compared with results arising from a comprehensive mathematical model widely employed to describe trickle-bed reactors behavior and with other particular criteria reported in the literature. Present criteria applications to different sets of experimental data exemplify their practical utility for various actual situations and verify their validity. Besides, they constitute simple tools to diagnose detrimental on trickle-bed reactors operation.
    Additional Material: 4 Ill.
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  • 119
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 438-442 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The measurement of transmission is an often used measuring principle in technology. The evaluation algorithms of fluctuating transmission signals are well known in the case of single particle measurement. By evaluating fluctuating transmission signals the particle characterization is also possible at high particle concentrations (0.01 to 30 vol.-%). In comparison with conventional photometers a significant gain of information can be received. Fluctuating signals are caused by the statistical probability of a limited number of particles being present in a defined measuring volume. The evaluation of such signals allows the determination of particle concentration, particle size of monodisperse particles (extinction diameter) and information about structure of agglomerates independent from each other. Mathematical fundamentals and practical ways to measure these parameters are shown. Experimental results are examplarily presented for monodisperse, polydisperse and agglomerated suspensions.
    Additional Material: 8 Ill.
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  • 120
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996) 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 121
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Carefully directed investments to reduce the thermodynamic losses in critical subsystems often leads to a reduction of the overall investment costs. This is demonstrated by recent developments in the technology of low temperature refrigeration. By replacing the Joule-Thomson valve by a work extracting expander and other modifications of the cycle, operating costs are reduced by 40% and investment costs by 20%.
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  • 122
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    Weinheim : Wiley-Blackwell
    Chemical Engineering & Technology - CET 19 (1996), S. 503-509 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: For highly viscous products, multiple shaft agitators represent an interesting alternative to expensive special mixers. A triple shaft agitator with a volume of 250 liters is used to determine the powder consumption of the impellers and its relationship with the process parameters. The result shows that the power consumption of a single impeller running in multiple shaft mode is significantly smaller than of one running in single shaft mode. But the power required for the whole multiple shaft machine is much higher than that for a single shaft machine. A model is presented for detailed description of the interactions between the individual agitators in multiple shaft mode.
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  • 123
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    Chemical Engineering & Technology - CET 19 (1996), S. 538-542 
    ISSN: 0930-7516
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A Comparative study of different Lewis acids (metal chlorides of valences, I, II, III, IV) has been made. These catalysts are used in the synthesis of a high molecular weight ester in a stirred tank reactor using octanoic acid and n-octyl alcohol as reactants. It was found that the best efficiency of the formatted ester (n-octyl octanoate) was obtained with ferric chloride. This could be explained by the high electronegativity and the existence of free d orbitals in the Lewis acid.
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  • 124
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996), S. 205-216 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The results of recent researches on twin-fluid atomization are briefly reviewed, with particular emphasis on the effects of air and liquid properties on mean drop size. It is stressed that no single equation for the mean drop sizes produced in twin-fluid atomization can satisfactorily correlate all the experimental data from any given atomizer. This is because for all types of atomizers the mechanism of liquid breakup changes from one basic mode to another with changes in atomizer operating conditions and/or liquid properties. These different modes of atomization exhibit different dependencies on atomizer dimensions and various physical properties such as liquid viscosity and air density. Equations for estimating the mean drop sizes produced in the various modes of twin-fluid atomization are presented and discussed.
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  • 125
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    Weinheim : Wiley-Blackwell
    Particle and Particle Systems Characterization 13 (1996) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 126
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    Particle and Particle Systems Characterization 13 (1996), S. 260-263 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: The avalanching behaviour of two coal types was determined, one of good and the other of poor handleability characteristics. This revealed significant differences in the nature of flow of the coals. Analysis of the strange attractors of the weight series of avalanches enabled quanitification of this difference, and the establishment of practical, relative criteria for the measurement of coal handleability. These criteria will now enable a structured study of the variables that affect handleability, for example proportion of fines and moisture content, and industrial consumers of coal to specify minimum acceptable limits for its transport characteristics.
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  • 127
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    Particle and Particle Systems Characterization 13 (1996), S. 249-253 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A concern about all reinforcing fibers is the extent to which they are respirable. The degree of respirability of a particle is frequently estimated in terms of its aerodynamic equivalent diameter being less than a certain value (typically 3.5 to 7 μ). However, the aerodynamic equivalent diameter, like the Stokes diameter, is only defined exactly for spheres, which is far from the shape of acicular fibers. Thus, it is useful to be able to calculate, based on actual fiber diameter and aspect ratio, the effective Stokes and aerodynamic equivalent diameters of various fibers. The present paper derives simple expression for relating the two effective diameters to actual fiber dimensions.Calculated results are compared with experimental data for glass fiber and three fractions of phosphate fiber [1], which is a short, reinforcing inorganic fiber. Agreement is seen to be good. Phosphate fiber was fractionated using a sedimentation technique described in the paper. The resulting fractions were characterized by semi-manual measurements of micrographic dimensions and compared with results obtained from particle size instruments based on sedimentation principles. Based on these results, a large weight fraction of phosphate fiber is predicted not to be respirable.
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  • 128
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    Particle and Particle Systems Characterization 13 (1996), S. 254-259 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: When properly measured and interpreted angle of repose (AOR) can be a useful method of characterising a powder. Unfortunately, a multitude of definitions and measuring equipment is used. A review of the inherent problems is presented in the first part of this paper.The second part of the paper describes the improvements made to a measuring device developed originally for measuring the angle of repose of soda ash, so that a wider range of powders can be tested. In the improved design, the tendency of cohesive and semi-cohesive powders to block the device's funnel has been eliminated.A total of 73 powders consisting of four different materials, and covering Groups A, A/C and C of Geldart's classification, have been tested using the new equipment. The results show that AOR increases systematically with decrease in mean particle size. Combination of AOR measured in the new device with aerated bulk density provides a quick, sensitive and effective method for characterising a wide range of powders.
    Additional Material: 8 Ill.
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  • 129
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    Particle and Particle Systems Characterization 13 (1996) 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 130
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    Particle and Particle Systems Characterization 13 (1996), S. 269-269 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 131
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    Particle and Particle Systems Characterization 13 (1996), S. 268-268 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Type of Medium: Electronic Resource
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  • 132
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    Particle and Particle Systems Characterization 13 (1996), S. 271-279 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper gives a theoretical basis for calculating Fraunhofer diffraction patterns of arbitrary polyhedron particles. It is shown that this solution can be used for calculating a scatter matrix adapted to the particle shape in a straightforward manner. Some simulations were made to show the difference between the size distribution by volume obtained with a scatter matrix for spheres and with that for the appropriate shape. Finally, some experimentally measured signatures from platelets and rods are evaluated in order to show that the spherical equivalent diameter could be accurately retrieved.
    Additional Material: 10 Ill.
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  • 133
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    Particle and Particle Systems Characterization 13 (1996), S. 287-290 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Many different methods for size measurement are known and since they differ in their physical principles, different results are also obtained. In the recent past, there were rapid developments in new measurement techniques and one can now quickly and routinely determine particle sizes in the very fine range. Smaller particle sizes, on the other hand, tend to increase the probability of agglomeration. The measurement of the particle sizes for magnetic materials is not well understood and this paper reports results regarding the size determination of very fine magnetic materials. Because of their dipole moment, these particles tend to agglomerate even more, which in turn causes certain difficulties during the measurements. Wet and dry laser measurement systems were compared and also magnetic materials with different permeabilities in order to establish the influence of individual factors on the measurement process and on the accuracy of the results obtained.
    Additional Material: 7 Ill.
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  • 134
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    Particle and Particle Systems Characterization 13 (1996), S. 280-286 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Within the past 20 years, particle size analysis with laser diffraction (LD) has been subject to rapid development, extending the size range stepwise from 1-200 μm to about 0.1-3500 μm. The limits of LD are discussed in terms of light sources, the influence of the beam diameter, special Fourier optics and a new detector design.It is shown that the size range is not only restricted by the wavelength of the laser and the transmission limits of the medium. Its extension is mainly related to improvements in the measurement of the angular intensity distribution. Influences from stability and flow dominate on the coarse side of the measuring range. On the fine side, the spatial extension of aerosols and the resulting demand for extended working distances can be covered only in a parallel laser beam. Extended Fourier optics in combination with an adapatable beam expansion technique and a detector with virtual borders between semicircular elements overcome the existing limits and extend the size range to a lower limit of about 0.05 μm and an upper limit above 10 mm.The sensititivity limit of LD is approaching that of single particle counting techniques. For medical spray and inhaler applications, a 0.1% optical concentration can be converted to particle size distributions even for time-resolved analyses with sample intervals of a few milliseconds.The reproducibility of the sensor, with a standard deviation typically much less than 0.5%, is no longer the limiting factor. The reproducibility of the results is mainly dominated by the reproducibility of sampling, sample splitting, dispersion and the contamination of the optical path. The latter can be improved by the control of flow, especially for in-line and inhaler applications.
    Additional Material: 12 Ill.
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  • 135
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    Particle and Particle Systems Characterization 13 (1996), S. 291-294 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Dynamic light scattering has become a standard technique of investigating colloidal suspensions and polymer solutions. The experimental field autocorrelation function ĝ1 (t) can often be well modelled by a Laplace transform relating ĝ1 (t) to a distribution of decay times A(τ). In simple systems A(τ) can usually be directly related to a distribution of molecular weights, particle sizes, diffusion coefficients or other physically relevant quantities, With constrained regularization methods, the parameter-free estimation of A(τ) has become straightforward. In complex systems, the resulting A(τ) may contain several components the identification of which is not always obvious. The problem often originates in a superposition of diffusive and angle-independent components that have different variations of their respective decay times with the scattering vector. A method is presented based on a simultaneous fit of several autocorrelation functions measured at several different scattering angles, which, using simple and reasonable assumptions, yields a robust analysis of the spectra of decay times. The application of the method is illustrated on simulated autocorrelation functions and also on real experimental data obtained on a variety of different polymer systems.
    Additional Material: 5 Ill.
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  • 136
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    Particle and Particle Systems Characterization 13 (1996), S. 295-300 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A light-scattering instrument that is normally used for particle size analysis was applied to obtain information about particle shape. Micro-cuboids of dimensions a × b × c in the range between 10 and 1000 μm, which can be accurately manufactured employing special technology, were used as labelled samples for the determination of 3-D features. Particle projections at different orientations due to turbulent motion were measured sequentially. The laser diffraction of cuboids rotating in a turbulent flow is described theoretically using a simplified model, i.e. rotation of a rectangle. The change in the projection areas of rotating cuboids is connected with their rotational velocity. The power spectrum density of rotational velocity of cuboids and spheres was determined and the influence of particle shape on the power spectrum density established. The frequency distribution of projection sizes was found to be suitable for particle shape estimation.
    Additional Material: 7 Ill.
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  • 137
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    Particle and Particle Systems Characterization 13 (1996), S. 339-339 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 138
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    Particle and Particle Systems Characterization 13 (1996), S. 333-338 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: This paper describes the use of a capacitance tomography system for imaging gas bubbles in a fluidized bed in the vicinity of an air distributor plate. The results show how the solid concentration distribution varies as a function of time for three different flow regimes: bubbling, slugging and the transition to turbulent. Bubble shape, Length and coalesence can be observed. A method of spatial correlation to elucidate the bubble formation process is described.
    Additional Material: 11 Ill.
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  • 139
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    Particle and Particle Systems Characterization 13 (1996), S. 368-373 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: It is well established that particle size and shape substantially influence the bulk properties of powdered materials. Although these characteristics are closely interrelated, the tendency has been to analyse the particle size independently from particle shape. The aim of this work was the assessment of particle shape through particle sizing data. For this purpose, three different particle shape materials - glass beads (spherical), crushed glass (moderately irregular) and mica (lamellar) - were tested, employing four particle sizers. The shape factor selected was the Wadell's sphericity, which was evaluated utilizing distinct equations. The comparison of the results reveals problems arising from the use of approximations rather than more fundamental equations.
    Additional Material: 1 Ill.
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  • 140
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    Particle and Particle Systems Characterization 13 (1996), S. 381-382 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 141
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    Particle and Particle Systems Characterization 13 (1996), S. 379-380 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 142
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    Particle and Particle Systems Characterization 13 (1996), S. 374-378 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A phenomenological model with 12 parameters for rotary drum granulation with the help of material balance equations taking into account the growth and death functions was developed. Experiments were conducted and the data were used to obtain model parameters with reference to the operating conditions and for validation of the model. It was concluded that the proposed model is adequate for the representation of dynamics and hence this model can be recommended for dynamic simulation leading to improved control of granulation circuits.
    Additional Material: 3 Ill.
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  • 143
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    Particle and Particle Systems Characterization 13 (1996), S. 2-2 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
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  • 144
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    Particle and Particle Systems Characterization 13 (1996), S. 3-9 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A novel technique to determine the size of particles suspended in a stirred vessel is investigated. The method uses microphotography to obtain a still image of the particles in situ. The equivalent circular diameter of the particles is obtained from the photographs using digital image analysis. The particles used for the test were certified particle size standards of a very small tolerance in diameter deviation. The size comparison was determined as a percent error between the measured particle diameter (equivalent circular diameter) and the diameter established by the particle manufacturer. To determine the limiting ranges of particle size and concentrations, spherical particles in a size range of approximately 1 to 10.0 μm (microns) in diameter were employed in the test. Concentrations varied from 0.00005% to 0.1% (mass basis). For each particle size, an aqueous solution of the particles was prepared at the desired concentration and placed in a stirred vessel. Photographs of the solutions were made at 25.5x, 40x, 60x and 80x magnification. For all sizes of particles, the entire range of concentration was examined.The results indicate a minimum size resolution of approximately 3μm, in a corresponding concentration range of 0.0001% to 0.05%. Similar limits on concentration were found for the larger diameter particles, although a true upper limit for the largest particle sizes was not established. The functional concentration range appears to shift towards higher mass concentrations with increasing particle size. For 2.92 μm diameter particles, the error in size measurement was found to be below 10% for a concentration range of 0.0005% to 0.05%. Additionally, a relationship between turbidity and the error was seen at low particle concentration levels where decreasing levels of turbidity generated increasing levels of error.
    Additional Material: 8 Ill.
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  • 145
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    Particle and Particle Systems Characterization 13 (1996), S. 27-33 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A new phase Doppler anemometry (PDA) signal processing method based on a Hilbert transform algorithm is introduced and analysed. By generating a 90° phase-shifted burst signal in the time domain, the envelope of the Doppler burst can be determined. In addition, this envelope is approximated by a Gaussian exponential function. The difference of the maxima of these Gaussian approximations for two related PDA bursts gives an estimate of the time difference between these time shifted signals. With the introduction of this estimation method, the restriction to the [0,360°] interval resulting from conventional signal analysis may be avoided in many cases. To investigate the dependence on SNR, burst position, burst frequency and sampling rate, results of computer simulations are presented. The feasibility of the method is demonstrated briefly by experimental results. Phase differences of more than 2000° arising from the measurement of monodisperse droplets by a conventional PDA setup could be determined.
    Additional Material: 8 Ill.
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  • 146
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    Particle and Particle Systems Characterization 13 (1996), S. 130-136 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Using a monodisperse poly(methyl methacrylate) dispersion it was shown that light reflection at the sample cuvette walls may greatly influence the results of both static (SLS) and dynamic (DLS) light scattering experiments. Considering SLS, this reflection phenomenon mostly causes an overestimation of the scattered intensity at high scattering angles, which may give rise to the emergence of an additional, artificial peak in the lower region of the particle size distribution. On the other hand, the influence of reflection on DLS experiments was shown to be particularly important in the upper region of the particle size distribution. The experimentally observed phenomena were explained from basic principles of both particle sizing methods. Finally, it was shown that the disturbing effect of reflection could be avoided by modifying either the hardware or the software of the SLS and DLS techniques.
    Additional Material: 9 Ill.
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  • 147
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    Particle and Particle Systems Characterization 13 (1996), S. 137-142 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: An instrument is proposed for the visualisation and measurement of mixtures of small and large particles. The original concept was to use spectral extinction for sub-micron particles and scattering patterns for larger sizes. However, the former method is sensitive to the refractive index, which may be unknown or vary with wavelength in an unknown way. The experiments demonstrated this to be a problem. The forward scatter, on the other hand, is not so sensitive to this. It is shown here that the combination of scattered intensity as a function of both angle and Wavelength provides scatter diagrams for which there is good agreement between theory and experiment. The influence of quite small volume fractions of particles as small as 0.3μm mixed with 90μ particles is easily seen. The scatter diagrams suggest the use of image analysis for size measurement and quality control.
    Additional Material: 8 Ill.
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  • 148
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    Particle and Particle Systems Characterization 13 (1996), S. 143-149 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A planar phase Doppler system is used to measure submicron droplets generated by an electrospray. Measured drop dia-meters are correlated with the liquid properties and the condition for transition of the spray from the single-jet mode to the multi-jet mode is introduced. In another set of measurements using a standard phase Doppler system, combined size and velocity data are employed to deduce the drag force on the drops. In a situation where the drag force is balanced primarily by the electric force, the phase Doppler measurements allow to estimate the power-law relationship between the charge on a drop and its diameter and hence, many provide insights into the underlying atomization mechanisms.
    Additional Material: 9 Ill.
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  • 149
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    Particle and Particle Systems Characterization 13 (1996), S. 150-155 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Only a few optical techniques are available to measure simultaneously the velocity and size of coarse particles dispersed in a fluid. Since particles are randomly shaped with a rough surface and inhomogeneous with respect to the refractive index, phase-based sizing techniques are not reliable. The applied optical sizing technique is based on light intensity measurement of a scattering particle crossing a top-hat laser beam. This optical set-up was first described by Gréhan et al. In the range of geometrical optics, the sampled light at the receiving system is proportional to the square of the equivalent particle diameter within the diameter range 20-700 μmVelocity information is obtained by using a smaller concentric laser Doppler probe volume. Coincidence of the signals is guaranteed by the optical set-up, since the smaller probe volume diameter defines the triggering event. To demonstrate the performance of the system, some diameter distributions measured with the top-hat beam system are compared with results for a commercial laser diffraction system for different materials. The system is applied to obtain size-correlated velocity information of a particle-laden two-phase flow at a single-sided backward-facing step.
    Additional Material: 14 Ill.
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  • 150
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    Particle and Particle Systems Characterization 13 (1996), S. 156-164 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: Imaging techniques in particle sizing have always been important. Nevertheless, owing to the progress in CCD cameras, these techniques have found new potential which strongly depends on the capability to describe the image formation. Based on a combination of the generalized Lorenz-Mie theory and the diffraction theory, the image characteristics are described, taking into account the beam size, particle location, direction of observation and collecting optics characteristics. In the case of forward detection, a finite coherence is introduced and the results are compared with those obtained by a convolution approach, with the point spread function assumed to be Gaussian. Then some experimental results are displayed which underline the improvement achieved in particle size measurement.
    Additional Material: 20 Ill.
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  • 151
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    Particle and Particle Systems Characterization 13 (1996), S. 196-204 
    ISSN: 0934-0866
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Process Engineering, Biotechnology, Nutrition Technology
    Notes: A Diesel spray injected into a high-pressure test chamber was investigated with two different holographic techniques. The usual off-axis recording geometry was used to investigate the very early beginning of the injection. Double pulsing of the recording laser facilitated velocity measurements. By using two different reference angles for the two recording the two images can be separated upon reconstruction of the holograms. Thus superior image quality could be achieved. Processes leading to jet formation could be identified: the spray tip is periodically axially decelerated and radially accelerated. Consequently, liquid moves at the tip off axis. The spray consists of fast central region surrounded by a slower outer jet region. The outer jet region exhibits periodic droplet concentration fluctuations which are interpreted as a result of the periodic processes at the spray tip. Some high concentration regions in the outer jet region were investigated using a dark-field holographic technique. This technique permits single droplet velocity measurements and local droplet concentration determination at extremely high droplet concentrations. The most important result of these investigations is that no correlation between the local droplet concentration and the droplet velocity could be found.
    Additional Material: 18 Ill.
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  • 152
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    Applied Organometallic Chemistry 10 (1996), S. 75-75 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
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  • 153
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    Applied Organometallic Chemistry 10 (1996), S. 13-22 
    ISSN: 0268-2605
    Keywords: arsenic-containing ribofuranosides ; arsenosugars ; dimethyl(β-D-ribofuranos-5-yl]-arsine ; dimethyl(β-D-ribofuranos-5-yl)arsine sulfides ; trimethyl(β-D-ribofuranos-5-yl)arsonium iodides ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Eight arsenic-containing ribosides were prepared from dimethyl(1-O-methyl1-5-deoxy-2,3-O-isopropylidene-β-D-ribofuranos-5-yl)arsine and (2′S)-dimethyl[1-O-(2′,3′-isopropylidenedioxypropyl)-5-deoxy-2,3-O-isopropylidene-β-D-ribofuranos-5-yl]arsine. Reactions of the arsines with sulfur produced the compounds with a (CH3)2As &= S group as substituent in the 5-position. Treatment of these dimethyl(ribosyl)arsine sulfides with trifluoroacetic acid water removed the isopropylidene groups and gave the unprotected derivatives as thick oils in 80% yield. The arsines and methyl iodide gave the protected trimethyl(ribosyl)arsonium iodides. These arsonium iodides were reacted with trifluoroacetic acid/water. Anomeric mixtures of the deprotected compounds were isolated. Deprotection of the dimethyl(ribosyl)arsines proceeded without anomerization. Reaction of the dimethyl[1-O-(2′,3′-dihydroxypropyl)-5-deoxy-β-D-ribofuranos-5-yl]arsine with methyl iodide produced the pure β-anomer of the arsonium iodide. The yields in these reactions were approximately 80%.
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  • 154
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    Applied Organometallic Chemistry 10 (1996), S. 377-387 
    ISSN: 0268-2605
    Keywords: organotins ; toxicity ; algae ; submicrostructure ; counterions ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The inhibition by 20 organotin compounds (RnSnX4-n), which included some newly synthesized pesticides, of the growth of two green algae (Scenedesmus obliquus and Platymonas sp.) was studied. The influence of the counterion X group on the toxicity of organotins was discussed. The destruction of submicrostructures of the algal cell by organotins was viewed by micrography and electron microscope scanning. It was found that the toxicity of the organotins varied significantly according to their substitution. The order of toxicity is tri- ≫ di- ≥ mono-organotins. Within the same substituent series, the toxicity depends on the properties of both R and X groups. The larger and the more lipophilic the R group, the more toxic is the organotin. The influence of the X group is more complex: when X is a small easily ionizable group, it has little effect on the toxicity; however, when it is a large organic group, it does change the bioactivity of the organotin. Large organic groups may influence the polarizability of the central tin atom, and so change the toxicity of organotins.
    Additional Material: 12 Ill.
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  • 155
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    Applied Organometallic Chemistry 10 (1996), S. 317-337 
    ISSN: 0268-2605
    Keywords: organotin compounds ; tin ; speciation ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The growing awareness over the environmental fate of organotin compounds is reflected in the large number of analytical methods developed for their separation. Organotin compounds have varying degrees of toxicological properties, depending on the nature and number of alkyl groups bonded to the tin atom. Most of the analytical speciation methods applied to actual environmental media have involved prior derivatization to transform organotin compounds into volatile hydrophobic analytes amenable to separation and identification by gas chromatography coupled to a sensitive and selective tin-detector. Evidence exists that members of the same homologous series are related by environmental degradation pathways. Chemical treatment prior to analysis, or high temperatures associated with gas chromatography separation, may alter the relative amounts of organotins in samples and blur the true environment picture. To avoid species redistribution that may occur during derivatization or gas speciation analysis, methods based on liquid chromatography and supercritical fluid chromatography have been investigated. This review documents analytical methods for determination of tin and speciation of organotin compounds, in the hope that it will be of value to those interested in initiating a programme for assessing the impact of such species on the environment.
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  • 156
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    Applied Organometallic Chemistry 10 (1996), S. 389-392 
    ISSN: 0268-2605
    Keywords: regiospecific lithiation ; 2-furoic acid ; 5-ethyl-2-furoic acid ; butyl-lithium ; lithium di-isopropylamide (LDA) ; furonaphthoquinone ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Treatment of 5-ethyl-2-furoic acid with n-butyl-lithium in tetrahydrofuran gave regiospecific C-3 lithiation, whereas treatment of the same acid with lithium di-isopropylamide (LDA) afforded only starting material. The synthetic utility of dilithiated 5-ethyl-2-furoic acid has been demonstrated with the synthesis of two substituted 3-benzyl-5-ethyl-2-furoic acid derivatives which are key intermediates for the preparation of naturally occurring cytotoxic 2-ethylfuronaphthoquinones. Reaction of the C-3 lithiated species with two equivalents of benzaldehyde and subsequent reduction affored the corresponding 3-benzyl-5-ethyl-2-furoic acids. An alternative route to 5-ethyl-2-furoic acid has been described allowing for a more convenient preparation of longer-chain 5-alkyl-2-furoic acids.
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  • 157
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    Applied Organometallic Chemistry 10 (1996), S. 683-688 
    ISSN: 0268-2605
    Keywords: inorganic arsenic ; methanearsonic acid ; dimethylarsinic acid ; tetramethylarsonium salt ; arsenocholine ; microorganisms ; conversion ; degradation ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Sediments, as sources of microorganisms, were added to two kinds of media, 1/5 ZoBell 2216E and a solution of inorganic salts, which contained inorganic arsenic(III), inorganic arsenic(V), methanearsonic acid, dimethyl- arsinic acid, trimethylarsine oxide, tetramethylarsonium salt or arsenocholine. After 17 days of incubation at 20 °C, the arsenicals that had accumulated in the microorganisms were analysed by high-performance liquid chromatography (HPLC). While the more toxic arsenicals [inorganic arsenic(III), inorganic arsenic(V), methanearsonic acid, dimethylarsinic acid] were not converted in the microorganisms, trimethylarsine oxide and tetramethylarsonium salt were considerably degraded to inorganic arsenic(V), and arsenocholine to arsenobetaine. Arsenobetaine that had accumulated in the microorganisms was extracted and confirmed by thin-layer chromatography (TLC) and fast atom bombardment (FAB) mass spectrometry.
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  • 158
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    Applied Organometallic Chemistry 10 (1996), S. 667-674 
    ISSN: 0268-2605
    Keywords: geochemical ; groundwater ; arsenic ; aquifer ; wells ; depth ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The geochemical behavior of arsenic-bearing groundwaters from four areas - Fukuoka, Kumamoto, Fukui, and Takatsuki - has been reviewed and considered from the viewpoints of the chemical composition of the water, the geological setting of the host formation, and the arsenic content in sediments and rocks. In all the areas except Fukui, arsenic-bearing water is concluded to have come from a specific aquifer during water-sediment interactions. Stagnant groundwater, having reducing and alkaline properties, played a significant role in the release of arsenic from such Quaternary sediments as silt-clay layers and brownish-colored gravel beds.
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  • 159
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    Applied Organometallic Chemistry 10 (1996), S. 727-732 
    ISSN: 0268-2605
    Keywords: immunotoxicity ; arsenocholine ; arsenobetaine ; tetramethylarsonium ion ; macrophages ; lymphocytes ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: In the present study, we demonstrated for the first time the immunotoxic effects of organic arsenic compounds in marine animals, namely arsenocholine [AsCho; trimethyl(2-hydroxyethyl)arsonium cation], arsenobetaine [AsBe; the trimethyl(carboxymethyl)arsonium zwitterion] and the tetramethylarsonium ion (TetMA), to murine principal immune effector cells (macrophages and lymphocytes), comparing them with the effects of inorganic arsenicals in vitro. Inorganic arsenicals (arsenite and arsenate) showed strong cytotoxicity to both macrophages and lymphocytes. The concentration of arsenite that reduced the number of surviving cells to 50% of that in untreated controls (IC50) was 3-5 μmol dm-3, and the cytotoxicity of arsenate (IC50=100 μ-1 m mol dm-3) was lower than that of arsenite. Compared with these findings, trimethylarsenic compounds in marine animals, AsCho and AsBe, were less toxic even at a concentration over 10 mmol dm-3 to both macrophages and lymphocytes; however, TetMA had weak, but significant, cytotoxicity to these cells (IC50 was about 6 mmol dm-3).
    Additional Material: 5 Ill.
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  • 160
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    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 161
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    Applied Organometallic Chemistry 10 (1996), S. 795-796 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
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  • 162
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    Applied Organometallic Chemistry 10 (1996), S. 779-790 
    ISSN: 0268-2605
    Keywords: organotin ; N-acetyltriglycine ; N-benzoyltriglycine ; Mössbauer ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Di- and tri-organotin(IV) derivatives of N-acetyltriglycine and N-benzoyltriglycine (HA) were obtained by refluxing equimolar mixtures of the ligand and the organotin(IV) oxide or hydroxide in methanol or acetone. According to the spectroscopic data, triorganotin(IV) derivatives adopt a trigonal-bipyramidal structure in which the planar R3SnIV unit is bonded by a monodentate carboxylate group and a donor group, presumably the amide C=O. The reaction of HA with the appropriate diorganotin(IV) compounds gave both dicarboxylates R2SnA2, with six-coordinated tin, and dimeric tetraorganodistannoxanes {[R2SnA]2O}2, in which the tin atoms are essentially five-coordinated.
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  • 163
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    Applied Organometallic Chemistry 10 (1996), S. 267-278 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
    Additional Material: 11 Ill.
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  • 164
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    Applied Organometallic Chemistry 10 (1996), S. 579-590 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
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  • 165
    ISSN: 0268-2605
    Keywords: arsenic-containing ribofuranosides ; arsenosugars ; (2′R)-dimethyl[1-O-(2′,3′-dihydroxypropyl)-5-deoxy-β-D-ribofuranos-5-yl]arsine oxide ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Six arsenic-containing β-D-ribofuranosides, including the naturally occurring (2′R)-dimethyl[1-O-(2′,3′-dihydroxypropyl)-5-deoxy-β-D-ribofuranos-5-yl]arsine oxide, were prepared in multi-step reactions from D-ribose and tetramethyldiarsine. The synthetic procedure uses the early substitution of the hydroxy group with bromine at C5, subsequent attachment of a chiral three-carbon aglycone at C1, and final delivery of arsenic at C5. The synthesis provides a viable route for the preparation of multigram quantities of the natural product.
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  • 166
    ISSN: 0268-2605
    Keywords: organotin ; pyrimidin-4-one derivatives ; complexes ; cytotoxicity ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The coordination behaviour of the diorganotin (IV) compounds R2SnCl2 (where R = Me, Ph) with 4H-pyrido [1,2-a] pyrimidin-4-one derivatives (L) has been described. The complexes R2SnCl2 · L obtained have been characterized physicochemically and spectroscopically. The pyrimidin-4-one ligands were found to coordinate with R2SnCl2 species in a monodentate fashion, mainly via the oxygen atom of the 4-one group or possibly via the nitrogen atom of the (SINGLE BOND)C(DOUBLE BOND)N linkage (the less sterically hindered nitrogen of the pyrimidine derivative) to give pentacoordinate tin complexes. Of the complexes selected to be screened against five tumour cell lines, some exhibited significant in vitro activity.
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  • 167
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    Applied Organometallic Chemistry 10 (1996), S. 69-73 
    ISSN: 0268-2605
    Keywords: trimethyl-lead ; reference material ; homogeneity ; stability ; rainwater ; road dust ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: This study was conducted to develop certified reference materials containing trimethyl-lead (TriML) in environmental matrices. A detailed description of the process to prepare candidate artificial rainwater and road dust reference materials, which includes pretreatment, homogenization and bottling procedures, is described. The homogeneity was assessed by comparing the variations within a bottle and between different bottles. The results demonstrated that the distribution of TriML in the same material is homogeneous. The stability of TriML in these materials was verified on the day of preparation and after 1, 3, 6 and 12 months. The results showed no significant difference between the initial TriML concentration and the concentration after 12 months' storage in candidate artificial rainwater kept at room temperature and in road dust stored at -20°C and 4°C, based on a statistical analysis of the results. At 37°C, however, TriML was shown to be unstable: this highlighted the need to store the materials in the dark, preferably at 4°C. TriML in both of the candidate reference materials was hence concluded to be stable for at least 12 months under the appropriate storage conditions.
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  • 168
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    Applied Organometallic Chemistry 10 (1996), S. 795-795 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
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  • 169
    ISSN: 0268-2605
    Keywords: selective reduction ; carbonyl compound ; sodium hydrogentelluride ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Aromatic aldehydes or ketones which have electron-withdrawing groups on the benzene ring were selectively reduced to the corresponding alcohols in good yields by sodium hydrogentelluride; common aldehydes such as benzaldehyde and tolualdehyde were inert.
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  • 170
    ISSN: 0268-2605
    Keywords: organolanthanide ; alkylaluminium ; bimetallic complex ; NMR spectra ; polymerization ; single-component catalyst ; epichlorohydrin ; methyl methacrylate ; tetrahydrofuran ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Three new lanthanide (Ln)-alkylaluminium (Al) bimetallic complexes with the formula [(μ-CF3CO2)2Ln(μ-CF3CHO2)AlR2 · 2THF]2 (Ln=Nd, Y, R=i-C4H9 (i-Bu); Ln=Eu, R=C2H5(Et); THF=tetrahydrofuran) were synthesized by the reaction of Ln(CF3CO2)3 (Ln=Nd, Y) with HAl (i-Bu)2 and of Eu(CF3CO2)3 with AlEt3, respectively. Their crystal structures were determined by X-ray diffraction at 233 K. [(μ-CF3CO2)2Nd (μ-CF3CHO2)Al(i-Bu)2 · 2THF]2 (Nd-Al) and [(μ-CF3CO2)2Y(μ-CF3CHO2)Al(i- Bu)2 · 2THF]2 (Y-Al) are isomorphous and crystallize in space group P1 with a=12.441(3) Å [12.347(5) Å for Y-Al], b=12.832(3) Å [12.832(4) Å], c=11.334(3) Å [11.292(8) Å], α=104.93 (2)° [104.45(4)°], β=98.47(2)° [98.81(4)°], γ=64.60(2)° [64.30(3)°], R=0.519 [0.113], Rw=0.0532 [0.110], Z=1 and [(μ-CF3CO2)2Eu(CF3 CHO2)AlEt2 · 2THF]2(Eu-Al) in space group P21/n with a=11.913(6) Å, b=14.051(9) Å, c=17.920(9) Å, α=101.88(11)°, β=γ=90°, R=0.0509, Rw=0.0471 and Z=2. The six CF3CO-2 (including CF3CHO-2) of each complex, among which pairs are equivalent, coordinated to Ln and Al in three patterns: (A) the two oxygen atoms in one of the three CF3CO-2 type coordinated to two different Ln; (B) the two oxygen atoms in the second of CF3CO-2 type coordinated to Ln and Al, respectively; (C) one of the two oxygen atoms in the third CF3CO-2 type bidentately coordinated to two Ln and another oxygen coordinated to Al and one of the two Ln, respectively. Unlike types A and B, in type C the carboxyl carbon with a hydrogen atom bonded to it was found to appear as an sp3-hybridized configuration rather than an sp2-one. 1D and 2D NMR results further confirmed the existence of such a disproportionated CF3CHO-2 ligand. Methyl methacrylate (MMA) and epichlorohydrin (ECH) could be polymerized by Y-Al or Eu-Al as a single-component catalyst and highly syndiotactic poly(MMA) was obtained. THF could also be polymerized by Y-Al in the presence of a small amount of ECH.
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  • 171
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    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 172
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    Applied Organometallic Chemistry 10 (1996), S. 83-99 
    ISSN: 0268-2605
    Keywords: laser ; chemical vapour deposition ; thin films ; Si/C/H materials ; silacyclobutane ; 1,3-disilacyclobutane ; silicon carbide ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: CO2 laser-induced infrared multiphoton decomposition (IRMPD) and SF6 photosensitized decomposition (LPD) of silacyclobutane (SCB) and 1,3-disilacyclobutane (DSCB) in the gas phase results in the very efficient deposition of Si/C/H and SiC materials, and it is inferred that the process is dominated by formation of transient silene; silene rearrangement to methylsilylene; silene and methylsilylene dehydrogenation; and polymerization of SiCHn (n 〈 4) species. The deposits are sensitive to oxygen.Decomposition and SiC formation are favoured with IRMPD experiments conducted with high-energy fluxes. The laser technique is promising for low-temperature chemical vapour deposition of amorphous SiC.
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  • 173
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    Applied Organometallic Chemistry 10 (1996), S. 77-82 
    ISSN: 0268-2605
    Keywords: gas chromatography ; flame photometric detector ; quartz tube ; butyltin species ; water analysis ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A flame photometric detector using quartz surface-induced tin emission was designed and evaluated for quantification analysis of butyltin species. It has been demonstrated that this quartz surface-induced tin emission, centred at 390 nm, is more sensitive than the commonly used gas-phase emission at 610 nm. The dependence of detector response on quartz enclosure was studied. The operational variables such as hydrogen-air flow rate, carrier-gas flow rate and purge-gas flow rate were optimized. An analytical procedure for speciation analysis of butyltin species in water using simultaneous hydride generation with sodium borohydride and extraction into dichloromethane was established. The detection limits (defined as the signals that equal three times the deviations of the noise) were 0.3 pg of Sn for tetrabutyltin (TeBT), 5 pg of Sn for monobutyltin (MBT), 18 pg of Sn for dibutyltin (DBT) and 2 pg of Sn for tributyltin (TBT), which are approximately 10- to 30-fold better than those reported for using more commonly used gas-phase emission centred at 610 nm.
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  • 174
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    Applied Organometallic Chemistry 10 (1996), S. 537-544 
    ISSN: 0268-2605
    Keywords: Methylmercury ; sediment ; interlaboratory study ; performance evaluation ; improvement ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The results are presented of an interlaboratory study on methylmercury (MeHg) in sediment carried out by a group of European laboratories within the framework of a project managed by the EC Standards, Measurements and Testing Programme (formerly BCR). The aim of this exercise was to evaluate the performance of current methods used for MeHg determination in sediment in order to improve the state-of-the-art prior to the certification of a candidate reference material. The paper describes the organization of the interlaboratory study, the preparation of the sediment material used, the techniques evaluated and the results obtained by the participating laboratories. The outcome of the collaborative project showed that certification could be contemplated, providing that certain analytical techniques were optimized, especially with regard to extraction methods.
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  • 175
    ISSN: 0268-2605
    Keywords: organotin biscarboxylates ; distannoxanes ; coordination bonds ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Several di-n-butyltin and diethyltin biscarboxylates and distannoxanes of α-methoxy- and α-acetoxy-phenylacetic acids were synthesized and (two of) their structures were studied by means of X-ray diffraction analysis as well as by means of IR and Mössbauer spectroscopies. It was shown for {[(n-Bu)2-SnOC(O)CH(OMe)Ph]2O}2 that there is an interaction between the OMe group and one of the endocyclic tin atoms, resulting in a distorted pentagonal-bipyramidal geometry with the pentagonal plane defined by five O atoms and an uncommon seven coordination number for this tin atom. Spectral data indicate that biscarboxylates have trans-octahedral structures.
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  • 176
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    Applied Organometallic Chemistry 10 (1996), S. 531-535 
    ISSN: 0268-2605
    Keywords: bile acids ; conjugated bile acids ; trimethylsilyl (TMS) derivatives ; GLC-MS analysis ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The trimethylsilyl (TMS) derivatives of a mixture of nine bile acids (six free and three conjugated), namely lithocholic, deoxycholic, chenocholic, cholic, hyodeoxycholic, ursodeoxycholic, glycodeoxycholic, glycocholic and glycochenodeoxycholic acids, have been prepared by a new, simple, efficient derivatization procedure, based on the use of a mixture of N-methyl-N-trimethylsilyl-1,1,1- trifluoroacetamide and 1-(trimethylsilyl)imidazole, as the silylating agent. The above-mentioned bile acids were completely trimethylsilylated on all hydroxyl and carboxyl groups whereas carbonyl and amino groups remained untouched.
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  • 177
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    Applied Organometallic Chemistry 10 (1996), S. 637-647 
    ISSN: 0268-2605
    Keywords: phthalocyanines ; discotic liquid crystals ; optoelectric materials ; molecular semiconductors ; charge transport ; pulse radolysis ; microwave conductivity ; electron tunneling ; molecular electronics ; molecular wires ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The pulse-radiolysis time-resolved microwave conductivity (PR-TRMC) technique has been used to obtain information on the transport of charge within columnarly stacked, peripherally octaalkoxy-substituted phthalocyanines. Data are presented on the one-dimensional, intracolumnar charge mobility and on the timescale of quasi-two-dimensional intercolumnar electron tunnelling. Particular attention is paid to materials that are liquid-crystalline at room temperature, because of their potential technological importance in optoelectric charge transport layers and molecular semiconductor devices. The relevance of the data to channeled charge transport in aligned thin layers is discussed.
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  • 178
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    Applied Organometallic Chemistry 10 (1996), S. 199-208 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
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  • 179
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    Applied Organometallic Chemistry 10 (1996), S. 241-256 
    ISSN: 0268-2605
    Keywords: inorganic polymers ; boron ; ceramics ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
    Additional Material: 10 Ill.
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  • 180
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    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
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  • 181
    ISSN: 0268-2605
    Keywords: ceramic precursors ; poly[silylene-co-(2,4-disilapentane-2,4-diyl)] ; polycarbosilanes ; silicon carbide ; fibers ; thermal cross-linking ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Novel oligomers possessing a backbone formed of ((TRIPLE BOND)Si(SINGLE BOND)CH2(SINGLE BOND)Si(TRIPLE BOND)) and (SINGLE BOND)Si(SINGLE BOND)n units were prepared by the copolycondensation of bis(chlorosilyl)methanes and various dichlorosilanes in the presence of sodium, in refluxing toluene. The effect of the respective molar ratios of comonomers on the yields and the structure of the copolymers was investigated. The role of substituents on silicon atoms in the ability of these materials to provide convenient ceramic precursors upon pyrolysis was examined. When (TRIPLE BOND)Si(SINGLE BOND)H bonds were present, thermal cross-linking was readily performed and ceramics possessing variable C/Si ratios were prepared.
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  • 182
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    Applied Organometallic Chemistry 10 (1996), S. 53-59 
    ISSN: 0268-2605
    Keywords: organotin compounds ; liposomes ; fluorescence ; 1,6-diphenyl-1,3,5-hexatriene ; 1-(4-trimethylaminophenyl)-6-phenyl-1,3,5-hexatriene ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The temperature dependence of 1,6-diphenyl-1,3,5-hexatriene (DPH) and 1-(4-trimethylaminophenyl)-6-phenyl-1,3,5-hexatriene (TMA-DPH) fluorescence anisotropy has been studied to investigate the influence of mono-n-butyltin chloride (MBTC), di-n-butyltin chloride (DBTC) and tri-n-phenyl chloride (TPTC) on the physicochemical state of dipalmitoyl phosphatidylcholine. Below the lipid chain melting transition (Tm), fluorescence anisotropy values of DPH and TMA-DPH are increased by the presence of the organotins, without important modifications of the phase transition temperature. A possible difference in localization of the organotin compounds is suggested by the differential effect of the probes. It is suggested that there is localization in the hydrophobic core of the bilayer for TPTC, and at the head-group level for DBTC, and a homogeneous distribution in the bilayer for MBTC. Similar studies have been performed in liposomal suspensions of cardiolipin, phosphatidylserine and egg phosphatidylcholine.
    Additional Material: 3 Ill.
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  • 183
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 101-111 
    ISSN: 0268-2605
    Keywords: ferrocenes ; flame retardancy ; smoke suppression ; PVC ; dehydrochlorination ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A range of substituted ferrocenes has been synthesized and studied for flame retardancy and smoke suppression on incorporation into plasticized PVC at 0.1-5.0 phr. Smoke suppression by up to 50 and enhancement of the limiting oxygen index by up to 4 units were observed. The differences in performance could not be correlated with char formation, thermal analysis or chemical structure of the additive. A negative correlation was found between smoke suppression and flame retardancy. The most effective smoke suppressant additive appears to accelerate the rate of dehydrochlorination of PVC while the most effective flame retardant appears to have little effect on the dehydrochlorination process.
    Additional Material: 6 Ill.
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  • 184
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 135-143 
    ISSN: 0268-2605
    Keywords: organotin ; particle beam ; mass spectra ; LC-MS ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Selected organotin compounds, relating to antifouling paints, have been analysed using a particle beam interface system designed for use on liquid chromatography-mass spectrometry (LC-MS) instruments. The resultant mass spectra matched those obtained from conventional electron-impact (EI) techniques, and consistent data over several injections and different elution times were obtained. Data obtained from tributyltin, dibutyltin, monobutyltin, triphenyltin and diphenyltin (each as the chlorides) are presented. This interface has been shown to maintain sample and therefore spectral integrity for these compounds and is of potential use in further investigations relating to organotin environmental pollution.
    Additional Material: 6 Ill.
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  • 185
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 649-660 
    ISSN: 0268-2605
    Keywords: naphthalocyanine ; ruthenium ; bridged ; oligomers ; solid state ; NMR ; conductivity ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Bridged 2,3-naphthalocyaninatoruthenium oligomers {[MacRu(L)]n} were synthesized and characterized using solid-state methods. For comparison, soluble t-butyl substituted phthalocyaninatoruthenium oligomers were prepared and their chain length examined by 1H NMR spectroscopy. The powder conductivities of all bridged compounds ([MacRu(L)]n) were measured and the dependence of the conductivities on the bridging ligands is discussed.
    Additional Material: 3 Ill.
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  • 186
    ISSN: 0268-2605
    Keywords: chemiluminescence ; ion chromatography ; luminol ; heteropoly acid ; arsenic(V) ; germanium(IV) ; phosphorus(V) ; silicon(IV) ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A flow-injection chemiluminescence (CL) method has been proposed for sensitive determination of arsenate, germanate, phosphate and silicate, after separation by ion chromatography (IC). The post-column detection system involved formation of heteropoly acid in a H2SO4 medium before the CL reaction with luminol in an NaOH medium. For separation, heteropoly acid formation and the CL detection reaction, pH requirements were not compatible. When present as a heteropoly acid complex with molybdenum(VI), ger- manium(IV) and silicon(IV) caused CL emission from oxidation of luminol, and such a CL oxidation of luminol was observed analogously for arsenic(V) and phosphorus(V) but with the addition of metavanadate ion to the acid solution of molybdate. Good sensitivity for the three analytes arsenic(V), ger- manium(IV) and phosphorus(V) could be given by a single set of reagent conditions, chosen carefully. Another set was suitable for determining phosphorus(V) and silicon(IV). The minimum detectable concentrations of arsenic(V), germanium(IV), phosphorus(V) and silicon(IV) were 10, 50, 1 and 10 μg l-1, respectively. Linear calibrations for arsenic(V), germanium(IV), phosphorus(V) and silicon(IV) were established over the respective concentration ranges of 10-1000, 50-25000, 1-1000 and 50-1 μg l-1. The proposed IC-CL method was successfully applied to analyses of a seaweed reference material, rice wine and water samples.
    Additional Material: 3 Ill.
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  • 187
    ISSN: 0268-2605
    Keywords: germathiazolidines ; germadithioacetals ; germylated oxide ; germylated sulfide ; N-substituted cysteamine ; toxicity ; radioprotective activity ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Further to our work concerning organometallic compounds active in chemical radioprotection, we report the synthesis and pharmacological study (radioprotective activity, toxicity) of new germathiazolidines and germadithioacetals derived from cysteamine, methylcysteamine and N-substituted cysteamine. A germylated oxide and sulfide with methylcysteamine hydrochloride as ligand were also investigated.A notable decrease in the toxicity and a fairly large increase in the radioprotective activity of these new organogermylated compounds were observed compared with cysteamine, methylcysteamine and N-substituted cysteamine.
    Additional Material: 10 Ill.
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  • 188
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 189
    ISSN: 0268-2605
    Keywords: Organotin complexes ; base strengths ; J(Sn-C-H) coupling constants ; pKb ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A study by titrimetric methods of the donor strength of pyridine and aniline and some of their para-substituted derivatives, and the J(119Sn-C-H) of their adducts with dimethyltin dichloride in nitrobenzene, has shown that the pKb of a Lewis base and its para-substituted derivatives varies linearly with the J(119Sn-C-H) of the adducts of dimethyltin dichloride (Me2SnCl2), with the Lewis base dissolved in an inert solvent.A graphical plot of the pKb of a given series of Lewis bases versus the J(Sn-C-H) of their complexes with Me2SnCl2 in nitrobenzene (at the same temperature, and same complex concentration) gives a straight line with a negative gradient, making possible the deduction of the other parameter (e.g. pKb) for a Lewis base in the series, where the one parameter (e.g. J(Sn-C-H) is known. The graph for each series of Lewis base has its own characteristic gradient, and the gradients appear proportional in magnitude to the donor strengths of each class of the bases, making it possible to deduce from such graphs which series of Lewis bases are the stronger donors.
    Additional Material: 3 Ill.
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  • 190
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 405-413 
    ISSN: 0268-2605
    Keywords: tributyltin ; embryo toxicity ; ascidians ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The effects of tributyltin(IV) chloride (TBT chloride) have been tested on embryos of the ascidian Ciona intestinalis, at two different stages of development: (1) before hatching (coiled larval stage) and (2) 2 h after hatching (swimming larval stage). In vivo observations carried out with a light microscope showed that embryos at the coiled larval stage did not hatch following exposure to TBT chloride. Severe anomalies in the swimming larva, mainly concerning the morphology of the tail, which appeared twisted and squatter than in the controls, were observed. Such anomalies were also found at a functional level, i.e. contractile movements were poor so that the larvae appeared motionless. Ultrastructural investigations carried out using a transmission electron microscope (TEM) evidenced that the muscle cells were damaged. Modifications mainly occurred in mitochondria and myofibrils, i.e. the energetic and enzymic centres. This fact is probably the main cause of the loss of mobility of the larvae.
    Additional Material: 15 Ill.
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  • 191
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    Applied Organometallic Chemistry 10 (1996), S. 415-420 
    ISSN: 0268-2605
    Keywords: cobaloxime ; radicals ; iodine atom abstraction ; ultrasound ; TEMPO-trapping ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: High yields of alkyl radicals derived from alkylcobaloximes have been achieved using tungsten light (or in some cases ultrasound) radiation in both organic and aqueous media. These improved yields are obtained when pyridine (the usual base ligand) is replaced by suitably bulky lone-pair donors or water. The alkyl radicals so generated take part in iodine abstraction reactions with benzyl iodide giving benzyl radicals which may be trapped in near-quantitative yield with 2,2,6,6-tetramethylpiperidinyloxy (TEMPO) or in good yield with lepidinium (4-methylquinolinium) trifluoroethanoate or lepidinium camphor-10-sulphonate. The usual drawbacks of cost and tedious work-up procedures associated with the more commonly used organotin hydride reagents are avoided.
    Additional Material: 3 Tab.
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  • 192
    ISSN: 0268-2605
    Keywords: triphenyltin ; carboxylate ; spectroscopy ; crystal structure ; fungitoxicity ; Ceratocystis ulmi ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Four triphenyltin carboxylates formulated as o-Ph3SnOCOC6H4CH=N-Ar (Ar=C6H5; p-CH3C6H4; o-CH3C6H4; o-HOC6H4) were prepared and spectroscopically characterized. The crystal structure of o-Ph3SnOCOC6 H4CH=NC6H5 indicates that the tin atom, in each of the two molecules comprising the asymmetric unit, exists in a distorted tetrahedral geometry owing to an intramolecular acyl O. . .Sn contact. These new triphenyltin carboxylates display marked toxicity against the fungus Ceratocystis ulmi.
    Additional Material: 2 Ill.
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  • 193
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 147-174 
    ISSN: 0268-2605
    Keywords: trifluoromethyl group ; aminoboranes ; trifluoromethyl boron compounds ; synthesis; reactions ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
    Additional Material: 40 Ill.
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  • 194
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    Applied Organometallic Chemistry 10 (1996), S. 175-182 
    ISSN: 0268-2605
    Keywords: boron nitride ; pyrolysis ; chemical vapor deposition ; aminoborane ; borazine ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Research efforts conducted in the Chemistry Division of the Oak Ridge National Laboratory on the preparation of polymeric precursors to boron nitride are reviewed. They evolved from the preparation of powders, which contained significant amounts of residual carbon, derived from the pyrolysis of aminoborane polymers to relatively pure films produced by chemical vapor deposition using polymeric cyanoborane as a single source. Interesting C/B/N films were produced from the pyrolyses of volatile borazine derivatives, and a polymeric borazine intermediate produced denser boron nitride (BN) compact bodies when used as a binder as opposed to bulk BN compressed without a binder. The challenges of producing boron nitride fibers have been defined.
    Additional Material: 5 Ill.
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  • 195
    ISSN: 0268-2605
    Keywords: radiolabeling ; trimethylamine-carboxyborane ; trimethylamine-carboxymethoxyborane ; leukemic cell uptake ; binding to nucleic acids and protein ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The anti-neoplastic agents trimethylamine-carboxyborane and its corresponding methyl ester have successfully been radiolabeled with carbon-14 in the carboxyl group. Using the radiolabeled agents we have shown that their L1210 leukemia cell uptake appeared to be by a passive process and binding of the agents to DNA, RNA and protein over 24 h was minimal.
    Additional Material: 2 Ill.
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  • 196
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 197
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 227-239 
    ISSN: 0268-2605
    Keywords: heteroborane ; cluster ; nitrogen ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: No Abstract
    Additional Material: 6 Ill.
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  • 198
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 125-133 
    ISSN: 0268-2605
    Keywords: organotin compounds ; electrospray ; mass spectra ; clusters ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: The limitations of conventional gas chromatography-mass spectrometry (GC-MS) analyses for alkyl- and aryl-tin compounds are discussed, particularly the excessive fragmentation from electron impact (EI) ionization. Negative EI methods exhibit low ionization capabilities and are restricted to compounds with an electronegative centre, and are thus not suitable for general routine analysis. Liquid chromatography-MS (LC-MS) interfaces offer potential advantages in terms of reduced sample work-up since no derivatization is required. Electrospray techniques give reproducible mass spectra for each compound studied under fixed instrumental parameters. Changes in the cone/repeller voltages can radically alter the observed mass spectra. High-mass species were observed for each compound studied and tentative structures for these species are proposed.
    Additional Material: 5 Ill.
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  • 199
    Electronic Resource
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996) 
    ISSN: 0268-2605
    Keywords: Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 200
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    New York, NY [u.a.] : Wiley-Blackwell
    Applied Organometallic Chemistry 10 (1996), S. 505-512 
    ISSN: 0268-2605
    Keywords: ethylation ; sodium tetraethylborate ; butyltin ; phenyltin ; gas chromatography ; flame photometric detector ; Chemistry ; Industrial Chemistry and Chemical Engineering
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: An organotin speciation method was optimized for the simultaneous determination of mono-, di- and tri-butyltin compounds and mono-, di- and tri-phenyltin compounds in water. The procedure was based on a one-step simultaneous ethylation and extraction using the sodium tetraethylborate reagent directly in the aqueous phase in the presence of an iso-octane layer. Direct extract analysis was performed using capillary gas chromatography and flame photometric detection (GC-FPD). This derivatization procedure reduces drastically the number of analytical steps, thus saving time and improving reliability. Relative detection limits range from 0.4 to 0.8 ng dm-3 for butyltin species and from 0.7 to 2.1 ng dm-3 for phenyltin species; the linearity ranges from 0 to 400 ng dm-3. Analysis of environmental aqueous samples and a Certified Reference Material (CRM) demonstrates the accuracy of the analytical method.
    Additional Material: 5 Ill.
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