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  • 1
    Electronic Resource
    Electronic Resource
    [S.l.] : American Institute of Physics (AIP)
    Review of Scientific Instruments 72 (2001), S. 4424-4433 
    ISSN: 1089-7623
    Source: AIP Digital Archive
    Topics: Physics , Electrical Engineering, Measurement and Control Technology
    Notes: A frequency response device has been designed and built based on previous efforts by Y. Yasuda, L. C. V. Rees, F. Meunier, and Ph. Grenier. This design uses the best attributes of the three previous devices and is improved in five specific ways. First, the device makes use of the fast response capacitance manometer. Second, the device uses a servomotor to push and pull a metal bellows pump, which drives the sinusoidal input function, removing the chance of "floating" the bellows. Third, both sinusoidal and step-change volume perturbations can be studied. Fourth, the overall cost of the device was kept below $30 000. Finally, the pressure transducer is mounted only 8 cm from the sample, instead of ∼30 cm, thus removing any averaging of the pressure signal at higher frequencies. The device is currently capable of measuring frequencies between 0.005 and 5 Hz, a range of three full orders of magnitude. The system can operate at temperatures between room temperature and 473 K and pressures between 0.3 and 300 Torr. Two systems were used to test the device, n-hexane/silicalite and methanol/silicalite. The model developed by Yasuda is used to analyze the frequency response of these systems. This model can describe a system as having more than one diffusivity and accounts for the presence of a surface resistance to diffusion. The results for n-hexane/silicalite and methanol/silicalite are compared to those of van den Begin and Nayak, respectively, and are in good agreement. Also, the diffusivities measured using this device are comparable to those estimated in 1997 by Rees using the frequency response method. In addition to measuring the diffusion rate processes, the kinetic parameters associated with a surface resistance to diffusion were also estimated. © 2001 American Institute of Physics.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Springer
    Catalysis letters 4 (1990), S. 75-83 
    ISSN: 1572-879X
    Keywords: NMR studies of zeolites ; flexibility of zeolites
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology
    Notes: Abstract Zeolites are most often perceived as rigid solids. Recent evidence has demonstrated that the temperature or the adsorption of molecules whose dimensions approach the pore dimensions induce changes in the solid structure, i.e., a flexing of the solid lattice. For pentacil zeolites, as ZSM-5, a transition between monoclinic and orthorhombic forms of the crystalline structure is found with a change in temperature or the adsorption of ring containing molecules. We find that the temperature at which this transition occurs depends on the Si/Al ratio within ZSM-5 and the discrete, reversible transition can be measured by29Si NMR, confirming prior X-ray studies. A similar dependence is found for ZSM-11. Phosphorous modification of the ZSM-5 does not change the transition temperature; however, steam treating of the zeolite does. The implications of these measurements to the flexibility and to the potential for transport is discussed. An analogy between transport and flexibility in one-dimensional polymers and that in the three-dimensional, open, solid network of zeolites is suggested.
    Type of Medium: Electronic Resource
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  • 3
    Electronic Resource
    Electronic Resource
    Springer
    Journal of porous materials 2 (1995), S. 191-199 
    ISSN: 1573-4854
    Keywords: adsorption ; analysis of pore structure ; estimation from sorption pore shape ; from ad-de-sorption surface area ; calculations from sorption
    Source: Springer Online Journal Archives 1860-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics
    Notes: Abstract The interpretation of pore dimensions based on physical ad-desorption analyses is central to the characterization of pore network structure. Several approaches have been proposed and are commonly employed in the analysis of physical adsorption and/or desorption to deduce the dimensions of the porous network. These approaches assume either theoretical (e.g., BET, the Halsey equation as interpreted by Pierce et al., or the more recent analyses of microporosity) or “standard” isotherms as model(s) for the sequential calculations required in estimating the pore network dimensions. Subsequent representation of the pore dimensions and the relationship between these distributions in dimension and other experimental parameters (such as catalytic activity, adsorptivity or transport); thus, depend explicitly on the model employed in the analyses. Each instrument currently available for the measurement of porous solid structure by sorption employs the same specific models for the relationship between the volume ad-desorbed and the dimensions of the porous network that is being characterized. This paper analyzes the interpretation of porous dimensions based on the sequential calculations required in the analyses. A new approach is proposed which is based on a modification to current practices reflecting Halsey's original theory for the thickness of the adsorbed layer (as a function of P/P 0). Further, the calculations of the incremental changes in the exposed surface area are discussed as they relate to pore network structure. A method is proposed to infer the differences in pore shape. Sorption data are analyzed by these new approaches, and these analyses will be compared with those approaches currently employed. Analyses based on these modified approaches provide a dramatically more consistent interpretation of the sorption data and the corresponding pore network structures.
    Type of Medium: Electronic Resource
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