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Zeolite Catalysis

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Zeolite Catalysis ( zeolite-catalysis )

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(Hitachi HighTechnolo-gies, Tokyo, Japan) and JEOL JEM-1011 microscope (Jeol, Tokyo, Japan), respectively. 3.2. Adsorption Isotherms Measurements The adsorption isotherms measurements were carried out by an intelligent gravimetric analyzer (IGA-002, Hiden, Warrington, UK) with three xylene isomers as the representative probe adsorbates and four Beta zeolite samples as absorbents. The key component of this apparatus is a sensitive microbalance with the accuracy of ±0.1 μg, which was used to record the changes in weight of the samples under the computer control. Before the sorption measurement, the zeolite sample about 50 mg was activated under vacuum below 10−7 mbar and maintained at 673 K for 300 min to remove the impurities and moisture until the sample weight keeping constant. In the process of measurement, the vapor of the sorbate was gradually introduced into the sample chamber until the set pressure value was obtained. On reaching the adsorption equilibrium under the set point, the weight change was recorded by the computer software and the vapor pressure was increased to the next designed pressure. Finally, a complete adsorption isotherm was drawn at a certain pressure range. The measurements of adsorption isotherms for xylene isomers on Beta zeolites in this work were conducted in the pressure range of 0–20 mbar and temperature range of 308–338 K, respectively. 3.3. ZLC Measurement and Theory The ZLC method was first proposed by Eic and Ruthven in the late 1980s [41]. Since then, it had become one of the most common methods to measure the intracrystalline diffusion coefficients [42–45]. This method has the advantage of eliminating the intrusion of extraneous heat and mass transfer resistances. The ZLC system was detailedly depicted in [41]. The experimental apparatus is similar to conventional gas chromatography; however, the packed column in gas chromatograph (GC) is replaced by a ZLC column, which is loaded with a very thin layer of sample sandwiched between two porous sintered metal disks. In accordance with the ZLC theory, the sorbate concentration was controlled under the very low relative partial pressures to guarantee the experiments were carried out within the linear region of the adsorption isotherms, i.e., within the Henry’s law region. The effluent stream concentration of ZLC was monitored online by the flame ionization detector. Assuming the adsorption occurring in a very thin layer of zeolite spherical crystals within the linear region of adsorption equilibrium at the very low adsorbate partial pressure, as well as neglecting the hold-up in the ZLC bed and the perfect 252

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