A simple new characterization method of ultra–microporous structures was developed by measuring pressure change through gas diffusion in constant volume around room temperature. Several gas species such as He, Ne, Ar, N2, and CH4, which had different molecular size each other, were utilized as molecular probes for detecting effective micropore volume for gas diffusion under a room temperature in gas phase. The feature of this characterization method was that observed micropore volume for gas diffusion depended on the probing gas molecular size, and it enabled the quantitative estimation of effective micropore volume for each probing molecule. Zeolite Y (FAU) and ZSM–5 (MFI), which were known to have regular micoporous structures, were adopted as a standard sample for verifying the mulita–gas diffusion method. The conventional N2 adsorption at 77 K was also employed to characterize microstructures of those zeolites and both the validity and superiority of the proposed multi-gas diffusion method were examined. The volume of major pores of FAU, which is calledα–cage whose size is about 1.3 nm, was also detected by diffusion of larger molecules such as Ar and N2. Ordinal N2 adsorption method can give the pore size and volume of onlyα–cage, however, a bi–modal porous structure of FAU comprised ofα–cage and SOD (β– cage) was successfully detected by diffusion of smallest He molecule. For the case of ZSM–5, all probing gas molecules showed similar but slightly different micropore volumes due to the different diffusing molecular size. Adsorption enthalpy was also reasonably estimated by the technique.
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