Wednesday, November 7, 2007 - 9:35 AM
346e

Far Fourier-Transform Infrared Spectroscopy As A Characterization Tool For Zeolite-Like Porous Adsorbents

Tyler M. McGown1, Xin Sun2, Jennifer L. Anthony2, and John R. Schlup3. (1) Burns & McDonnell, Kansas City, MO 64131, (2) Chemical Engineering, Kansas State University, 105 Durland Hall, Manhattan, KS 66506, (3) Department of Chemical Engineering, Kansas State University, 105 Durland Hall, Manhattan, KS 66506

Far-infrared (FIR) spectroscopy has been shown to be capable of identifying compositional and structural differences in zeolitic materials. The ability to observe differences between similar zeolites in the near- and mid-infrared regions can be limited; however, notable variations can become apparent in the far-infrared region. Although it is often an underused resource, this work illustrates the clear potential for using far-infrared spectroscopy to explore the inorganic and coordinated metal bonding sites in zeolite-like molecular sieves.

Diffuse reflectance Fourier transform infrared (DRIFT-IR) spectroscopy was employed to characterize a range of zeolites and zeolite-like molecular sieves in their powdered forms. Whiles spectra were collected from 8500 cm-1 to 150 cm-1, the far-IR region (400 cm-1 - 10 cm-1, but typically < 650 cm-1 in practice) was of particular interest as it can yield information on bonding of heavier elements, such as metals within the framework of the zeolite, tetrahedral atom-oxygen bending, and pore openings in zeolites. The advantage of these particular experiments is that diffuse reflection spectroscopy permits IR spectra of powders to be acquired with a minimum of sample preparation. Far-IR spectra result from vibrations involving elements heavier than those typically observed in mid-IR spectra or coordinated vibrations involving structures such as rings. Such species are expected with the zeolite-like materials being considered and in the products resulting from processes such as ion-exchange or calcination. Thus, these experiments are expected to address the questions often asked of these materials more directly than other spectroscopic techniques.

Results are presented for a series of zincosilicates with different framework structures (VPI-7, VPI-9, and VPI-10). Dramatic differences were observed across the far-IR region for each of the materials. Spectra are compared for as-made samples as well as calcined, ion-exchanged, and intentionally collapsed samples. Subtle differences in the far-IR region were identified for materials that had the same crystalline framework but different composition (zeolite beta (*BEA) and the zincosilicate CIT-6, treated to yield pure silicate, aluminosilicate, and zincosilicate forms).