Quantitative Determination of Catalytic Surface Adsorption Sites by Fourier Transform Infrared Photoacoustic Spectroscopy

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Abstract
The use of Fourier transform infrared photoacoustic spectroscopy (FT-IR/PAS) as a method for quantitative analysis of surface adsorption sites is demonstrated. Mid-IR information about the amount of adsorption is available with the sampling advantages of PAS: ability to analyze opaque materials with minimal sample preparation, qualitative information about both gas [CO(g)] phase and adsorbed [CO(ads)] species, a sealed sample environment for control of the gas phase in contact with the sample, and the ability to monitor in situ reaction kinetics. In this study a calibration curve is constructed for the amount of CO(g) in the sample cell with a silica internal reference. This calibration curve is utilized to calculate the amount of CO(ads) by subtraction on a catalytic surface where both CO(g) and CO(ads) exist at equilibrium. Using standard parameters from gas titration/volume uptake studies, the surface covered and the percentage of active sites on the surface are determined. This analysis combines the qualitative analytical capabilities of PAS with quantitative analysis, thus demonstrating another facet of the usefulness of FT-IR/PAS in addressing unusual problems.