Chromatographic Dynamic Chemisorption: An Alternative to Conventional Estimation of Metallic Dispersion

05 February 2025, Version 1
This content is a preprint and has not undergone peer review at the time of posting.

Abstract

Rigorous standards for reporting the rate of catalytic turnovers over metallic nanoparticles entail normalizing the observed macroscopic observable rate with the active site density. Techniques like transmission electron micrographs and estimating carbon monoxide/ hydrogen uptake have been employed to characterize the active site density of Group 8 dispersed nanoparticles. Based on the principle of dynamic carbon monoxide (CO) chemisorption, the work delineates a novel technique using a gas chromatograph (GC) to estimate the active site density. The dispersion of a Micromeritics™ standard, which provides a benchmark, was measured using the proposed method and compared with conventional techniques. Furthermore, the dispersion of supported platinum group catalysts, varying in supported identity and metal loading, was measured. The amount of dispersed metal as low as 0.02 mg could be estimated by this technique.

Keywords

Chemisorption
Dispersion
Platinum group catalyst
Gas chromatography

Supplementary materials

Title
Description
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Title
Supplementary Information
Description
Description of catalyst loading in inlet liners, metallic dispersion estimations based on nanoparticle size (TEM images), sample calculations for CO uptake measurements via dynamic chemisorption, absence of channeling in the proposed method, comparisons of dispersion estimate by TEM and proposed method, automation of proposed method using a GC, actuation of an electric actuator by a 5890 GC, and comparisons between estimated dispersions between different labs.
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Chemisorption methods and sequences
Description
All the methods and a mock sequence for the proposed method
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