Journal
REACTION CHEMISTRY & ENGINEERING
Volume 4, Issue 5, Pages 862-883Publisher
ROYAL SOC CHEMISTRY
DOI: 10.1039/c9re00011a
Keywords
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Funding
- American Chemical Society [58044-DNI5]
- National Science Foundation [OIA-1539105]
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This work describes the application of in situ/operando modulation excitation-phase sensitive detection-diffuse reflectance Fourier transform spectroscopy (ME-PSD-DRIFTS) for the characterization of heterogeneous catalysts. ME was enabled using a low void-volume diffuse reflectance cell which allowed rapid gas exchange (gas residence times <2 s) and by periodic feed concentration changes to the reaction cell by a simple switching valve system that provided quasi-square shaped modulation. PSD analysis of a relatively large data set of rapid scan spectra over many periodic cycles was done via a discrete Fourier transform (DFT)/frequency filtering/inverse discrete Fourier transform (IDFT) procedure. A general description of the ME-PSD principle, mathematical framework, guidelines for planning, running, and interpreting results was provided while focusing on ME-PSD-DRIFTS. Aspects such as the modulation frequency and amplitude, modulation waveform, sampling rate, in situ cell residence time, and limitations and future opportunities for ME-PSD-DRIFTS were also discussed. The proposed DFT/IDFT methodology uncovered the use of frequency magnitude plots for the evaluation of spectra baseline shifts, signal response to modulation, the response waveform type, noise, and signal decay/growth. Additionally, ethanol dehydration on gamma-Al2O3 was presented as an example of application of the ME-PSD-DRIFTS methodology.
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