2DCOR-GC:  An Application of the Generalized Two-Dimensional Correlation Analysis as a Route To Optimization of Continuous Flow Supercritical Fluid Reactions

• Published in: Analytical chemistry (Washington) Vol. 76; no. 21; pp. 6197 - 6206
• Main Authors: Hyde, Jason R, Bourne, Richard A, Noda, Isao, Stephenson, Phil, Poliakoff, Martyn
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 01.11.2004
• Subjects: Analytical chemistry; Chemistry; Chromatographic methods and physical methods associated with chromatography; Exact sciences and technology; Gas chromatographic methods; Spectrometric and optical methods; Water; Fourier transform spectroscopy; Alcohol; Alkylation; Optimization; Two dimension spectrometry; Cresol; Infrared spectrometry; Gas chromatography; Correlation analysis; Continuous flow method; Catalyst; Monitoring
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/ac049360l

A new approach for optimization and monitoring of continuous reactions has been developed using 2D correlation methods for the analysis of GC data (2DCOR-GC). 2DCOR-GC maps are obtained following perturbation of the system that allow the effect of changing reaction parameters such as time, temperature, pressure, or concentration to be both monitored and sequenced with regard to changes in the raw GC data. In this paper, we describe the application of the 2DCOR-GC technique to monitoring the reverse water−gas shift reaction in scCO2. 2DCOR-GC is combined with FT-IR data to validate the methodology. We also report the application of 2DCOR-GC to probe the mechanism of the alkylation of m-cresol with isopropyl alcohol in scCO2 using Nafion SAC-13 as the catalyst. These results identify coeluting peaks that could easily be missed without exhaustive method development.