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Wunsch, Marco R.; Lehnig, Rudolf; Janke, Christiane; Trapp, Oliver (2018): Online High Throughput Measurements for Fast Catalytic Reactions Using Time-Division Multiplexing Gas Chromatography. In: Analytical Chemistry, Vol. 90, No. 15: pp. 9256-9263
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Abstract

Developing new catalysts is crucial for optimization of chemical processes. Thus, advanced analytical methods are required to determine the catalytic performance of new catalysts accurately. Usually, gas chromatographic methods are employed to analyze quantitatively the product distribution of volatile compounds generated by a specific catalyst. However, the characterization of rapidly changing catalysts, e.g., due to deactivation, still poses an analytical challenge because gas chromatographic methods are too slow for monitoring the change of the complex product spectra. Here, we developed a gas chromatographic technique based on the concept of multiplexing gas chromatography (mpGC) for fast and comprehensive analysis of the product stream from a catalytic testing unit. This technique is applied for the study of the catalytic reaction of methanol-to-olefins (MTO) conversion. For this method, the time distance between two measurements is chosen so that the chromatograms but not the peaks themselves are superimposed. In this way, stacked chromatograms are generated in which the components from successively injected samples elute baseline separated next to each other from the column. The peaks from different samples are interlaced, and for this reason, the method is referred to as time-division multiplexing gas chromatography (td-mpGC). The peaks are analyzed by direct peak integration not requiring a Hadamard transformation for deconvolution of the raw data as usual for many mpGC applications. Therefore, the sample can be injected equidistantly. The integrated peaks have to be allocated to the correct retention times. The time distance between two measurements for studying the reaction and regeneration cycles of MTO catalysts is 4.3 min and 38 s, respectively. Column switching techniques such as back-flush and heart-cut are introduced as general tools for multiplexing gas chromatography.