Complete carbon analysis of sulfur‐containing mixtures using postcolumn reaction and flame ionization detection

Quantitative analysis of complex mixtures containing hundreds-to-thousands of organic compounds rich in heteroatoms, including oxygen, sulfur, and nitrogen, is a major challenge in the fuel, food, and chemical industries. In this work, a two-stage (oxidation and methanation) catalytic process in a 3-D–printed metal microreactor was evaluated for its capability to convert sulfur-containing organic compounds to methane. The microreactor was inserted into a gas chromatograph between the capillary column and flame ionization detector. Catalytic conversion of all sulfur-containing analytes to methane enabled carbon quantification without calibration, by the method identified as “quantitative carbon detection” or QCD. Quantification of tetrahydrothiophene, dimethyl sulfoxide, diethyl sulfide, and thiophene indicated complete conversion to methane at 450°C. Long-term performance of a commercial microreactor was evaluated for 2000 consecutive injections of sulfur-containing organic analytes. The sulfur processing capacity of the microreactor was identified experimentally, after which reduced conversion to methane was observed. © 2017 American Institute of Chemical Engineers AIChE J, 63: 5438–5444, 2017