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Metal insulator silicon carbide field-effect transistor sensors, metal-oxide sensors, and a linear Lambda sensor in an electronic nose was used to measure on-line in hot flue gases from a boiler. Flue gas from a 100-MW pellets-fuelled boiler has been used to feed the experimental setup. Several reference instruments, which measure the flue gases in parallel to the sensor array, are connected to the electronic nose. Data was collected during six weeks and then evaluated. Using principal component analysis as the data evaluation method, different operating modes for the boiler have been identified in the data set. The different modes could be described in terms of high or low O2 and CO concentration. Furthermore, we have shown that it seems possible to use a sensor array to determine the operating mode of the boiler and, by partial least-squares models, measure the CO concentration when the boiler operates in its optimum mode.