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This study evaluates the performance advancement of electronic noses, on-chip engineered multisensor systems, exploiting a combinatorial approach. We analyze a spectrum of metal oxide semiconductor materials produced by individual methods of liquid-phase synthesis and a combination of chemical deposition and sol–gel methods with hydrothermal treatment. These methods are demonstrated to enable obtaining a fairly wide range of nanomaterials that differ significantly in chemical composition, crystal structure, and morphological features. While synthesis routes foster diversity in material properties, microplotter printing ensures targeted precision in making on-chip arrays for evaluation of a combinatorial selectivity concept in the task of organic vapor, like alcohol homologs, acetone, and benzene, classification. The synthesized nanomaterials demonstrate a high chemiresistive response, with a limit of detection beyond ppm level. A specific combination of materials is demonstrated to be relevant when the number of sensors is low; however, such importance diminishes with an increase in the number of sensors. We show that on-chip material combinations could favor selectivity to a specific analyte, disregarding the others. Hence, modern synthesis methods and printing protocols supported by combinatorial analysis might pave the way for fabricating on-chip orthogonal multisensor systems. [ABSTRACT FROM AUTHOR]