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We developed combinatorial screening techniques for the efficient design and optimization of sensor materials formulations for gas and liquid optical sensors. Our approach is based on the fabrication and performance screening of discrete and gradient sensor materials arrays. Simultaneous formation of multiple sensor coatings into discrete arrays and their screening provides not only a well-recognized acceleration in the screening rate, but also considerably reduces or even eliminates sources of variability, which are randomly affecting sensors response during a conventional one-at-a-time sensor coating evaluation. The application of gradient sensor arrays provides additional capabilities for rapid finding of the optimal formulation parameters.