In this paper, we describe a technique for the qualitative and quantitative analysis of such gas mixtures as “hydrogen sulfide in air” and “methane in air” using temperature modulation of a single metal oxide sensor. Using regression analysis in the principal components plane (PC1, PC2), we performed a selective determination of analytes on the minimum set of their concentrations in the training set, which is essential for solving practical problems. An important feature of this work is the difference in test gas concentrations from their concentrations in the training set. For the qualitative analysis of gas mixtures in a wide range of concentrations, we have developed an improved method for processing arrays of multidimensional data. For this improvement, we form a Mahalanobis neighborhood for polynomial regression lines constructed from the projection of training samples for each analyte on the (PC1, PC2) plane. Using the temperature modulation mode for the metal oxide sensor allowed us to increase its response when determining hydrogen sulfide by two to four orders of magnitude compared with the constant temperature mode.