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Abstract Aggregation‐induced emission has eliminated the problem of fluorescence quenching in the solid state, making molecules with this property excellent candidates for vapor sensing due to their portability and ease of interpretation. Here, films of polystyrene / 2‐[4‐vinyl(1,10‐biphenyl)‐40‐yl]‐cyanovinyljulolidine copolymers are reported that exhibit aggregation‐induced emission behavior for the detection of toluene, m‐xylene, dichloromethane, and chloroform. After exposure to the analytes, the emission of the copolymers shows significant changes in intensity and spectral shape corresponding to the reduced microviscosity of the molecular environment. However, these changes are similar for different analytes, resulting in low chemical selectivity. Therefore, label‐free selectivity is achieved by controlling the molecular diffusion of the four vapor analytes within the films using the Flory–Huggins solution theory with capping layers of cellulose acetate (CA) and poly(vinyl alcohol) (PVA) polymers.