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• A novel methodology for rapidly detecting and identifying BTEX based on energy transfer ratiometric cataluminescence. • BTEX exhibit different energy transfer processes to Eu3+ and Tb3+ on the surface of Eu,Tb-MgO nanomaterial. • The synergistic effect of ozone induction and high active sensing material enhanced sensitivity of BTEX. The detection and discrimination of benzene, toluene, ethylbenzene and xylene (BTEX) are tricky and challenging issues no matter in environmental monitoring or process controlling in industrial fields. Herein, an ozone-inducted ratiometric cataluminescence strategy for fast quantifying and recognizing BTEX was developed. With ozone as oxidant and rare earth ions Eu3+, Tb3+ co-doped MgO nanocatalyst as sensing material, BTEX were found to produce strong cataluminescence (CTL) emission. And each analyte has unique ratio of the intensities under the characterization wavelength of Eu3+ and Tb3+ in a wide range of concentrations, which can be assumed as the qualitative parameter for BTEX recognition. On that basis, BTEX were supposed to be identified successfully with discrepant ratios for I Eu /I Tb of 0.73 ± 0.03, 1.34 ± 0.03, 4.47 ± 0.18, 2.39 ± 0.11, and measured simultaneously with detection limit of 0.13, 0.21, 0.092, 0.053 μg ml−1, respectively. Besides, the prepared catalysts were characterized and the possible CTL sensing recognition mechanism for BTEX were discussed in detail. The proposed methodology provides a new insight for monitoring and identifying low active compounds. [ABSTRACT FROM AUTHOR]