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This study was conducted to investigate the effect of inorganic salts on the mass-transfer coefficient of O3 and decolorization of azo dye (Acid Red 14, AR14) solution through ozonation in a microporous tube-in-tube microchannel reactor (MTMCR). The overall volumetric mass-transfer coefficient (K G a) of O3 in the MTMCR was deduced by material balance. The effects of different salts on the K G a of O3 and decolorization efficiency of the AR14 solution were studied, and results show that both were significantly affected by the inorganic salts. Although the K G a of O3 and the decolorization efficiency of AR14 increased with increasing salt concentration and pH, the effect of NaNO3 was much weaker than that of NaCl, Na2SO4, Na2CO3, and NaHCO3. The enhanced K G a of O3 and decolorization could be due to the generation of species with high oxidizing ability in the presence of the salts.