Atmospheric pollution has been found to modify the hygroscopicity of particles and the ability of aerosols to become cloud condensation nuclei (CCN). Aerosols and the bulk CCN were measured in urban Guangzhou during pollution periods in January 2016, and the particle liquid water content (PLWC) and aerosol acidity (Aero-pH) were calculated to examine their possible effects on aerosols’ CCN activation. The results demonstrate that the PLWC and Aero-pH likely play key roles in enhancing aerosol activation during the early stages of pollution episodes. The analysis of the calculated and the observed data shows that CCN, PLWC, Aero-pH and water-soluble inorganic matter (WSIM) are closely linked to each other, particularly at night, and Aero-pH and PLWC act as pre-occurring indicators of activated aerosols and aerosol activity, respectively, during the rapid onset of pollution. In theory, the feedback between chemical reactions, aerosol acidity and particle water content accounts for the changes in aerosol activation accompanying particle accumulation and aging. Our research provides insights into the swift formation of particle pollution characterized by secondary aerosols and suggests a possible approach to tracking or characterizing its effects on the activation of aerosols into CCN without requiring CCN or aerosol number measurements.