- Detection of aromatic volatile organic compounds (VOCs) is important for monitoring occupational hazards, industrial safety, and environmental applications. Here, we present a new in-situ -synthesized carbon dot – aerogel matrix and demonstrate its application for sensing aromatic VOCs. The composite aerogel exhibited high specific surface area and pore diameter, enabling efficient adsorption of the organic vapors. In particular, the excitation-dependent luminescence emission properties of the carbon dots were retained upon embedding within the aerogel host, and provided a sensitive transduction mechanism through both shifts and quenching of the fluorescence emissions. We show that distinct fluorescence shifts and degrees of quenching were induced by different aromatic VOCs. In particular, the C-dot-aerogel sensor could distinguish between isomers of phenylenediamine, an important achievement which has not been previously demonstrated in VOC sensing platforms.