It has been shown by earlier studies on the formation of the Los Angeles smog aerosol, that a significant fraction of the particulate matter in the visible size range is made by secondary gas-particle conversion processes, and that it consists mainly of liquid matter. In this study the volatility was studied quantitatively by heating the smog aerosol up to 250°C and simultaneously measuring the scattering coefficient using a nephelometer and the change of size distribution by an optical counter. The thermal analyses revealed that 50–80% of the submicron aerosol mass is volatile at 220°C. Inspection of the shapes of thermo-nephelograms (bscat vs temperature) also revealed that photochemically formed aerosols have distinctly different thermo-nephelograms than those obtained on humid “hazy” days. Thus it is suggested that thermal analyses may at least in some instances provide the means of on-line monitoring the origin of the ambient aerosol.