Ultratrace amounts of cobalt at parts-per-trillion (ppt) levels were extracted into m-xylene from aqueous solution as nitrosonaphthol chelates, and colorimetric determination of the m-xylene phase was carried out with photoacoustic spectroscopy (PAS). Coexistent metals and excessive reagents were completely eliminated by acidic and alkaline washings of the m-xylene phase, and the background level became constant and low enough for ultrasensitive PAS determination.