The part of palladium in ambient urban air that is bound to particles and soluble in aqua regia was determined by means of sorbent extraction, coupled with graphite furnace atomic absorption spectrometry (GFAAS) and laser absorption fluorescence spectrometry (LAFS). Samples of about 200 m3 air were taken in a suburb of Berlin, Germany. The coupling of the selective and automated pre-concentration procedure for Pd as N,N-diethyl-N'-benzoylthiourea complex with the respective detection methods proved to be sufficiently sensitive. Severe interference with other matrix constituents, occurring mainly by direct LAFS detection, could be overcome and the detection limit was improved tremendously. The concentration of Pd in ambient air was determined to be in the range from 0.2 to 14.6 pg/m3.