Instrumental and radiochemical neutron activation analysis has been applied to a comprehensive trace characterization of AlSiCu sputter targets. By instrumental neutron activation analysis via long-lived indicator radionuclides, up to 33 elements were assayed with detection limits between 0.01 and 200 ng·g–1. The high activity of64Cu and24Na produced from the matrix significantly limits the instrumental performance via short- and medium-lived indicator dionuclides. For this reason, a radiochemical separation was developed based on adsorption of24Na on hydrated antimony pentoxide and extraction of64Cu by diethylammonium diethyldithiocarbamate from HCl medium. By this radiochemical method, As, Ga, K, La, Mn, Mo, Re, Sb, U and W could be assayed via medium-lived radionuclides and the achievable limits of detection were between 0.1 and 25 ng·g–1. Further improvement of detection limits for U and Th was achieved by a selective radiochemical separation of239Np and233Pa on a Dowex 1×8 column in HF and HF/NH4F medium providing limits of detection for U and Th of 0.06 and 0.02 ng·g–1, respectively. These techniques were applied to the analysis of two AlSiCu sputter target materials. Results are compared with those of glow discharge mass spectrometry.