Abstract: Copper and lead in activated sludges were determined successfully by platform graphite furnace atomic absorption spectrometry, digest sample by microwave-heating in a tightly closed PTEF vessel. Under the experiment condition, RSD of copper was in the range of 1.0%～2.0%, recoveries 95.6%～98.3%, and detection limit 0.005 2 ng/g. RSD of lead was in the range of 2.0%～2.9%,recoveries 92.3%～97%, and detection limit 0.007 3 ng/g. The feasibility of this method was proved by the satisfactory results obtained in the analyses of three sludge samples.