An inductively coupled plasma atomic emission spectrometry (ICP-AES) method has been developed for the trace metal characterization of high-level liquid waste solutions originating from reactor fuels of burn-up varying from 1000 to 15,000 MWD per ton. After optimization of various analytical, parameters, the method was validated by analysis of three synthetic samples containing elements in the composition range as expected in high-level radioactive liquid waste (HLLW). The analytical results obtained by ICP-AES from simulated high-level liquid waste (SHLW) of a pressurized heavy water reactor (PHWR), research reactor (RR), fast breeder reactor (FBTR), and high-level radioactive liquid waste (HLLW) from the Plutonium Resprocessing Plant (PREFRE) and Waste Immobilisation Plant (WIP) in Tarapur, India, are also included.