A radiochemical separation method to determine plutonium (Pu) radioisotopes in environmental samples has been established in Radiochemistry and Environmental Laboratory in Malaysia. The analysis involving sample digestion with aqua regia solution and followed by radiochemical separation using ion exchange method. The source for alpha spectrometry was prepared by electrodeposition. The chemical recoveries were determined using 242 Pu tracer. The method was tested on reference materials and on real sediments from Malaysia marine environment. The validity of the method was checked for coherence using the t-test, relative error and relative standard deviation. All the results obtained were in good agreement with the reference values which indicated that the recommended procedures was successfully applied for the determination of plutonium activities in Radiochemistry and Environmental Laboratory in Malaysia.