Accurate and reliable analytical methods have been developed for the measurement of Pu, Am and Cm in typical waste streams from nuclear power plants. Pu, Am and Cm were separated using anion exchange and coprecipitation techniques. The solution of Am and Cm was electrodeposited and measured by α-particle spectrometry. In the case of Pu the solution was divided into two aliquots, one for liquid scintillation counting and the other for electrodeposition followed by α-particle spectrometry. To determine the chemical recovery of α emitters of the Pu fraction and the Am and Cm fraction, the sample was spiked with 236Pu and 243Am. The chemical recovery of 241Pu was calculated using two different methods which gave reliable results. Analysis of every sample was carried out twice to examine the reproducibility of the analytical methods. The radiochemical yields of Pu and Am ranged from 80% to 100% and from 60% to 80% respectively.