Abstract: Using 0.1 mol/L(NH 4) 2SO 4 as deposition solution, the voltage between plutinum anode and stainless steel cathode is controlled at about 15 V,and the current density is 0.65 A/cm 2.After electrolyzing for 40 minutes, plutonium,neptunium and americium can be deposited quantitatively on the cathode. The recovery of them is more than 98%.Influence of 18 coexisted materials are investigated, most cations influence the recovery and resolution except alkaline and alkaline earth elements at the same time,some interference limits are given. Small amount of NO - 3,Cl -,TBP,TRPO,kerosene and oxalic acid don't influence the deposition. When the activity of alpha nuclide is more than 0.25 Bq and the measuring time is more than 60 minutes, the total uncertainty of depositon and measurement is better than ±4.0%. The electrodeposition procedure is suitable for both aqueous and organic samples.