Procedures for determination of neptunium in marine sediment and seawatersamples are described. Iron hydroxide Fe(OH)2 –Fe(OH)3 is used for preliminary pre-concentration of neptunium. Secondly,neptunium Np4+ and Pu3+ are separated by tri-isooctylamine-(TIOA)extraction in 8–10M HCl by redox with SO32–-Fe3+ Neptunium Np4+ and uranium U6+ areseparated by back extraction the Np4+ with 2M HCl. Finally, theneptunium is purified from the uranium and thorium by anion exchange in 8MHNO3 and 12M HCl. The stripping of 6M HCl + NH2 OH HClfurther separates the neptunium Np3+ and uranium. Reduction bySO 32– –Fe3+ appeared to be an efficientway to obtain Np4+ The decontamination factors of the procedureare 4.0. 104 for 232 Th, 5.6 . 104 for uraniumand 1.6 . 104 for plutonium.