Abstract: A method is developed for the simultaneous measurement of low-level ~(60)Coand ~(65)Zn in seawater, marine organisms and sediments by an ion-exchange separa-tion, solvent extraction with MIBK, electrodeposition on a copper plate and beta-counting. By this method, the minimum detectable concentration is 1.2×10~(-3) Bq/1(g) for ~(60)Co and 1.1×10~(-2) Bq/1(g) for ~(65)Zn respectively. The decontamination factors for some important radionuclides, such as ~(54)Mn,~(59)Fe,~(90)Sr, ~(95)Zr- ~(95)Nb, ~(106)Ru- ~(106)Rh and ~(137) Cs, are greater than 10~3. The chemicalrecovery is about 90% for cobalt and about 85% for zinc respectively. The che-mical and radiochemical recoveries are coincident. This method is simple, rapidand accurate for the simultaneous determination of low-level ~(60)Co and ~(65)Zn inmarine environmental samples.