Copper-61 (T-1/2 = 3.33 h) produced via the Zn-nat(p, x)(61) Cu nuclear reaction using natural zinc target, was separated from the irradiated target material by a two-step method developed in our laboratory and was used for the preparation of [Cu-61]-pyruvaldehydebis(N-4-methylthiosemicarbazone) ([Cu-61]-PTSM) using an in house-made PTSM ligand. An electroplated natural zinc layer on a gold-coated copper backing (zinc and gold layer thicknesses were 80 and 50 mu m respectively) was irradiated with 22 MeV protons (22-12 MeV on the target). 61 Cu was separated by a two-step chromatography method using a cation and ail anion exchange column which gave satisfactory results. After 180 mu A irradiation of the target for 3.2 hours, about 6.006 Ci Of (CU2+)-C-61 was obtained with a radiochemical separation yield of more than 95% and a radionuclidic purity of more than 99% (Cu-60 as impurity). Colorimetric methods showed that traces of chemical impurities in the product were below the accepted limits. The solution of [Cu-61]-PTSM was prepared with a radiochemical yield of higher than 80%, radiochemical purity of better than 98% and specific activity of about 246 Ci/mmol.