An analytical procedure for determining the relative amounts of 60Co and its 60Ni daughter in a radioactive cobalt source by means of chromatographic separation and radiometric and mass spectrometric detection was developed, optimized and assessed through two round robin exercises for nuclear forensic investigations. Solid phase extraction (EXC) using Ni resin (Eichrom) and ion exchange (IEC) using Dowex-1X8 (Acros Organics) chromatographic approaches were considered for separating Co and Ni. Decontamination factors of 25 and 2.8 × 106 were measured for EXC and IEC, respectively. Based on those results, only the IEC option was pursued. The effects of particle size, mass of resin, and degree of cross-linkage for decontamination performance were assessed, and the loading/eluting conditions were optimized. Canadian (CNSC, RPB, UL, RMC, AECL) and American (ANL) laboratories participated in two round robin exercises designed by the National Research Council of Canada to determine the suitability and limitations of the proposed methods. Age determination for freshly irradiated sources (<1 a) and for sources with high Ni content was challenging for the laboratories. Nevertheless, age estimates were obtained with sufficient accuracy for nuclear forensic purposes.
