Production of high specific activity (HSA) 60Co has recently resumed at the Advanced Test Reactor (ATR) at the Idaho National Laboratory. The technical steps of performing in-canal assay of HSA 60Co targets at the ATR are described herein. The HSA targets are assayed on a regular basis, between cycles at the ATR, in order to assess the progress of activation. The targets are also assayed at the conclusion of the irradiation in order to provide activity estimates for the distributor and to be used for safety and shipping evaluations. These target assay activities must take place in the ATR canal to provide sufficient radiological shielding. A specialized assay fixture is used in conjunction with custom 60Co radiation standards to assess the irradiated target. The specific activity of each irradiated target was determined by first measuring the 60Co standards to determine a sensitivity factor. Then, each irradiated target was measured, and the integrated measurement was multiplied by the sensitivity factor to determine the total activity of the irradiated target. Finally, a correction factor was determined to adjust the reported activity, accounting for differences in the physical geometries of the standards and targets. These methods were used to accurately assay the gross activity of nine irradiated 60Co targets, two of which were delivered to the distributor where confirmatory hot-cell assays were performed verifying the accuracy of the in-canal assay method.