The Analytical Development Section of Savannah River Technology Center (SRTC) was requested by the Facilities Disposition Projects (FDP) to determine the holdup of enriched uranium in the 321-M facility as part of an overall deactivation project of the facility. The 321-M facility was used to fabricate enriched uranium fuel assemblies, lithium-aluminum target tubes, neptunium assemblies, and miscellaneous components for the production reactors. The results of the holdup assays are essential for determining compliance with the Waste Acceptance Criteria, Material Control & Accountability, and to meet criticality safety controls. This report covers calibration of the detectors in order to support holdup measurements in the C and D out-gassing ovens. These ovens were used to remove gas entrained in billet assembly material prior to the billets being extruded into rods by the extrusion press. A portable high purity germanium detection system was used to determine highly enriched uranium (HEU) holdup and to determine holdup of 235U, 237Np, and 241Am that were observed in these components. The detector system was run by an EG&G Dart system that contains the high voltage power supply and signal processing electronics. A personal computer with Gamma-Vision software was used to control the Dart MCA and provide space to store and manipulate multiple 4096-channel -ray spectra. The measured 237Np and 241Am contents were especially important in these components because their presence is unusual and unexpected in 321-M. It was important to obtain a measured value of these two components to disposition the out-gassing ovens and to determine whether a separate waste stream was necessary for release of these contaminated components to the E-Area Solid Waste Vault. This report presents determination of the calibration constants from first principles for determination of 241Am and 237Np using this detection system and compares the values obtained for 237Np with the calibration factors obtained with a subsequent measurement using a point source of radioactive equilibrium 237Np/233Pa.