The Analytical Development Section of SRTC was requested by the Facilities Disposition Division (FDD) 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 facility also includes the 324-M storage building and the passageway connecting it to 321-M. The results of the holdup assays are essential for determining compliance with the Solid Waste's Waste Acceptance Criteria, Material Control & Accountability, and to meet criticality safety controls. This report describes and documents the use of a portable HPGe detector and EG&G Dart system that contains a high voltage power supply, signal processing electronics, a personal computer with Gamma-Vision software, and space to store and manipulate multiple 4096-channel γ-ray spectra to assay for 235 U content in 268 uranium shipping and storage pigs. This report includes a description of three efficiency calibration configurations and also the results of the assay. A description of the quality control checks is included as well.