SINCE the original publication by Moore1, gel permeation chromatography has been widely recognized as a rapid means of assessing the molecular weight distributions of polymeric materials soluble in organic solvents. While the use of this technique, principally based on the reliable commercial instrument2, is well established, reference in published work to the preparation of the cross-linked polystyrene gel, and its packing into columns with high plate count, is very brief. Some information is to be found in the writings of Moore1 and Altgelt3 and in the review of Johnson, Porter and Cantow4. This communication describes how gels of varying porosity may be prepared, and packed into columns having a plate count within the range 700–1,300 theoretical plates/ft.