Vitrinite reflectance forms the basis of a study of coal rank variation in two areas of the Upper Hunter Valley, New South Wales, on the northern margin of the Sydney Basin. A selective analysis procedure, based on samples rom twenty-two boreholes, has resulted in a small range of reflectance values for each sample and consequently a high degree of significance for calculated mean values. The patterns of rank distribution derived from these data have facilitated an interpretation of the rclative timing of coalilication and deformation in each area.This study provides support for the suggestion by several authors that there were at least two periods of folding in the tJpper Hunter Valley. In the Hebden-Ravensworth area, minor folding took place after most of the coalilication was completed.To the west, in the region of the Muswellbrook Anticline, coalification occurred during or after the formation of this major structure. Tectonic instability during deposition of the Singleton Super-Group, in the region of the Hunter-Thrust on the basin margin, is evidenced by rank variation suggesting differential subsidence across this zone.