Gold at the Harbour Lights Mine (HLM), WA occurs principally in pyrite (Py) and arsenopyrite (AsPy) minerals rendering it inaccessible to direct cyanidation. Froth flotation produces a concentrate with low mass recovery and with high recoveries of sulfides. After investigating several alternatives, a novel flotation process has been developed to separate the concentrate into pyrite and arsenopyrite rich fractions. The pyrite fraction is finely ground and cyanide leached, while the arsenopyrite is treated off-site. This paper describes the separation process from laboratory bench scale through to commercial operation at the HLM gold plant.