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Metallography, DTA, x-ray, and electron-probe microanalysis methods have been applied to alloys with four compositions in the cast and annealed states. A phase diagram has been constructed for the entire concentration range on the basis of these data together with published ones. The diagram is of peritectic type, and the peritectic temperature is 1500°C. The mutual solubilities of the components at that temperature are 13.3 at.% osmium in nickel and 13 at. % nickel in osmium. The solubility of osmium in nickel falls to 9.2 at. % when the temperature is reduced to 1200°C.