The determination of phosphorus in milk samples by thermal neutron activation analysis employing radiochemical separation is described. The radiochemical separation consists of the simultaneous irradiation of samples and standards, dissolution of the milk samples in a perchloric acid and nitric acid mixture, addition of zinc hold-back carrier, precipitation of phosphorus as ammonium phospho molybdate (A.M.P.) and sample counting in a Geiger-Mueller detector. The analysis sources of error were studied and the established method was applied to phosphorus analyses in commercial milk samples. (author).