Nanostructured NiS was prepared by inclusion into anodic alumina templates. Theresultant particles were found to be stoichiometric and highly crystalline. The particlesdisplayed small particle superparamagnetism, and a low temperature (at 48 K(Tsg)) spin-freezing phenomenon (a spin-glass) and higher temperature (170 K) thermal blockingof small particle magnetic moment fluctuations were both observed for the firsttime for a sulfide material. Very unusually, these NiS materials are quite distinctfrom antiferromagnetic nanoparticulate sulfide materials, as they display a hightemperature ferromagnetic-like phase. The saturation magnetization, the remanentmagnetization, the coercivity and the ferromagnetic mass susceptibility were measured as0.58 emu g − 1 (at 100 K),0.19 emu g − 1, 219.5 Oe (at170 K) and ∼ 900 × 10 − 6 emu Oe − 1 g − 1 respectively and these are consistent with a moderately strong ferromagnetism. Thematerials had an unexpectedly high Curie temperature of 390 K. The decrease of thesaturation magnetization value at 30 K suggests that the ferromagnetic response is a surfacephenomenon and the high coercivity of the paramagnetic component well aboveTsg suggests that the core can be described as superparamagnetic.