Nanocrystalline films and powders of semiconducting ZnS, with and without doping with Cr, Co and Ni ions, have been synthesized using a low-temperature chemical bath deposition approach in aqueous solution. X-ray diffraction analyses evidenced that ZnS structures consisted of cubic or a mixture of a cubic/hexagonal phase. Average crystallite size was estimated to be 3-4 nm using Scherrer's equation. ZnS and transition metal-doped ZnS were thermally oxidized into corresponding oxides. Magnetic and optical behavior of the sulfide films and powders were investigated using SQUID and UV-visible spectrometry, respectively. Preliminary magnetic measurements suggest antiferromagnetic ordering in Zn0.9Cr0.1S. © 2005 American Institute of Physics.