We report the effect of the chain length of carboxylic acid on the photoluminescence(PL) of /ZnS nanocrystals. /ZnS nanocrystals with emission wavelength ranging from 566 nm through 583 nm were synthesized with zinc acetate and carboxylic acids with various chain length. In this study, /ZnS nanocrystals prepared using long chain carboxylic acid showed more improved PL intensity. The origin of strong photoluminescence of the nanocrystals prepared with zinc acetate and long chain carboxylic acid was ascribed to improved size distribution due to strong reactivity between long chain carboxylic acid and zinc acetate.