A preconcentration procedure based on the adsorption of Cu(II), Co(II), Cd(II), Pb(II), Mn(II), and Ni(II) as their O-O-diethylphosphorodithioic acid chelates on activated carbon cloth (ACC) is presented. The analytical parameters including pH of the working media, amount of O-O-diethylphosphorodithioic acid, and eluent type, etc., were optimized. The effects of matrix components were also investigated. The analyte elements were quantitatively recovered at pH 6.0 with 0.5 mg O-O-diethylphosphorodithioic acid and 10 mL 3M HNO3 was used as the eluent. Addition recovery tests were also performed for real samples. The relative standard deviations were generally lower than 5%. The validation of the proposed procedure was checked by the analysis of SPS-WW2 Wastewater certified reference material. The solid phase extraction method was applied to the separation-preconcentration of the analyte elements from environmental samples, including natural water and soil samples from Kayseri, Turkey.