This study presents a solid phase extraction (SPE) procedure for preconcentration and separation of Cu(II), Cd(II), Pb(II) and Ni(II), as their diethyldithiocarbamate chelates on Sepabeads SP-207 resin using flame atomic absorption spectrometry. The parameters, including pH, sample volume, eluent type and volume etc., were optimised. The influences of the some alkali, alkali earth and transition metal ions on the involvement of copper(II), cadmium(II), lead(II) and nickel(II) were also examined. The preconcentration factor was calculated as 50. The limit of detections of the analyte ions (k = 3, N = 21) were 0.18 μg L−1 (Cu), 0.17 μg L−1 (Cd), 0.55 μg L−1 (Pb) and 1.67 μg L−1 (Ni). GBW 07605 Tea and NRCC-DORM-2 Dogfish Muscle certificated reference materials were used for confirm of method. The method was successfully performed for determination of Cu(II), Cd(II), Pb(II) and Ni(II) ions in water and food samples. The relative standard deviation was found to be lower than 7%.