In the presented study, a new solid phase extraction technique was developed based on the preconcentration of ions including Ni2+, Zn2+, Cu2+ and Cr3+ ions in environmental samples on SDS-A prior to the determination by FAAS. The conditions for quantitative and reproducible preconcentration, elution and FAAS determinations were studied. The method is simple, accurate, and economical and can be applied for the determination of these understudy metal ions in environmental samples. The system showed reproducibility and reliability in analytical data, with an R.S.D. value of lower than 5% on triplicate experiment. 1.0 g of SDS-A can be used
as high as greater than 10 experiments without any loss in its sorption behavior. The system was successful in preconcentration of analytes from large sample volume (1250 mL).