In the present study, activated carbon (AC) surface modified with sodium dodecyl sulfate (SDS), written as SDS/AC, was applied as an adsorbent for preconcentration and determination of trace amount of cadmium ions in environmental sample waters. The SDS modification on AC was performed at the same time, while cadmium ions were concentrated in the flow system as solid-phase extraction. After the separation and preconcentration steps, cadmium retained on SDS/AC was eluted with HNO3 and was subsequently determined by flame atomic absorption spectrometry (FAAS). The analytical parameters that influence the quantitative determination of trace cadmium, such as SDS concentration, pH and volume of sample solution, eluent conditions, and interference, were optimized. At the optimum conditions, the general matrix elements had little interference on the proposed procedure. The detection limits was 17 ng·L−1, and the relative standard deviation (RSD) for 12 experiments at 10 µg·L−1 cadmium solutions was 2.8%. The developed method was applied into the analysis of environmental samples spiked cadmium.