Fe-Ni@ACC nanocomposite was synthesized by hydrothermal method and characterized using scanning electron microscope (SEM) and Fourier-transform infrared spectroscopy (FT-IR). Fe-Ni@ACC was used as adsorbent for magnetic dispersive micro solid-phase extraction (M-D-μSPE) procedure for separation and preconcentration of trace level of copper at trace levels before its determination by microsampling flame atomic absorption spectrometry (FAAS). The effects of various parameters such as pH, amount of adsorbent, eluent type and eluent volume, and sample volume on the recoveries of copper on Fe-Ni@ACC were optimized. The presented method is accurate, inexpensive and environmentally friendly and due to magnetic properties of the adsorbent, the separation process is very simple and fast. The method presents limit of detection (LOD)(3s/m) of 0.69 μg L?1, limit of quantification (LOQ)(10s/m) of 2.29 μg L?1, preconcentration factor of 40 and relative standard deviation (RSD %) (s/x) 1,18%. The accuracy of the method was confirmed by the analysis of TMDA-53.3 fortified water and TMDA-64.2 fortified water certified reference materials and addition-recovery tests to real samples. The present M-D-μSPE method was successfully applied to determination of copper level of tap water, cigarette, human hairs and black teas samples.