A solid-phase extraction (SPE) method has been developed using a column filled with double-walled carbon nanotubes for the preconcentration-separation of Co(II), Cu(II), Ni(II), Pb(II), Fe(III), and Mn(II) ions. Experimental parameters, including pH of the solution, sample volume, flow rate of the sample solution and eluents, etc., were investigated. Quantitative recoveries for the anayte ions were obtained at pH 9.0 with 2 M HNO(3) eluent at a flow rate of 2 mL/min. The influences of matrix ions were also investigated. The preconcentration factor was 100. Addition and recovery experiments for analyte ions in real water samples gave good results. The validity of the presented SPE method was tested by analysis of HR-1 Humber River Sediment certified reference material for each element.