The paper describes a novel method for copper preconcentration using microcrystalline triphenylmethane loaded with malachite green prior to the determination by the flame atomic absorption spectrometry (FAAS). Under the optimum conditions, Cu(II) can be totally adsorbed on the surface of microcrystalline triphenylmethane, and completely separated from Pb(II), Cd(II), Co(II), Cr(III), Ni(II), Mn(II), Fe(III) and Al(III) by controlling acidity. The preconcentration factor of this proposed method is 200. The recovery is in a range of 97.5%-105%. The relative standard deviation (RSD) is not beyond 3.0%. The proposed method has been successfully applied to the determination of trace copper in various water samples with satisfactory results.