A new microsample-pulse method is described for the determination of copper, iron and zinc by ion exchange microcolumn preconcentration-derivative flame atomic absorption spectrometry. The optimum conditions concerning the sensitivity were studied. The method was applied to the determination of Cu, Fe and Zn in tapwater with sensitivity being 0.29, 0.59 and 0.06 microgram.L-1, respectively. The recovery range and the relative standard deviation of the proposed method were 91.13%-101.34% and 1.95%-4.28%, respectively. The detection limits were found to be 1.28, 5.85 and 0.68 micrograms.L-1, respectively. The method is sensitive, accurate, precise and rapid.