An enrichment-separation method using solid-phase extraction of trace amounts of Fe(III), Cu(II), and Pb(II) as their pyrocatechol violet chelates on multiwaled carbon nanotube column has been established. Analytes were desorbed from the column by using 5mL of 2.0M HNO3. Influences of some analytical parameters like pH and sample volume on the recoveries of the analyte ions were investigated. Effects of matrix ions were also evaluated. The presented procedure was validated by using additional recovery test and analyzing the certified reference materials (SRM 1570aTrace Elements in Spinach Leaves and TMDA-70 fortified lake water). The application of this method was successfully performed for the determination of copper, iron, and lead levels in various fertilizer samples marketed in Kayseri-Turkey and some water samples.