Introduction: This study compared the efficacy of BioPure MTAD (Dentsply Tulsa, Tulsa, OK), 17% EDTA, and 42% citric acid in endodontic smear layer removal and degree of erosion in the apical third of endodontic canals. Methods: Ninety-six extracted single-rooted human teeth were randomized into four groups (n = 24) and instrumented using System GT nickel-titanium rotary instruments (Dentsply Tulsa, Tulsa, OK). Each canal was irrigated with one of the following solutions: BioPure MTAD, 17% EDTA, 42% citric acid, or 5.25% NaOCl (control). Next, all specimens were irrigated with 5.25% NaOCl. Results: Evaluation by scanning electron microscopy showed no significant differences among test irrigants in removing the smear layer. However, the efficacy of BioPure MTAD and 17% EDTA in removing the smear layer was significantly greater than 5.25% NaOCl (control). The erosive effects of irrigating solutions could not be evaluated. Conclusions: In conclusion, the protocols used in this study were not sufficient to completely remove the smear layer in the apical third of prepared root canals. (J Endod 2009;35:900-903)