Various organic acids, ultrasonic instruments, and lasers have been used to remove the smear layer from the surface of instrumented root canals. The purpose of this study was to investigate the effect of various concentrations of sodium hypochlorite (NaOCl) as an intracanal irrigant before the use of MTAD (a mixture of a tetracycline isomer, an acid, and a detergent) as a final rise to remove the smear layer. Ten operators, using a combination of passive step-back and rotary 0.04 taper, nickel-titanium files, prepared 80 single- and multirooted human teeth. Distilled water, four different concentrations of NaOCl, or MTAD was used as intracanal irrigant. The canals were then treated for 2 min with 5 ml of one of the following solutions as a final rinse: 5.25% NaOCl, sterile distilled water, 17% EDTA, or MTAD. The presence or absence of smear layer and the amount of erosion on the surface of the root canal walls at the coronal, middle, and apical portion of each canal were examined under a scanning electron microscope. The results show that although MTAD removes most of the smear layer when used as an intracanal irrigant, some remnants of the organic component of the smear layer remain scattered on the surface of the root canal walls. The effectiveness of MTAD to completely remove the smear layer is enhanced when low concentrations of NaOCl are used as an intracanal irrigant before the use of MTAD as a final rinse. This regimen does not seem to significantly change the structure of the dentinal tubules.