Mechanical instrumentation of root canals produces a smear layer that adversely affects the root canal seal. The aim of this study was to evaluate efficacy of MTAD and citric acid solutions used with self-adjusting file (SAF) system on smear layer. Twenty-three single-rooted human teeth were used for the study. Canals were instrumented manually up to a number 20 K file size. SAF was used to prepare the root canals. The following groups were studied: Group 1: MTAD + 5.25% NaOCl, Group 2: 20% citric acid + 5.25% NaOCl, and Group 3: Control (5.25% NaOCl). All roots were split longitudinally and subjected to scanning electron microscopy. The presence of smear layer in the coronal, middle, and apical thirds was evaluated using a five-score evaluation system. Kruskal-Wallis and Mann-Whitney U tests were used for statistical analysis. In the coronal third, Group 2 exhibited the best results and was statistically different froms the other groups (P < 0.05). There was not a significant difference among the three thirds of groups according to in-group comparisons (P > 0.05). The solutions used in Group 1 and 2 could effectively remove smear layer in most of the specimens. However, citric acid was more effective than MTAD in the three thirds of the canal.