Objectives: Potential adverse effects and pH-related effectiveness of bleaching agents have raised some concerns. The aim of this study was to compare three bleaching agents containing hydrogen peroxide (HP) and carbamide peroxide (CP) in terms of whitening effectiveness, pH variation, and changes in enamel surface roughness. Methods: After controlled staining with a black tea solution, 42 human enamel specimens underwent bleaching treatment using the following agents: HP 40%; HP 35%; CP 16%. Color changes were evaluated according to the CIEDE2000 system. Gel pH was measured before and after each application. Surface roughness (Sa) was assessed through optical 3D profilometry before and after bleaching treatment. Results: The whitening effectiveness was similar for HP 40% and HP 35% while CP 16% had significantly lower results. HP 40% showed a remarkable pH acidification (−0.41), while HP 35% and CP 16% showed a mild increase in pH values (+0.26 and +0.03, respectively), and the differences between HP 40% and HP 35% and between HP 35% and CP 16% were statistically significant. Sa slightly decreased in all groups after bleaching, with no significant differences among them and a significant difference in HP 40% before and after treatment. Conclusions: Similar bleaching results were achieved regardless of pH and HP concentration for HP-based agents, while a lower bleaching effect was observed for the less concentrated CP-based agent, as anticipated. Higher HP and greater tendency to pH instability induced more pronounced modifications of surface roughness. This in vitro study suggests that bleaching gels with neutral and stable pH ensure good bleaching effectiveness and are less likely to cause enamel surface changes.
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