The purpose of this study was to evaluate in vivo changes in the pH of plaque and of a 10% carbamide peroxide solution occurring within the bleaching gurad during a 2-hour nightguard vital bleaching prcedure. Baseline pH values for plaque and the carbamide peroxide solution were established. A small hole was placed in the anterior interproximal region of the guard to allow placement of the pH electrode. The pH of the carbamide peroxide solution was meausred at 5-minute intervals. After 2 hours, the guard was removed and pH of the plaque was remeasured. The procedure was repeated three times on each of four subjects. The mean baseline pH reading for plaque was 6.31 and mean final pH reading was 6.86. The difference was statistically significant. At initial placement of the carbamide peroxide-filled guard, the mean intraguard pH was 4.50 (range of 2.80 to 7.80). The mean peak intraguard pH of 8.06 (range of 7.30 to 8.43), which was significantly different from baseline, was obtained within 31 minutes. The pH of plaque, saliva, and a 10% carbamide peroxide bleaching solution within the guard increased significantly during bleaching and remained significantly elevated for the duration of the study (2 hours).