This study aimed to investigate the effects on enamel surface treated with hydrogen peroxide bleaching and acidic soft drink immersion and/or brushing with whitening dentifrices. Fifty-six standardized enamel slabs obtained from labial surfaces of bovine incisors were used. Enamel slabs were ground flat, polished, and randomly assigned to one of seven treatment groups: (1) control, in which no treatment was performed, (2) soft drink immersion, (3) 38% hydrogen peroxide bleaching, (4) simulated toothbrushing with whitening dentifrice, (5) soft drink immersion and bleaching, (6) soft drink immersion, bleaching, and toothbrushing, and (7) bleaching and toothbrushing. The mineral concentration of enamel surfaces was determined before and after treatments by means of Fourier transform (FT)-Raman spectroscopy and energy dispersive x-ray fluorescence spectrometry (EDXRF). Data were statistically analyzed by ANOVA and Tukey test (p < 0.05). Raman spectroscopy results indicated that enamel mineral content decreased after all treatments except in group 1, whereas EDXRF results exhibited mineral decrease in groups 3, 4, 5, and 7. Bleaching alone or in combination with soft drink immersion and brushing decreases enamel mineral content.