Heating stability, physical and chemical analysis of calcium silicate-based endodontic sealers.

AIM: To evaluate possible modifications in root canal sealers subjected to a variety of heating conditions using vibrational spectroscopy and analysis of physical and chemical properties. METHODOLOGY: EndoSequence BC Sealer HiFlow, Bio-C Sealer, BioRoot RCS and AH Plus were analysed chemically using Raman spectroscopy (25-220 °C) and Fourier-transform infrared spectroscopy (FT-IR) (37-100 °C ). For FT-IR, the materials were tested individually and mixed with root dentine powder. Scanning electron microscopy (SEM) and coupled energy dispersive spectroscopy (EDS) were used to evaluate surface and chemical elements. ISO 6876-2012 and ASTM-C266-07 specifications were followed to evaluate flow, setting time (moist and dry), solubility and radiopacity. Also, pH analysis at 37 and 100 °C was performed. Shapiro-Wilk and Mixed ANOVA (within and between the effects of the subjects), Levene, and a post hoc analyses with Bonferroni correction were performed (P < 0.05). RESULTS: Vibrational spectroscopy revealed peaks of tricalcium silicate, dicalcium silicate and zirconium dioxide. Chemical changes in the Raman spectra during heating were discrete, as the inorganic content predominated the signalling for all root canal sealers. FT-IR analysis exhibited spectral changes in water absorption for EndoSequence BC Sealer HiFlow and Bio-C Sealer, probably related to dehydration. For BioRoot RCS and AH Plus, no significant chemical changes were observed. Bio-C Sealer exhibited a band of polyethylene glycol only after heating to 100 °C, probably related to its thermal decomposition. SEM/EDS analysis corroborated the composition results observed in vibrational spectroscopy for all materials. Heating to 100 °C significantly changed the flowability of all calcium silicate-based sealers with a wide variation in setting times at both temperatures, along with solubility levels above ISO standards. For all tested sealers, radiopacity fulfilled the requirements, and pH exhibited alkaline values. CONCLUSIONS: The tested calcium silicate-based sealers were affected by heating. Calcium silicate-based root canal sealers had high solubility which is a concern for their clinical use. AH Plus was the only root canal sealer that was stable after heating.

Limited Etching Time Increases Self-adhesive Resin Cement Adhesion to Enamel.

AIM: To evaluate the influence of different enamel etching times on the bond strength of two self-adhesive resin cements (RCs) with and without thermocycling (TMC). METHODS: One hundred twenty bovine teeth were used. Blocks of enamel (8×4×2mm) were obtained, polished, and randomly divided into two groups, according to the RC used: MaxCem Elite or RelyX U200. Groups were subdivided into four groups (n=16), according to the etching time: Control (0 seconds), 5 seconds, 10 seconds, and 20 seconds. Three RC cylinders (1-mm diameter) were built on each enamel block. The specimens were submitted to two storage conditions: 24 hours in distilled water or TMC (5000 cycles/5°C-55°C). Afterward, the specimens were submitted to the shear bond strength (SBS) test. The failure modes and adhesive interfaces were analyzed by scanning electron microscopy (SEM) and confocal laser scanning microscopy (CLSM). Data were analyzed with three-way analysis of variance (ANOVA) and Tukey test (α=0.05). RESULTS: Etching increased the SBS for both the RCs,especially forthe groups etched for 5 and 10 seconds. TMC affected negatively the SBS of the control groups (p<0.05). No resin tags were observed in control groups, and the formation of tags was time dependent. CONCLUSION: The 10 seconds etching time was more effective in increasing the enamel-resin bond strength. TMC negatively affected bond strength in specimens without acid etching.