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.

Two methods to simulate intrapulpal pressure: effects upon bonding performance of self-etch adhesives.

AIM: To evaluate the effects of two methods to simulate physiological pulpal pressure on the dentine bonding performance of two all-in-one adhesives and a two-step self-etch silorane-based adhesive by means of microtensile bond strength (µTBS) and nanoleakage surveys. METHODOLOGY: The self-etch adhesives [G-Bond Plus (GB), Adper Easy Bond (EB) and silorane adhesive (SIL)] were applied to flat deep dentine surfaces from extracted human molars. The restorations were constructed using resin composites Filtek Silorane or Filtek Z350 (3M ESPE). After 24 h using the two methods of simulated pulpal pressure or no pulpal pressure (control groups), the bonded teeth were cut into specimens and submitted to µTBS and silver uptake examination. Results were analysed with two-way anova and Tukey's test (P < 0.05). RESULTS: Both methods of simulated pulpal pressure led statistically similar µTBS for all adhesives. No difference between control and pulpal pressure groups was found for SIL and GB. EB led significant drop (P = 0.002) in bond strength under pulpal pressure. Silver impregnation was increased after both methods of simulated pulpal pressure for all adhesives, and it was similar between the simulated pulpal pressure methods. CONCLUSIONS: The innovative method to simulate pulpal pressure behaved similarly to the classic one and could be used as an alternative. The HEMA-free one-step and the two-step self-etch adhesives had acceptable resistance against pulpal pressure, unlike the HEMA-rich adhesive.

Effects of surface treatments, thermocycling, and cyclic loading on the bond strength of a resin cement bonded to a lithium disilicate glass ceramic.

SUMMARY Objectives : The aim of this present study was to investigate the effect of two surface treatments, fatigue and thermocycling, on the microtensile bond strength of a newly introduced lithium disilicate glass ceramic (IPS e.max Press, Ivoclar Vivadent) and a dual-cured resin cement. Methods : A total of 18 ceramic blocks (10 mm long × 7 mm wide × 3.0 mm thick) were fabricated and divided into six groups (n=3): groups 1, 2, and 3-air particle abraded for five seconds with 50-µm aluminum oxide particles; groups 4, 5, and 6-acid etched with 10% hydrofluoric acid for 20 seconds. A silane coupling agent was applied onto all specimens and allowed to dry for five seconds, and the ceramic blocks were bonded to a block of composite Tetric N-Ceram (Ivoclar Vivadent) with RelyX ARC (3M ESPE) resin cement and placed under a 500-g static load for two minutes. The cement excess was removed with a disposable microbrush, and four periods of light activation for 40 seconds each were performed at right angles using an LED curing unit (UltraLume LED 5, Ultradent) with a final 40 second light exposure from the top surface. All of the specimens were stored in distilled water at 37°C for 24 hours. Groups 2 and 5 were submitted to 3,000 thermal cycles between 5°C and 55°C, and groups 3 and 6 were submitted to a fatigue test of 100,000 cycles at 2 Hz. Specimens were sectioned perpendicular to the bonding area to obtain beams with a cross-sectional area of 1 mm(2) (30 beams per group) and submitted to a microtensile bond strength test in a testing machine (EZ Test) at a crosshead speed of 0.5 mm/min. Data were submitted to analysis of variance and Tukey post hoc test (p≤0.05). Results : The microtensile bond strength values (MPa) were 26.9 ± 6.9, 22.2 ± 7.8, and 21.2 ± 9.1 for groups 1-3 and 35.0 ± 9.6, 24.3 ± 8.9, and 23.9 ± 6.3 for groups 4-6. For the control group, fatigue testing and thermocycling produced a predominance of adhesive failures. Fatigue and thermocycling significantly decreased the microtensile bond strength for both ceramic surface treatments when compared with the control groups. Etching with 10% hydrofluoric acid significantly increased the microtensile bond strength for the control group.

Influence of the volume of composite and photoactivation method on push-out bond strength and Knoop hardness of a resin composite.

AIM: The aim of this paper was to evaluate the influence of modulated photoactivation methods and volume of composite on Knoop hardness (KHN) and push-out bond strength (PBS) of Filtek Z350 to root dentin. METHODS: Three volumes (small, medium and large) of composite were bulk inserted in cavities prepared in 90 premolars. The specimens were photoactivated with continuous light, pulse-delay, or soft-start methods and submitted to PBS and KHN tests. The failure pattern was evaluated in stereomicroscope after the bond strength test. The data were submitted to two-way ANOVA and Tukey's test (P<0.05). RESULTS: Modulated photoactivation methods showed a higher PBS than continuous method (P<0.05). Medium volume of composite showed higher PBS than small and large volumes when photoactivated with continuous method (P<0.05). Pulse-delay significantly increased KHN for medium and large volumes in comparison to continuous method (P<0.05). Medium volume of composite showed KHN significantly higher than small and large volumes (P<0.05). CONCLUSION: The volume of composite influenced the PBS and KHN of resin composites. Pulse-delay showed the highest bond strength to dentin, as well KHN similar to the conventional method. The analysis of the failure pattern showed predominance of adhesive failure.

Influence of natural weathering on colour stability of materials used for facial prosthesis.

Colour stability of resin and silicone is an important factor for longevity of facial prostheses. The aim of this study was to evaluate the colour stability of resins and silicone for facial prostheses. Three brands of acrylic resin and one of facial silicone were evaluated considering pigment incorporation for the colourless materials. Ten samples of each material were fabricated and submitted to measurements of chromatic alteration initially and after 90 and 180 days of weathering natural through visual analysis and spectrophotometry. Data were evaluated by ANOVA and Tukey test (p < 0.05). Statistically significant colour alteration was observed among some materials regardless of the period. The materials did not present a statistical difference between 90 and 180 days except for the pigmented heat-polymerized resin. The colour difference between pigmented Silastic MDX4-4210 and colourless Silastic was statistically significant (p < 0.01) in both periods as well as between pigmented and colourless heat-polymerized resin, and between the resins Rapidaflex and Lentaflex. The visual method demonstrated colour alteration in all materials evaluated during the first 90 days of ageing. All materials exhibited colour alteration due to exposure to environment.

Comparison between two methods to evaluate temperature changes produced by composite light curing units and polymerization techniques.

AIM: This study evaluated the temperature change into the pulp chamber during the light curing of composite resin by direct (bovine tooth) and indirect (matrix) methods. METHODS: Direct method: fifty standardized cavities (2x2x2 mm) were prepared in bovine incisors, which were randomly assigned to evaluation of the temperature changes in the pulp chamber. Indirect method: temperature changes were evaluated through a dentine slice of 1.0 mm thickness in a elastomer cubic mold (2x2x2 mm). Filtek Z250 composite resin (3M/ESPE) was photo-activated using three light curing units: quartz-tungsten-halogen (QTH) by continuous, soft-start or intermittent light modulations; light emitting diode (LED); and plasma arc-curing (PAC). Ten groups (N.=10) were established according to technique evaluation and photo-activation methods. All experiments were carried out in a controlled environment (37 °C and 50 ± 10% relative humidity). The temperature changes were recorded using a digital thermometer attached to a type-K thermocouple in contact with the dentin slice (indirect method) or in contact with the axial wall (dentin) of pulp chamber (direct method). The results were submitted to ANOVA and Tukey's test (α=0.05). RESULTS: Temperature changes were statistically higher for the matrix indirect method (2.56 ºC) than bovine teeth direct method (1.17ºC). The change temperature was statistically higher for the PAC (1.77 ºC) when compared to other photo-activation modes in bovine teeth direct method. CONCLUSION: The two methods of temperature evaluation were different, however indirect method detected the higher temperature increase. Higher energy density arising from the light curing units and polymerization techniques promoted higher temperature increase.

Radiodensity and hardness of enamel and dentin of human and bovine teeth, varying bovine teeth age.

Studies have evaluated dental hard tissues characteristics from animal species in order to be used as a substitute for human teeth. The aim of this study was to evaluate the radiodensity and hardness of human and bovine enamel and dentin, varying bovine teeth age. Five specimens (1mm thick) were obtained from animals aged 20 (B20), 30 (B30), 38 (B38) and 48 (B48)months and from 20 to 30-years-old human third molars (H). The radiographic images were taken with a phosphor plaque digital system (Digora Optime). The radiodensity was obtained and Knoop hardness (KHN) was recorded (100g for 15s--5 indentations per specimen). Data were analyzed by one-way ANOVA following Tukey's HSD test and Dunnet's two-sided t-test. Radiodensity was similar within enamel groups, but bovine dentin presented higher radiodensity than human one regardless of age groups. Enamel-KHN showed differences between B20-B30 and B38-B48-H, and dentin-KHN was similar within all groups. Enamel was always more radiodense than dentin and also presented higher KHN (p=0.001). The use of bovine enamel or dentin should take into consideration the teeth age, but as a general rule it should be recommended to select older bovine teeth due to better chances to find greater similarity with human teeth.

Radiopacity of root filling materials using digital radiography.

AIM: To evaluate radiopacity of root filling materials using digital radiography. METHODOLOGY: The sealers tested were AH Plus, Endofill, EndoREZ and Epiphany. Gutta-percha (Dentsply Maillefer) and Resilon cones were also tested. Acrylic plates, containing six wells, measuring 1 mm in depth and 5 mm in diameter, were prepared for the test, and filled with the materials. The test samples were radiographed together with an aluminium stepwedge calibrated in millimetres, according to ANSI/ADA Specification 57. For the radiographic exposures, digital imaging plates and an X-ray machine at 70 kVp and 8 mA were used. The object-to-focus distance was 30 cm, and the exposure time, 0.2 s. After the laser optic reading process, the software determined the radiopacity of the standardized areas, using grey-scale values, calculating the average radiographic density for each material. RESULTS: The decreasing values of radiopacity of the studied materials, expressed in millimetres of aluminium equivalent, were: Resilon (13.0), AH Plus(TM) (11.2), gutta-percha (9.8), Epiphany (8.0), Endofill (6.9) and EndoREZ (6.6). CONCLUSION: All materials had radiopacity values above 3 mm of aluminium recommended by ANSI/ADA Specification 57.

Effect of the photo-activation method on polymerization shrinkage of restorative composites.

This study measured the gap that resulted from polymerization shrinkage of seven restorative resin composites after curing by three different methods. Contraction behavior, according to the specimen region, was also characterized. The materials used for this study were Alert (Jeneric/Pentron, Wallingford, CT 06492, USA), Surefil (Dentsply Caulk, Milford, DE 19963, USA), P60 (3M Dental Products, St Paul, MN 55144, USA), Z250 (3M), Z100 (3M), Definite (Degussa-Hüls, Hanau, Germany) and Flow-it (Jeneric/Pentron). The composite was placed in a circular brass mold 7 mm in diameter and 2 mm in height. Photo-activation was performed by a) continuous light (500 mW/cm2) for 40 seconds; b) stepped light with low intensity (150 mW/cm2) for 10 seconds and high intensity (500 mW/cm2) for 30 seconds and c) intermittent light (450 mW/cm2) for 60 seconds. The top and bottom surfaces were then polished and after 24 +/- 1 hours, the contraction gap was measured by SEM at variable pressure (LEO 435 VP, Cambridge, England). Results were analyzed by ANOVA and the means compared by Tukey's test (5%). The results demonstrated 1) the continuous light method presented the greatest gap values (15.88 microm), while the other methods demonstrated lower polymerization shrinkage values (stepped light, 13.26 microm; intermittent light, 12.79 microm); 2) restorative composites shrunk more at the bottom surface (15.84 microm) than at the top surface (12.11 microm) and (3) the composites Alert (12.02 microm), Surefil (11.86 microm), Z250 (10.81 microm) and P60 (10.17 microm) presented the least contraction gaps, followed by Z100 (15.84 microm) and Definite (14.06 microm) and finally Flow-it (23.09 microm) low viscosity composite, which had the greatest mean value.