Cesar Augusto Galvão Arrais

Effect of curing mode on the polymerization characteristics of dual-cured resin cement systems

OBJECTIVES To evaluate the effects of different curing conditions on the degree of conversion (DC) of dual-cured cementing systems [combination of bonding agent (BA) and resin cement (RC)] using infrared spectroscopy. METHODS Four fourth generation products [Scotchbond Multipurpose Plus/RelyX (3M ESPE), Optibond/Nexus 2 (Kerr), All Bond2/Duolink (Bisco), and Bond-It!/Lute-It! (Pentron)], and three fifth generation materials [Bond1/Lute-It! (Pentron), Prime&Bond NT Dual-Cure/Calibra (Dentsply), and Optibond Solo Dual Cure/Nexus 2 (Kerr)] were applied to the surface of a horizontal attenuated-total-reflectance unit, and were polymerized using one of four conditions: self-cure (SC), direct light exposure through glass slide (DLE, XL3000/3M ESPE) or through pre-cured resin discs (shades A2;A4/2mm thick/Z250/3M ESPE). Infrared spectra of the uncured cementing systems were recorded immediately after application to the ATR, after the system was light-cured or left to self-cure, and spectra were obtained 5 and 10 min later. DC was calculated using standard techniques of observing changes in aliphatic-to-aromatic peak ratios pre- and post-curing. Data (n=5) were analyzed by two-way repeated measures ANOVA and Tukeys test (p=0.05). RESULTS Changes in aliphatic-to-aromatic peak ratios before and after placing RC onto the BA demonstrated that a combined layer was created. All groups exhibited higher DC after 10 min than after 5 min, except the DLE group of Bond-it!/Lute-it!. No significant differences in DC were observed among light-activated groups regardless of the resin disc shade in three of the four fourth generation cementing systems. The SC groups exhibited lower DC than the DLE groups for both fourth and fifth generation products either after 5 or 10 min. CONCLUSION The chemistry of the bonding interface changed when RCs were applied to uncured BAs. The presence of an indirect restoration can decrease the DC of some cementing systems and the self-curing mode leads to lower DC than the light-activating one.

Effect of sodium sulfinate salts on the polymerization characteristics of dual-cured resin cement systems exposed to attenuated light-activation

OBJECTIVES To evaluate the effectiveness of sodium sulfinate salt co-initiators on the degree of conversion (DC) of dual-cured cementing systems [combination of bonding agent (BA) and resin cement (RC)] when the activating light is attenuated or not available. METHODS Two 5th generation products [Prime&Bond NT Dual-Cure/Calibra (Dentsply), and Excite DSC/Variolink II (Ivoclar/Vivadent)] were applied, either with or without co-initiators (sodium sulfinate salts) added to the bonding agents, to the surface of a horizontal attenuated-total-reflectance unit, and were polymerized using one of four conditions: self-cure (SC), or direct light exposure (DLE/XL3000/3M) through a glass slide or through pre-cured resin discs (shades A2 or A4/2mm-thick) (Z250/3M-ESPE). Real-time infrared spectra were obtained after placing components (uncured) and during 10 min (cured) (16 scans at 2 cm(-1), FTS-40/Digilab/Bio-Rad) to obtain polymerization kinetics. DC and maximum rate of polymerization (Rpmax) were calculated using standard techniques of observing changes in aliphatic-to-aromatic peak ratios pre- and post-curing. Data (n=5) were analyzed by two-way ANOVA and Tukeys test (p=0.05). RESULTS The addition of co-initiators increased the DC in most of the groups. No significant difference in DC was observed between Prime Bond NT Dual-Cure/Calibra and its version without co-initiator using the DLE curing mode. All DLE groups exhibited the highest DC after 10 min. No significant difference in DC was observed between A2 and A4 pre-cured overlay groups. The SC groups exhibited lower DC than the light-activated groups regardless of the presence of co-initiator. Use of co-initiators increased the Rpmax only in the SC groups. The A2 and A4 groups exhibited lower Rpmax than DLE groups, regardless of the presence of co-initiator. CONCLUSION The detrimental effects of light attenuation on the DC were not avoided by inclusion of sodium sulfinate salts, despite their ability to eliminate the chemical incompatibility between acidic monomers and self-curing components.

Kinetic analysis of monomer conversion in auto- and dual-polymerizing modes of commercial resin luting cements

STATEMENT OF PROBLEM Lack of knowledge regarding the kinetics of the setting reaction of dual- and autopolymerizing resin luting agents (RLA) leads the clinician to underestimate the care required during occlusal adjustments of indirect restorations. PURPOSE The purpose of this study was to evaluate the degree of conversion (DC), maximum rate of polymerization (R(p)(max)), and potential of cure (ratio of conversions in autopolymerized relative to dual-polymerized modes; PC(A/D)) of 5 dual-polymerizable RLAs at 5 and 10 minutes, after mixing RLA components using infrared (IR) spectroscopy. MATERIAL AND METHODS The RLAs evaluated included Calibra, Duo-Link, Lute-It, Nexus 2, and RelyX ARC. The RLAs were manipulated and applied to the horizontal diamond element in the optical bench of an IR spectrometer. The materials were either light activated for 40 seconds (dual-polymerizing mode) or were allowed to autopolymerize (autopolymerizing mode). The DC, R(p)(max), and PC(A/D) were calculated using standard techniques of observing changes in aliphatic-to-aromatic peak ratios before and after polymerization. Data (n=5) were analyzed by 2-way repeated measures ANOVA and Tukeys post hoc test (alpha=.05). RESULTS All autopolymerizing groups exhibited lower DC and R(p)(max) values than the dual-polymerizing groups (P<.001), and higher DC values at 10 minutes than at 5 minutes, only in the autopolymerizing mode. Duo-Link exhibited the highest R(p)(max) values among dual-polymerizing groups, while Lute-It and Calibra showed the lowest R(p)(max) values and the highest PC(A/D) values. Within autopolymerizing groups, Nexus 2 and Lute-It exhibited the highest R(p)(max) values, while RelyX ARC demonstrated the lowest R(p)(max) as well as the lowest PC(A/D) values. CONCLUSIONS The DC values of all autopolymerized groups of RLAs were lower than those of the dual-polymerized RLAs, but the differences in R(p)(max) and PC(A/D) were product dependent. The DC of all products was higher at the 10-minute interval than at the 5-minute interval, only in the autopolymerizing mode.

Occluding effect of dentifrices on dentinal tubules

OBJECTIVES The objective of this study was to evaluate the tubule occluding ability of three commercial available dentifrices (Sensodyne, Emoform and Sorriso) by Scanning Electron Microscopy. METHODS Fifty cervical areas from buccal and lingual surfaces of sound third human molars were used. Cervical enamel was wet abraded to expose flat dentin surfaces and further polished with diamond pastes. Specimens were randomly divided into five groups (n=10): G1-no brushing; G2-brushing without dentifrice; G3-brushing with Sensodyne; G4-brushing with Emoform; G5-brushing with Sorriso. Brushed specimens were treated for 4 min per day, for 7 days in a toothbrushing machine. Specimens were prepared and observed under SEM for calculation of the percentage of occluded tubules. In addition, slurries of toothpastes were analyzed by X-ray microanalysis. Data were statistically analyzed by ANOVA and Tukey test (p<0.05). RESULTS Means of occluded tubules in descending order were: G5-98.83+/-3.31% (a), G4-96.02+/-5.24% (a), G3-80.12+/-24.65% (a), G1-37.31+/-24.22% (b); G2-22.92+/-15.19% (b). The three tested dentifrices produced increased dentinal occlusion as compared to controls (p<0.05) but equivalent occlusion among each other. Calcium from calcium-carbonate abrasive was identified in all dentifrices. CONCLUSIONS Results indicated that the use of all dentifrices occluded tubules more than no brushing and brushing without dentifrices groups. Thus, the tested dentifrices seem effective for desensitization by tubule occlusion.

Effects of desensitizing agents on dentinal tubule occlusion

The aim of this study was to evaluate the features of dentinal tubules occlusion following application of three commercially available desensitizing agents: potassium oxalate-based / Oxa-Gel (OX), HEMA and glutaraldehyde-based / Gluma Desensitizer (GD) and acidulated phosphate fluoride-based / Nupro Gel (AF). Buccal cervical areas of twenty-four extracted human third molars were smoothed and wet-polished with SiC papers and diamond pastes, in order to simulate the clinical aspect of hypersensitive dentin cervical surfaces. The teeth were randomly divided into four groups (n=6), according to the dentin surface treatments: G1: untreated; G2: OX; G3: GD; G4: AF. Specimens were fractured in the lingual-buccal direction and prepared for SEM analysis. OX promoted tubule occlusion by crystal-like deposits in the lumen of the tubules. While GL created a thin layer over the dentin surface, AF application produced precipitates that occluded the tubules. According to the SEM analysis, all desensitizing agents were able to occlude the dentinal tubules.

Influence of Curing Mode and Time on Degree of Conversion of One Conventional and Two Self-adhesive Resin Cements

This study evaluated the effect of curing mode (auto- and dual-polymerizing mode) and time interval (5, 10 and 15 minutes) on the degree of conversion of resin cements. One conventional dual-cured resin cement (Panavia F 2.0 [Kuraray Medical Inc]) and two self-adhesive cements (RelyX Unicem [3M ESPE] and BisCem [BISCO, Inc]) were evaluated. The products (n = 5) were manipulated according to the manufacturers instructions and applied to the surface of a horizontal attenuated reflectance unit attached to an infrared spectrometer. The materials were either light-cured for 40 seconds (dual-polymerizing mode) or allowed to auto-polymerize. The degree of conversion was calculated according to changes in the aliphatic-to-aromatic peak ratios prior to and 5, 10 and 15 minutes after light-activation or after mixing when the specimens were allowed to auto-polymerize. Data (%) were analyzed by two-way repeated measure ANOVA (curing mode and time interval) and Tukeys post-hoc test (alpha = 0.05%). The light-activating mode led to a higher degree of conversion values than the self-curing mode in self-adhesive cements (RelyX Unicem and BisCem), while there was no difference in the degree of conversion between the self- and light-cured groups of Panavia F 2.0 resin cement. All products showed a higher degree of conversion at 15 minutes postcuring than any other evaluation interval. The self-adhesive cements provide a higher degree of conversion values when light-activated. After 15 minutes of polymerization initiation, the degree of conversion was higher in all resin cements, regardless of the curing mode.

Degree of conversion of adhesive systems light-cured by LED and halogen light

This study evaluated the effect of blue light emitting diode (LED) and quartz tungsten halogen (QTH) on the degree of conversion (DC) of an etch-and-rinse Single Bond adhesive system (SB) and a mixture composed of primer solution and resin bond from Clearfil SE Bond self-etching adhesive system (CB) using Fourier transform infrared analysis (FTIR). Adhesives were applied to potassium bromide pellet surfaces and FTIR analyses were performed before and after photo-activation for 10 s with either LED (Freelight 1 - 400 mw/cm(2)) or QTH (XL 3000 - 630 mw/cm(2)) light-curing units (n=8). Additional FTIR spectra were obtained from photo-activated samples stored in distilled water for 1 week. The DC was calculated by comparing the spectra obtained from adhesive resins before and after photo-activation. The results were analyzed by two-way split-plot ANOVA and Tukeys test (p<0.05). Both adhesive systems exhibited low DC (%) immediately after photo-activation (SB/QTH: 18.7 +/- 3.9; SB/LED: 13.5 +/- 3.3; CF/QTH: 13.6 +/- 1.9; CF/LED: 6.1 +/- 1.0). The DC of samples light-cured with LED was lower than DC of those light-cured with QTH, immediately after light curing and after 1 week (SB/QTH: 51.3 +/- 6.6; SB/LED: 50.3 +/- 4.8; CF/QTH: 56.5 +/- 2.9; CF/LED: 49.2 +/- 4.9). The LED curing unit used to photo-activate the adhesive resins promoted lower DC than the QTH curing unit both immediately after light curing and 1 week after storage in water.

Effect of Temperature on the Degree of Conversion and Working Time of Dual-Cured Resin Cements Exposed to Different Curing Conditions

OBJECTIVES This study evaluated the degree of conversion (DC) and working time (WT) of two commercial, dual-cured resin cements polymerized at varying temperatures and under different curing-light accessible conditions, using Fourier transformed infrared analysis (FTIR). MATERIALS AND METHODS Calibra (Cal; Dentsply Caulk) and Variolink II (Ivoclar Vivadent) were tested at 25°C or preheated to 37°C or 50°C and applied to a similar-temperature surface of a horizontal attenuated-total-reflectance unit (ATR) attached to an infrared spectrometer. The products were polymerized using one of four conditions: direct light exposure only (600 mW/cm(2)) through a glass slide or through a 1.5- or 3.0-mm-thick ceramic disc (A2 shade, IPS e.max, Ivoclar Vivadent) or allowed to self-cure in the absence of light curing. FTIR spectra were recorded for 20 min (1 spectrum/s, 16 scans/spectrum, resolution 4 cm(-1)) immediately after application to the ATR. DC was calculated using standard techniques of observing changes in aliphatic-to-aromatic peak ratios precuring and 20-min postcuring as well as during each 1-second interval. Time-based monomer conversion analysis was used to determine WT at each temperature. DC and WT data (n=6) were analyzed by two-way analysis of variance and Tukey post hoc test (p=0.05). RESULTS Higher temperatures increased DC regardless of curing mode and product. For Calibra, only the 3-mm-thick ceramic group showed lower DC than the other groups at 25°C (p=0.01830), while no significant difference was observed among groups at 37°C and 50°C. For Variolink, the 3-mm-thick ceramic group showed lower DC than the 1-mm-thick group only at 25°C, while the self-cure group showed lower DC than the others at all temperatures (p=0.00001). WT decreased with increasing temperature: at 37°C near 70% reduction and at 50°C near 90% for both products, with WT reduction reaching clinically inappropriate times in some cases (p=0.00001). CONCLUSION Elevated temperature during polymerization of dual-cured cements increased DC. WT was reduced with elevated temperature, but the extent of reduction might not be clinically acceptable.

Effects of the Solvent Evaporation Technique on the Degree of Conversion of One-Bottle Adhesive Systems

This study evaluated the effect of four methods of solvent evaporation on the degree of conversion (DC) of seven one-bottle adhesive systems: Excite (EX), ONE-STEP (OS), Optibond Solo Plus (OB), Prime&Bond 2.1 (PB), Prime&Bond NT (NT), Single Bond (SB) and Single Bond Plus (SP) using Fourier Transform Infrared Analysis (FTIR). Adhesive resins were: 1) applied to KBr pellet surfaces and left undisturbed for 30 seconds (condition 1), 2) left undisturbed for 30 seconds and air-dried with an air stream for 10 seconds (condition 2), 3) left undisturbed for 60 seconds (condition 3) and 4) left undisturbed for 60 seconds and air-dried for 10 seconds (condition 4) before curing. FTIR spectra were obtained and the DC was calculated by comparing the ratio of aliphatic/aromatic double carbon bonds before and after light-activation for 10 seconds (XL 3000, 3M). The results of each product were analyzed by one-way repeated measure ANOVA and post-hoc Tukeys test (p<0.05). The DC of PB, NT, OB and SP adhesives was not affected by the four evaporation conditions, while the DC of EX, OS and SB changed according to the evaporation method. The results suggested that the DC of some adhesives was similar regardless of the evaporation method when no water from dentin or rinsing was involved. Other bonding agents showed higher DC after specific conditions of solvent evaporation.

Morphology and thickness of the diffusion of resin through demineralized or unconditioned dentinal matrix.

The formation of a hybrid layer is the main bonding mechanism of current dentin-bonding systems. This study evaluated the morphology and thickness of the resin-infiltrated dentinal layer after the application of adhesive systems. The dentin-bonding agents were evaluated on flat dentinal preparations confected on the occlusal surfaces of human teeth. The test specimens were prepared and inspected under scanning electron microscopy at a magnification of X 2,000. The adhesive systems were responsible for different hybrid layer thicknesses (p < 0.05), and the mean values were: for Scotchbond MP Plus (SM), 7.41 +/- 1.24 micrometer for Single Bond (SB), 5.55 +/- 0.82 micrometer for Etch & Prime 3.0 (EP), 3.86 +/- 1.17 micrometer and for Clearfil SE Bond (CB), 1.22 +/- 0.45 micrometer. The results suggest that the conventional three-step adhesive system (SM) was responsible for the thickest hybrid layer, followed by the one-bottle adhesive (SB). The self-etching adhesives, EP and CB, produced the formation of the thinnest hybrid layers.