Physicochemical Properties of Methacrylate Resin-based Root Canal Sealers

Introduction: This study assessed in vitro the physicochemical properties of 2 methacrylate resin-based sealers (Epiphany SE and Hybrid Root SEAL), comparing the results with a well-established epoxy resin-based sealer (AH Plus). Methods: Five samples of each material were used for each test (setting time, flow, radiopacity, dimensional change after setting, and solubility) according to American National Standards Institute/American Dental Association (ANSI/ADA) Specification 57. The samples were assigned to 3 groups: I, AH Plus; II, Epiphany SE; and III, Hybrid Root SEAL. The distilled and deionized water used at the solubility test was submitted to atomic absorption spectrometry to observe the presence of Ca2+, K+, Ni2+, and Zn2+ ions. In addition, the surface morphology of the specimens was analyzed by means of scanning electron microscopy (SEM). Statistical analysis was performed by using one-way analysis of variance and Tukey-Kramer test (P < .05). Results: Flow, radiopacity, and solubility of all sealers were in accordance with ANSI/ADA. The setting time of Hybrid Root SEAL did not agree with ANSUADA requirements. The dimensional change of all sealers was greater than the values considered acceptable by ANSI/ADA. The spectrometry analysis showed significant Ca2+ ions release for AH Plus. In SEM analysis, Hybrid Root SEAL presented spherical monomers with inferior size than AH Plus and Epiphany SE. Conclusions: It might be concluded that physicochemical properties of the tested sealers conformed to ANSI/ADA (2000) standardization, except for the setting time of Hybrid Root SEAL and the dimensional change of all sealers, which did not fulfill the ANSI/ADA requirements. (J Endod 2010;36:1531-1536)

In vitro wear resistance of three types of polymethyl methacrylate denture teeth

The wear resistance of denture teeth is important to the longevity of removable prostheses of edentulous patients. The ability of denture teeth to maintain a stable occlusal relationship over time may be influenced by this property. The purpose of this in vitro study was to evaluate the wear resistance of polymethyl methacrylate (PMMA) denture teeth based on their chemical composition when opposed by a ceramic antagonist. The maxillary canines (n=10) of 3 PMMA denture teeth (Trubyte Biotone, cross-linked PMMA; Trilux, highly cross-linked IPN (interpenetrating polymer network)-PMMA; and Vivodent, highly cross-linked PMMA) were secured in an in vitro 2-body wear-testing apparatus that produced sliding contact of the specimens (4.5 cycles/s, sliding distance of 20 mm, under 37°C running water) against glazed or airborne particle abraded ceramic. Wear resistance was measured as height loss (mm) under 300 g (sliding force) after 100,000 cycles, using a digital measuring microscope. Mean values were analyzed by 2-way ANOVA and Tukey's test (a=0.05). The wear of Trubyte Biotone (0.93 ± 0.14 mm) was significantly higher than that of both other types of teeth tested against abraded ceramic (p<0.05). The Vivodent tooth (0.64 ± 0.17 mm) exhibited the best wear resistance among the denture teeth tested against airborne particle abraded ceramic. There were no statistically significant differences (p>0.05) in wear among the 3 denture teeth evaluated against glazed ceramic. Trilux and Vivodent teeth tested against either glazed or airborne particle abraded ceramic did not differ significantly from each other (p<0.05). All teeth showed significantly more wear against airborne particle abraded ceramic than against glazed ceramic (p<0.05). In conclusion, the three types of PMMA denture teeth presented significantly different wear resistance against the abraded ceramic. The high-strength PMMA denture teeth were more wear-resistant than the conventional PMMA denture tooth.

Effect of cerium (IV) ions on the anticorrosion properties of siloxane-poly(methyl methacrylate) based film applied on tin coated steel

This work investigates the influence of the addition of cerium (IV) ions on the anticorrosion properties of organic-inorganic hybrid coatings applied to passivated tin coated steel. In order to evaluate the specific effect of cerium (IV) addition on nanostructural features of the organic and inorganic phases of the hybrid coating, the hydrolytic polycondensation of silicon alkoxide and the radical polymerization of the methyl methacrylate (MMA) function were induced separately. The corrosion resistance of the coatings was evaluated by means of linear polarization, Tafel type curves and electrochemical impedance measurements. The impedance results obtained for the hybrid coatings were discussed based on an electrical equivalent circuit used to fit the experimental data. The electrochemical results clearly showed the improvement of the protective properties of the organic-inorganic hybrid coating mainly when the cerium (IV) was added to the organic phase solution precursor, which seemed to be due to the formation of a more uniform and densely reticulated siloxane-PMMA film. (C) 2010 Elsevier Ltd. All rights reserved.

Characterization of dimethacrylate polymeric networks: A study of the crosslinked structure formed by monomers used in dental composites

The resin phase of dental composites is mainly composed of combinations of dimethacrylate comonomers, with final polymeric network structure defined by monomer type/reactivity and degree of conversion. This fundamental study evaluates how increasing concentrations of the flexible triethylene glycol dimethacrylate (TEGDMA) influences void formation in bisphenol A diglycidyl dimethacrylate (BisGMA) co-polymerizations and correlates this aspect of network structure with reaction kinetic parameters and macroscopic volumetric shrinkage. Photopolymerization kinetics was followed in real-time by a near-infrared (NIR) spectroscopic technique, viscosity was assessed with a viscometer, volumetric shrinkage was followed with a linometer, free volume formation was determined by positron annihilation lifetime spectroscopy (PALS) and the sol-gel composition was determined by extraction with dichloromethane followed by (1)H NMR analysis. Results show that, as expected, volumetric shrinkage increases with TEGDMA concentration and monomer conversion. Extraction/(1)H NMR studies show increasing participation of the more flexible TEGDMA towards the limiting stages of conversion/crosslinking development. As the conversion progresses, either based on longer irradiation times or greater TEGDMA concentrations, the network becomes more dense, which is evidenced by the decrease in free volume and weight loss after extraction in these situations. For the same composition (BisGMA/TEGDMA 60-40 mol%) light-cured for increasing periods of time (from 10 to 600 s), free volume decreased and volumetric shrinkage increased, in a linear relationship with conversion. However, the correlation between free volume and macroscopic volumetric shrinkage was shown to be rather complex for variable compositions exposed for the same time (600 s). The addition of TEGDMA decreases free-volume up to 40 mol% (due to increased conversion), but above that concentration, in spite of the increase in conversion/crosslinking, free volume pore size increases due to the high concentration of the more flexible monomer. In those cases, the increase in volumetric shrinkage was due to higher functional group concentration, in spite of the greater free volume. Therefore, through the application of the PALS model, this study elucidates the network formation in dimethacrylates commonly used in dental materials. (C) 2010 Elsevier Ltd. All rights reserved.

Bis-GMA co-polymerizations: Influence on conversion, flexural properties, fracture toughness and susceptibility to ethanol degradation of experimental composites

Objectives. The aim of this study was to evaluate the influence of monomer content on fracture toughness (K(Ic)) before and after ethanol solution storage, flexural properties and degree of conversion (DC) of bisphenol A glycidyl methacrylate (Bis-GMA) co-polymers. Methods. Five formulations were tested, containing Bis-GMA (B) combined with TEGDMA (T), UDMA (U) or Bis-EMA (E), as follows (in mol%): 30B:70T; 30B:35T:35U; 30B:70U; 30B:35T:35E; 30B:70E. Bimodal filler was introduced at 80 wt%. Single-edge notched beams for fracture toughness (FT, 25 mm x 5 mm x 2.5 mm, a/w = 0.5, n = 20) and 10 mm x 2 mm x 1 mm beams for flexural strength (FS) and modulus (FM) determination (10 mm x 2 mm x 1 mm, n = 10) were built and then stored in distilled water for 24 h at 37 degrees C. All FS/FM beams and half of the FT specimens were immediately submitted to three-point bending test. The remaining FT specimens were stored in a 75%ethanol/25%water (v/v) solution for 3 months prior to testing. DC was determined with FT-Raman spectroscopy in fragments of both FT and FS/FM specimens at 24 h. Data were submitted to one-way ANOVA/Tukey test (alpha = 5%). Results. The 30B:70T composite presented the highest K(Ic) value (in MPa m(1/2)) at 24 h (1.3 +/- 0.4), statistically similar to 30B:35T:35U and 30B:70U, while 30B:70E presented the lowest value (0.5 +/- 0.1). After ethanol storage, reductions in K(Ic) ranged from 33 to 72%. The 30B:70E material presented the lowest reduction in FT and 30B:70U, the highest. DC was similar among groups (69-73%), except for 30B:70U (52 +/- 4%, p < 0.001). 30B:70U and 30B:35T:35U presented the highest FS (125 +/- 21 and 122 +/- 14 MPa, respectively), statistically different from 30B:70T or 30B:70E (92 +/- 20 and 94 +/- 16 MPa, respectively). Composites containing UDMA or Bis-EMA associated with Bis-GMA presented similar FM, statistically lower than 30B:35T:35U. Significance. Composites formulated with Bis-GMA:TEGDMA:UDMA presented the best compromise between conversion and mechanical properties. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Push-out strength of methacrylate resin-based sealers to root canal walls

P>Aim To assess the push-out strength of Epiphany SE, Epiphany and Hybrid Root SEAL to the dentine walls of root canals. Methodology Sixty roots of canines were prepared and distributed to six groups (n = 10) according to the filling material: GI - Epiphany SE, GII - Epiphany primer and sealer, GIII - Epiphany primer, sealer and resinous solvent, GIV - Clearfil DC Bond and Epiphany sealer, GV - Clearfil, Epiphany sealer and solvent and GVI - Hybrid Root SEAL. Resilon cones were used in all groups. Roots were sectioned transversally to obtain three slices from each third. One slice was subjected to the push-out test (MPa), and results were analysed by anova and Tukey`s test (P < 0.05). The other two slices were prepared for scanning electron microscopy (SEM). Failure mode was also analysed. Results A statistically significant difference (P < 0.05) occurred between Hybrid Root SEAL (5.27 +/- 2.07) and the other materials, GI (0.40 +/- 0.23), GII (0.78 +/- 0.45), GIII (0.57 +/- 0.28), GIV (0.40 +/- 0.24) and GV (0.50 +/- 0.41), which did not differ significantly from each other (P > 0.05). Adhesive failures predominated in groups I, II, IV and V, whilst mixed and cohesive failures were the most frequent in groups III and VI, respectively. There were gaps in the adhesive interface of GI and GII, continuity areas of the filling material with dentine in GIV and GV and good adaptation of the interface of GVI. Conclusion Hybrid Root SEAL had greater push-out strength to root canal dentine than Epiphany SE and Epiphany. The use of primer, solvent and adhesive system did not influence the adhesion of Epiphany.

Effect of methyl methacrylate monomer on bond strength of denture base resin to acrylic teeth

Bond failures at the acrylic teeth and denture base resin interface are still a common clinical problem in prosthodontics. The effect of methyl methacrylate (MMA) monomer on the bond strength of three types of denture base resins (Acron MC, Lucitone 550 and QC-20) to two types of acrylic teeth (Biotone and Trilux) was evaluated. Twenty specimens were produced for each denture base resin/acrylic tooth combination and were randomly divided into control (acrylic teeth received no surface treatment) and experimental groups (MMA was applied to the surface of the acrylic teeth for 180 s) and were submitted to shear tests (1 mm/mm). Data (MPa) were analyzed using three-way ANOVA/Student`s test (alpha = 0.05). MMA increased the bond strength of Lucitone denture base resins and decreased the bond strength of QC-20. No difference was detected for the bond strength of Acron MC base resin after treatment with MMA. (C) 2008 Elsevier Ltd. All rights reserved.

De-aggregation of polyfluorene derivative by blending with a series of poly(alkyl methacrylate)s with varying sidegroup sizes

A polyfluorene derivative of the PPV, poly(9,9`-n-dihexyl-2,7-fluorenedilvinylene-alt-1,4-phenylenevinylene), with a strong tendency to aggregation was blended with several members of a series composed by poly(alkyl methacrylate)s with the following substituents in the ester position: methyl, ethyl, isopropyl, isobutyl, n-butyl, and cyclohexyl. The de-aggregation effect in blends was studied by steady-state photoluminescence spectroscopy using several blend compositions. The efficiency of each dispersing phase was discussed in terms of the polymer miscibility, controlled by interaction parameters between the polyfluorene and every poly(alkyl methacrylate)s, here described using Hilde-brand solubility parameters. (c) 2009 Elsevier Ltd. All rights reserved.

Structure-Activity Relationship for Quaternary Ammonium Compounds Hybridized with Poly(methyl methacrylate)

Hybrid films from poly (methylmethacrylate) (PMMA) and dioctadecyldimethylammonium bromide (DODAB), cetyltrimethylammonium bromide (CTAB), or tetrapropylammonium bromide (TPAB) were characterized by determination of wettability, ellipsometry, atomic force microscopy, active compounds diffusion to water, X-ray photoelectron spectroscopy (XPS) with determination of atomic composition on the films surface, and biocidal activity against Pseudomonas aeruginosa or Staphylococcus aureus. QAC mobility in the films increased from DODAB to CTAB to TPAB. Diffusion and optimal hydrophobic hydrophilic balance imparted the highest bioactivity to CTAB. DODAB sustained immobilization at the film surface killed bacteria upon contact. TPAB ability to diffuse was useless because of its unfavorable hydrophobic hydrophilic balance for bioactivity.

Ab Initio Analysis of Monomers and Dimers of Trialkylphosphine Oxides: Structural and Thermodynamic Stability

Structural and thermodynamic stabilities of monomers and dimers of trialkylphosphine oxides (TRPO) were Studied using quantum chemistry calculations. Density functional theory calculations were carried Out and the structures Of four TRPO have been determined: TMPO (methyl; R = CH(3)), TEPO (ethyl; R = CH(3)CH(2)), TBPO (n-butyl; R = CH(3)(CH(2))(3)), and TOPO (n-octyl; R = CH(3)(CH(2))(7)). TRPO homodimers were investigated considering two isomeric possibilities for each dimer. Relative binding energies and the enthalpic and entropic contributions to the Gibbs free energy were Calculated for all dimers. The formation of dimers from the individual monomeric TRPO species as a function of temperature was also analyzed. (C) 2008 Wiley Periodicals, Inc. Int J Quantum Chem 109: 250-258, 2009

Fluorescent probes with malononitrile side group in methyl methacrylate copolymers

Fluorescent probes derivated from auramine, 1-aminopyrene, and 9-aminoacridine containing a malononitrile group are copolymerized with methyl methacrylate. These new fluorescent polymeric materials are studied in solution of different solvents by steady-state and time-resolved emission techniques. Their spectroscopic properties and excited state dynamics are driven by charge transfer from the aromatic group to the electron withdrawing CN groups, and this factor is responsible for the non-exponential emission decay behavior. (c) 2008 Elsevier B.V. All rights reserved.

Evaluation of the light polymerization efficiency of copolymers used in dental formulations by differential scanning calorimetry

Different compositions of visible-light-curable triethylene glycol dimethacrylate/bisglycidyl methacrylate copolymers used in dental resin formulations were prepared through copolymerization photoinitiated by a camphorquinone/ethyl 4-dimethylaminobenzoate system irradiated with an Ultrablue IS light-emitting diode. The obtained copolymers were evaluated with differential scanning calorimetry. From the data for the heat of polymerization, before and after light exposure, obtained from exothermic differential scanning calorimetry curves, the light polymerization efficiency or degree of conversion of double bonds was calculated. The glass-transition temperature also was determined before and after photopolymerization. After the photopolymerization, the glass-transi-tion temperature was not well defined because of the breadth of the transition region associated with the properties of the photocured dimethacrylate. The glass-transition temperature after photopolymerization was determined experimentally and compared with the values determined with the Fox equation. In all mixtures, the experimental value was lower than the calculated value. Scanning electron microscopy was used to analyze the morphological differences in the prepared copolymer structures. (C) 2007 Wiley Periodicals, Inc.

Evaluation of Postpolymerization as a Function of the Storage Time of Triethylene Glycol Dimethacrylate/2,2-Bis[4-(2-Hydroxy-3-Methacryloxy-Prop-1-Oxy)-Phenyl]-propane Bisphenyl-alpha-Glycidyl Ether Dimethacrylate Copolymers Used in Dental Resins by Differential Scanning Calorimetry and Dynamic Mechanical Analysis

The aim of this work was to evaluate the effect of the storage time on the thermal properties of triethylene glycol dimethacrylate/2,2-bis[4-(2-hydroxy-3-methacryloxy-prop-1-oxy)-phenyl]propane bisphenyl-alpha-glycidyl ether dimethacrylate (TB) copolymers used in formulations of dental resins after photopolymerization. The TB copolymers were prepared by photopolymerization with an Ultrablue IS light-emitting diode, stored in the dark for 160 days at 37 degrees C, and characterized with differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and Fourier transform infrared spectroscopy with attenuated total reflection. DSC curves indicated the presence of an exothermic peak, confirming that the reaction was not completed during the photopolymerization process. This exothermic peak became smaller as a function of the storage time and was shifted at higher temperatures. In DMA studies, a plot of the loss tangent versus the temperature initially showed the presence of two well-defined peaks. The presence of both peaks confirmed the presence of residual monomers that were not converted during the photopolymerization process. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 112: 679-684, 2009

Thioxanthone Sensitized Photodegradation of Poly(alkyl methacrylate) Films

The thioxanthone-sensitized photodegradation of poly(alkyl methacrylate) films [alkyl = methyl, ethyl, butyl, and hexyl] was studied using near UV-vis light. The photooxidation process continued even after the total consumption of the sensitizer, possibly due to the excitation of the ketyl groups formed during the first stages of the process. The rate of oxidation, as well as the formation of hydroxy, peroxy, and ketyl groups was faster for polymers with larger ester groups. The decrease of the molecular weight of the degradated polymers was also larger for the hexyl substituted polymer. The side-chain size effect was attributed to the larger amount of secondary hydrogens available for abstraction by the triplet state of thioxanthone, present in the larger ester groups. The lower glass transition temperature of the hexyl substituted polymer allows a better diffusion of oxygen to the deeper layers of the films that also contributes to the faster photodegradation rate. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 115: 1283-1288, 2010

FiltekTM Silorane and FiltekTM Supreme XT resins: tissue reaction after subcutaneous implantation in isogenic mice

The aim of this study was to evaluate the tissue compatibility of a silorane-based resin system (FiltekTM Silorane) and a methacrylate-based nanoparticle resin (FiltekTM Supreme XT) after implantation in the subcutaneous connective tissue of isogenic mice. One hundred and thirty five male isogenic BALB/c mice were randomly assigned to 12 experimental and 3 control groups, according to the implanted material and the experimental period of 7, 21 and 63 days. At the end of each period, the animals were killed and the tubes with the surrounding tissues were removed and processed for microscopic analysis. Samples were subjected to a descriptive and a semi-quantitative analyses using a 4-point scoring system (0-3) to evaluate the collagen fiber formation and inflammatory infiltrate. Data were statistically analyzed using the Kruskal Wallis test (?=0.05). The results showed that there was no significant difference between the experimental and control groups considering the three evaluation periods (p>0.05). The silorane-based and the methacrylate-based nanoparticle resins presented similar tissue response to that of the empty tube (control group) after subcutaneous implantation in isogenic mice.