Effects of water storage of E-glass fiber reinforced denture base polymers on residual methyl methacrylate content

This study investigated the effect of water storage on residual methyl methacrylate (MMA) content of continuous E-glass fiber (Wetrotex International) reinforced denture base polymers. Heat-polymerization (short- and long-term boiling and conventional curing cycle using Meliodent), autopolymerization (processed in air at room temperature and in water at 60 degrees C with the use of Meliodent Rapid Repair), and microwave-polymerization (3 min at 500 W with the use of Acron MC) were employed. The residual MMA contents of 120 specimens were analyzed by high-performance liquid chromatography at deflasking (control) and after water (37 degrees C) storage of 1 day, 1 week, and 1 month. Bonferroni's pairwise comparison test was used for statistical analysis. Significant reduction were determined only in the long-term terminal boiled heat-polymerized test group at the end of 1 day (p < 0.01), 1 week (p < 0.05) and also 1 month of water storage (p < 0.01). Significant reduction in autopolymerized test groups started even after 1 week of water storage (p < 0.05). Microwave-polymerized test groups did not show a significant residual MMA reduction in all time intervals (p > 0.05). The polymerization methods and cycles applied to the glass fiber reinforced denture base polymers influence both the content and the reduction of residual MMA after water storage.     

Evaluation of polymerization of light-curing hybrid composite resins

The quality of polymerization of hybrid composite resins was tested to explore their feasibility for dental restorations. For this, microhardness, polymerization shrinkage, the coefficient of thermal expansion, and surface morphology were evaluated during or after light curing in conjunction with the thermocycling process. Each product had different microhardness values. The repeated thermal stimulus has no specific effect on the change of microhardness. The difference of microhardness between the thermocycled specimens and specimens stored only in distilled water was minor. The measured microhardness had a linear correlation with the filler content (vol %) of the tested specimens. The polymerization shrinkage had rapidly increased only during the light curing, and then it reached a plateau. Among the specimens, Z250 showed the least amount of shrinkage for all tested thicknesses. Regardless of the product, the shrinkage values increased as the specimens became thick. The coefficient of thermal expansion of the control specimens ranged between 42 and 55 microm/degrees C in the temperature range of 30-80 degrees C. The coefficient showed an inverse correlation with the filler content. Through the thermocycling process, Palfique Estelite showed randomly propagating cracks on the surface. Larger fillers showed a more apparent detachment than the smaller fillers.     

Creep studies of multiphase acrylic systems

The influence of type and quantity of five different crosslinking agents on tensile creep properties of multiphase acrylic systems has been studied. The polymeric materials, commonly applied in bioengineering, were processed by polymerization of a mixture of liquid methacrylate monomers and poly(methyl methacrylate) powder. The specimens were made with various ratios of methyl methacrylate and crosslinking agents in the monomer liquid. Two different processing conditions were used, i.e., heat-polymerization at 100 degrees C and autopolymerization at 45 degrees C. Creep behavior was determined at 37 +/- 0.2 degrees C and 50 +/- 0.5 degrees C. The investigation showed higher creep values for autopolymerized than for heat-polymerized materials. In heat-polymerized materials the creep curves showed little variation with type and quantity of crosslinking agents at low stress levels. However, at high stress levels the creep values decreased with increasing quantity of crosslinking agents. The autopolymerized materials showed a more inhomogeneous structure, and great variation in creep. Both among the heat-polymerized and autopolymerized materials, the systems with diethyleneglycol dimethacrylate clearly deviated from the others by showing higher creep values.     

Loss into water of residual monomer from autopolymerizing dental acrylic resin

A study has been made of the loss of residual monomer from samples of autopolymerizing acrylic resin immersed in water. Diffusion of monomer out of the resin into the water could account for only part of the loss. It was shown that free radicals continue to be present in the acrylic after completion of cure, and it is postulated that the residual monomer in an autopolymerized acrylic resin may be removed by further polymerization at these sites, as well as by diffusion out of the resin. The implications of this hypothesis are discussed.     

Dynamic mechanical properties of multiphase acrylic systems

The influence of type and quantity of five different dimethacrylate crosslinking agents on the dynamic mechanical properties of multiphase acrylic systems has been studied. These materials, commonly used in bioengineering, were processed by polymerization of a mixture of liquid methacrylate monomers, and poly(methyl methacrylate) powder. The specimens were made with various ratios of methyl methacrylate and dimethacrylate crosslinking agents in the monomer liquid. Two different processing conditions were used, heat-polymerization at 100 degrees C and autopolymerization at 45 degrees C. By using a forced torsional vibration apparatus the storage modulus (G'), loss modulus (G"), and dissipation factor (tan delta) were determined over the temperature range -60 degrees C to 140 degrees C at frequencies of 0.1, 1.0, 10, and 100 rad/s. In the autopolymerized materials, the glass transition temperature (Tg), as determined via tan delta data, increased with increasing quantities of crosslinking agents. The storage modulus likewise increased. In the heat-polymerized materials only minor variations in modulus and tan delta with type and quantity of crosslinking agents were observed. Tg values of the heat-polymerized materials were, in all cases, greater than those of the autopolymerized materials.     

Determination of residual stresses in denture base polymers using the layer removal technique

In order to study the influence of residual stresses on dimensional accuracy and mechanical properties of denture bases, an experimental model was devised for measurement of residual stresses in acrylic denture base polymers. Rectangular bar coupons were cut from resin plates heat processed by conventional dental methods. They included samples which had been slow and fast cooled after polymerization and had been stored in dry and wet environments. Uniaxial residual stress distributions for each coupon were disclosed by removing layers of known thicknesses and measuring the ensuing deflection of the specimens. Coupons of a commercial acrylic resin were annealed and used as controls. ANOVA and Scheffe's test were used to compare experimental conditions at the 95% confidence level. Dry specimens exhibited residual surface compressive stresses from 0.43-0.83 MPa (62-120 psi). Water-stored specimens showed higher stress levels, 2.86-3.24 MPa (414-470 psi). Slow cooled pigmented acrylic coupons which were dry showed higher residual stresses compared with other dry but nonpigmented specimens. No significant differences were found between pigmented or clear coupons which contained moisture.     

Polymerization- and solvent-induced phase separation in hydrophilic-rich dentin adhesive mimic

Current dental resin undergoes phase separation into hydrophobic-rich and hydrophilic-rich phases during infiltration of the over-wet demineralized collagen matrix. Such phase separation undermines the integrity and durability of the bond at the composite/tooth interface. This study marks the first time that the polymerization kinetics of model hydrophilic-rich phase of dental adhesive has been determined. Samples were prepared by adding varying water content to neat resins made from 95 and 99 wt.% hydroxyethylmethacrylate and 5 and 1 wt.% (2,2-bis[4-(2-hydroxy-3-methacryloxypropoxy)phenyl1]-propane prior to light curing. Viscosity of the formulations decreased with increased water content. The photopolymerization kinetics study was carried out with a time-resolved Fourier transform infrared spectrometer. All of the samples exhibited two-stage polymerization behavior which has not been reported previously for dental resin formulation. The lowest secondary rate maxima were observed for water contents of 10–30 wt.%. Differential scanning calorimetry (DSC) showed two glass transition temperatures for the hydrophilic-rich phase of dental adhesive. The DSC results indicate that the heterogeneity within the final polymer structure decreased with increasing water content. The results suggest a reaction mechanism involving both polymerization-induced phase separation and solvent-induced phase separation for the model hydrophilic-rich phase of dental resin.     

HPLC analysis of eluted monomers from two composite resins cured with LED and halogen curing lights

This study investigated the leaching of monomers (Bis-GMA and TEGDMA) from nano-hybrid (Filtek Supreme) and flowable (Filtek Flow) dental composite resins cured with LED or conventional halogen curing lights, and immersed in saliva or water for 24 h. Nine disc specimens were made for each experimental group. After the polymerization process, the specimens were immersed in either water or saliva and incubated at 37 degrees C for 24 h. Eluted Bis-GMA and TEGDMA monomers were detected using high performance liquid chromatography (HPLC). The data were analyzed using three-way ANOVA (p = 0.05) and the independent samples t test. TEGDMA (53.15-1 microg/L) was leached from the resins at a higher level than Bis-GMA (28-0.5 microg/L) (p < 0.01), regardless of the affecting factors: composite type, solvent (media) and type of curing light. In general, Filtek Flow resin released more TEGDMA than Filtek Supreme (p < 0.05), but the Supreme resin released more Bis-GMA than TEGDMA (p < 0.05). Halogen light induced greater monomer elution than LED light immersion in water. Saliva released more TEGDMA than water (p < 0.05). We conclude that (1) total leached TEGDMA was higher than total Bis-GMA, (2) saliva and halogen light (lower intensity than LED) leached more monomers from the resins, and (3) the flowable composite resin leached more TEGDMA than the nano-hybrid.     

Light-curing efficiency of dental adhesives by gallium nitride violet-laser diode determined in terms of ultimate micro-tensile strength

The purpose of this study was to evaluate whether violet-laser diode (VLD) can be used as light-curing source. The ultimate (micro-)tensile strength (μTS) of three adhesives was determined when cured by VLD in comparison with curing by two different types of commercial LED light-curing units. One VLD (VLM 500) and two LED units (Curenos and G-Light Prima) were used to cure the adhesive resin of the two-step self-etch adhesives Clearfil SE Bond, Tokuso Mac Bond II, and FL-Bond II. A 0.6-mm thick acrylic mould was filled with adhesive resin and cured for 60 s. After 24-h water storage, specimens were trimmed into an hourglass shape with a width of 1.2 mm at the narrowest part, after which the μTS was determined (n=10). In addition, the light transmittance of each adhesive was characterized using a UV-vis-NIR spectrometer. No significant difference in curing efficiency between VLD and LED were observed for both Tokuso Mac Bond II and FL-Bond II (p>0.05). For Clearfil SE Bond, the μTS of VLD-cured specimens was higher than that of the specimens cured by the LED Curenos unit (p<0.05). Spectrometry revealed that this marked difference must be attributed to a different light transmittance of Clearfil SE Bond for visible blue light versus for the lower area of UV and visible violet light. In conclusion, A GaN-based violet laser diode can be used as light-curing source to initiate polymerization of dental resins.     

Effects of resin hydrophilicity on water sorption and changes in modulus of elasticity

As acidic monomers of self-etching adhesives are incorporated into dental adhesives at high concentrations, the adhesive becomes more hydrophilic. Water sorption by polymers causes plasticization and lowers mechanical properties. The purpose of this study was to compare the water sorption and modulus of elasticity (E) of five experimental neat resins (EX) of increasing hydrophilicity, as ranked by their Hoy's solubility parameters and five commercial resins. METHODS: After measuring the initial modulus of all resin disks by biaxial flexure, half the specimens were stored in hexadecane and the rest were stored in water. Repeated measurements of stiffness were made for 3 days. Water sorption and solubility measurements were made in a parallel experiment. RESULTS: None of the specimens stored in oil showed any significant decrease in modulus. All resins stored in water exhibited a time-dependent decrease in modulus that was proportional to their degree of water sorption. Water sorption of EX was proportional to Hoy's solubility parameter for polar forces (delta(p)) with increasing polarity resulting in higher sorption. The least hydrophilic resin absorbed 0.55 wt% water and showed a 15% decrease in modulus after 3 days. The most hydrophilic experimental resin absorbed 12.8 wt% water and showed a 73% modulus decrease during the same period. The commercial resins absorbed between 5% and 12% water that was associated with a 19-42% reduction in modulus over 3 days.     

Elution study of unreacted Bis-GMA, TEGDMA, UDMA, and Bis-EMA from light-cured dental resins and resin composites using HPLC

In the present work the elution of residual monomers from light-cured dental resins and resin composites into a 75% ethanol:water solution was studied using High-Performance Liquid Chromatography (HPLC). The resins studied were made by light-curing of bisphenol A glycol dimethacrylate (Bis-GMA), triethylene glycol dimethacrylate (TEGDMA), urethane dimethacrylate (UDMA), ethoxylated bisphenol A glycol dimethacrylate [Bis-EMA(4)] and mixtures of these monomers. The resin composites were made from two commercial light-cured restorative materials (Z100 MP and Filtek Z250), the resin matrix of which is based on copolymers of these monomers. The effect of the curing time on the amount of monomers eluted was investigated. The concentration of the extractable monomers was determined at several immersion periods from 3 h to 30 days. For all the materials studied, it was observed that the chemical structure of the monomers used for the preparation of the resins, which defines the chemical and physical structure of the corresponding resin, directly affects the amount of eluted monomers, as well as the time needed for the elution of this amount. In the case of composites, it seems that the elution process it is not influenced by the presence of filler.     

Comparison of the fracture resistance of six denture base acrylic resins

Fracture strength of denture base resins is of great concern, and many approaches have been used to strengthen acrylic resin dentures. Fracture resistance of six commercially available acrylic resin denture base materials were compared, through impact and transverse strength tests. Three rapid heat-polymerised resins (QC 20, Meliodent and Trevalon), two high-impact strength resins (Trevalon Hi and Lucitone 199) and a strengthened injection-moulded acrylic resin (SR Ivocap plus) were included in the study. Twenty acrylic resin test specimens were fabricated from each resin. For impact strength test, ten notched specimens were tested in a Charpy-type impact tester. The other ten specimens were used for transverse strength tests, deflection and modulus of elasticity values were also determined, which were assessed with three-point bending tests using an Universal Testing Machine. Impact test values showed significant differences among acrylic resins (F= 4.817 p = 0.0). SR Ivocap resin showed the highest impact strength values, followed by Trevalon Hi and Lucitone 199. The transverse strength test values were not significant when six acrylic resins were compared (F= 1.705 p = 0.151). High-impact resins can be recommended to increase the impact strength of denture base. If the cause of fracture is mechanical or anatomical, strengthened acrylic resins and conventional acrylic resins have similar fracture resistance.     

Effect of resin hydrophilicity and water storage on resin strength

This study evaluated the change in the ultimate tensile strength (UTS) of five polymerised resin blends of increasing hydrophilicity, after ageing in distilled water or silicon oil. Resin blocks were prepared from each resin blend by dispensing the uncured resin into a flexible, embedding mould, containing multiple cavities. The resins were polymerised in the moulds under nitrogen at 551.6 kPa and light-activated at 125 degrees C for 10 min. After dry ageing for 24 h at 37 degrees C, the middle third of each resin specimen was trimmed into an 'I' shape. Fifteen control specimens were randomly selected from each resin blend for baseline UTS evaluation. The UTS of the experimental specimens were determined after 1, 3, 6 and 12 months of ageing in water or oil. The UTS of each group of resins at different storage periods in water or oil were analysed using the Friedman multiple ANOVA on ranks and Dunn's multiple comparison tests at 95% confidence level. Significant reduction (p < 0.01) in UTS was observed in Groups II-V resins after 12-month storage in water, while the most hydrophobic Group I resin showed no significant change (p > 0.05) in the same period. The percentage reduction in UTS increased with the hydrophilicity of the resin blends. Long-term water storage of hydrophilic resin blends such as those employed in dentine adhesives, resulted in a marked reduction in their mechanical strength that may compromise the durability of resin-dentine bonds.     

The effect of temperature on viscoelastic properties of glass ionomer cements and compomers

The objective of this study was to determine the viscoelastic properties of different types of glass ionomer cements (GICs) and compomers under varying temperature conditions found in the mouth. The materials tested were a conventional GIC (Aqua Ionofil U), a resin modified GIC (Fuji II LC), a highly viscous GIC (Voco Ionofil Molar), and two polyacid modified composite resins/compomers (Glasiosite and Dyract Flow). Six groups of four specimens were prepared from each material. One group was stored dry for 24 h and was subsequently tested dry at 21 degrees C. Each of the remaining five groups was stored for 24 h in distilled water at the temperatures 21, 30.5, 37, 43.5, and 50 degrees C, respectively, and was subsequently tested at that temperature. Shear storage modulus and loss tangent were determined by conducting dynamic torsional loading. Static shear moduli were determined by applying a constant torque (below the proportional limit of the materials) for 10 s and recording the angular deformation of the specimens. Data were analyzed by ANOVA and Duncan's test (alpha= 0.05). It was found that the viscoelastic properties varied significantly (p < 0.05) across the different materials. The compomer Glasiosite, with the highest filler content, and the highly viscous GIC Voco Ionofil Molar exhibited the highest elastic moduli and lowest loss tangents. Viscoelastic properties varied also significantly (p < 0.05) with temperature levels, but changes in the tested region were not indicative of a glass transition. Dynamic shear storage moduli were highly correlated to the static ones. Storage in water lowered the values of elastic moduli.     

The effect of different power densities and method of exposure on the marginal adaptation of four light-cured dental restorative materials

PURPOSE: To determine whether marginal adhesion is sensitive to different irradiation parameters, we investigated the in vitro adhesion values of four dental resins on metal surfaces. METHODS: Four groups of eight specimens each of Z250, Filtek flow, Dyract AP and Dyract flow were placed in pre-treated stainless steel cavities and irradiated using different methods of exposure. The curing lights used were a Spectrum 800 halogen curing light at settings of 800 and 450 mW/cm(2) and an Optilux 501 ramping light. The maximum amount of push-out force required to displace the resin from the metal cavity was equated with adhesive value (shear bond strength). Comparisons (ANOVA, p<0.0001) were made within the same material and between the different materials when using different curing protocols. RESULTS: Significant lower bond strengths were recorded when curing was done by gradually increasing the intensity (ramping method) compared to curing with the fixed intensities (p>0.0001) Comparing the fixed intensities, significant lower bond strength values were obtained at 800 mW/cm(2) compared to 450 mW/cm(2) (p<0.0001). For all exposures, the two flowable materials demonstrated weaker values when compared to the higher filled materials. CLINICAL SIGNIFICANCE: The advantage of initial slow polymerization (more elasticity and less tension) obtained by the so-called "soft start" method, was offset by a rise in total polymerization shrinkage, when final curing was completed at 1130 mW/cm(2). These tests demonstrated that using halogen units, exposure for 40s with an intensity of 450 mW/cm(2) appeared to be the most promising for light-curing dental resin composites.     

Oligomers with pendant isocyanate groups as tissue adhesives: II. Adhesion to bone and other tissues

The adhesive properties of a series of oligomers prepared from 2-isocyanatoethyl methacrylates (IEM) and/or m-isopropenyl-alpha,alpha-dimethylbenzyl isocyanate (TMI) and various acrylates or methacrylates were studied. The bond strength of bone, dentin, or soft tissue specimens joined with these oligomers respectively to bone, dental composite restorative, or denture base resin were determined by tensile adhesion or shear tests. These oligomers are more effective in forming stronger bonds to bone than are other tissue adhesives. Fracture occurs cohesively, usually within the bone. Thermocycling in water for 1 week between 5 degrees C and 55 degrees C did not decrease adhesion indicating that exposure to water or thermal shock produced no deterioration of the bond. Tensile adhesion of bovine or human dentin joined to composite restorative resin by means of the oligomers is similar to that of the best dental bonding agents such as Gluma (glutaraldehyde and 2-hydroxyethyl methacrylate) or ferric oxalate + N-phenylglycine + dimethylacryloxyethyl-pyromellitate. These oligomers also strongly bond soft tissues and calfskin and to acrylic resins and composites.     

Dendrimer/methyl methacrylate co-polymers: residual methyl methacrylate and degree of conversion

Dendrimer/methyl methacrylate co-polymers were studied for use in dental composites. The aim was to determine the effects of methyl methacrylate concentration in the resin mixture and polymerization method on the degree of conversion and residual monomer content of the copolymers. Two dendrimers were studied, D12 with 12 reactive methacrylate groups and D24 with 24 reactive groups. The concentration of methyl methacrylate varied from 20 wt% to 50 wt% of monomers. Camphorquinone (CQ) was used as the light-activation initiator and 2-(N,N-dimethylamino)ethyl methacrylate (DMAEMA) as the activator, both in the quantity of 3.0 wt%. Three polymerization methods were used: photo-polymerization, photo-polymerized immediately followed by post-polymerization at 120 degrees C for 15 min, and photo-polymerization followed by postpolymerization after 7 days. The degree of conversion was determined using FT-IR. Residual monomers were extracted with tetrahydrofuran and methanol and analyzed with HPLC. The highest degrees of conversion were 65 and 62%, and the lowest residual monomer contents 1.0 and 1.5% for D12 and D24, respectively. These were measured after heat-induced post-polymerization. For D12, increasing the proportion of methyl methacrylate decreased the degree of conversion and increased the residual monomer content after photo-polymerization. Post-polymerization enhanced the polymerization of the dendrimer co-polymers in respect of degree of conversion and residual monomer content. The present study suggested that the tested dendrimer/methyl methacrylate copolymers require heat-induced polymerization to reach the generally accepted levels of degree of conversion and residual monomers.     

Internal adaptation and some physical properties of methacrylate-based denture base resins polymerized by different techniques

This study evaluated the internal adaptation, porosity, transverse and impact strength of three denture base polymers: (1) conventional heat-polymerized, (2) microwave-polymerized, and (3) injection-molded resins. Internal adaptation was measured by weighing a vinyl polysiloxane film reproducing the gap between the denture base and the metallic master model of an edentulous maxilla. The measurements were performed immediately after finishing and after 30-day storage in water. Porosity was evaluated by weighing each specimen in air and in water using an analytical scale balance. Transverse strength test (three-point bending test) was performed using a universal machine under axial load, at a crosshead speed of 5 mm/min. Impact strength test (Charpy's test) was performed with a 40 kJ/cm load. Data were analyzed by ANOVA and Tukey test (alpha = 0.05). Internal adaptation, porosity, transverse and impact strength varied according to the type of acrylic resin and the processing technique. The injection-molded resin showed better internal adaptation compared with the conventional heat-polymerized and the microwave-polymerized resins, particularly after 30 days, but there was no relevant improvement of porosity, transverse and impact strength.     

Bond strength of adhesively luted ceramic discs to different core materials

The purpose of this in vitro study was to compare the shear bond strengths of resin, glass-ionomer, and ceramic-based core materials to all ceramic discs. Five core materials (Core max, Sankin; Clearfil AP-X, Kuraray; Empress Cosmo, Ivoclar-Vivadent; Photocore, Kuraray; Dyract Extra, Dentsply) were prepared as discs 10 mm in diameter and 2 mm in height according to the manufacturer's instructions. Ten disc specimens per group were prepared, and dentin served as the control. All resin specimens were embedded in autopolymerizing acrylic resin, with one surface facing up. All ceramic discs (IPS Empress I, Ivoclar-Vivadent) 3 mm in diameter and 2 mm in height were prepared and bonded to core specimens with a dual-curing luting resin cement (Variolink II, Vivadent). Specimens were stored in distilled water at 37 degrees C. Shear bond strength of each sample was measured after 24 h using a universal testing machine at a crosshead speed of 0.5 mm/min. The data were analyzed with one-way analysis of variance and Tukey HSD tests (alpha = 0.05). Shear bond strength varied significantly depending on the core material used (p < 0.05). Clearfil AP-X and Photocore showed the highest shear bond strength value while Empress Cosmo provided the lowest (p < 0.05). There were no statistically significant differences among Clearfil AP-X, Photocore, and Core-Max (p > 0.05). And also there were no statistically significant differences between Dyract Extra and the control group (p > 0.05). In vitro shear bond strengths of ceramic discs bonded to resin-based core materials showed higher bond strength values than ceramic-based core material.     

Thermal expansion characteristics of light-cured dental resins and resin composites

The thermal expansion characteristics of dental resins prepared by light-curing of Bis-GMA, TEGDMA, UDMA, Bis-EMA(4) or PCDMA dimethacrylate monomers and of commercial light-cured resin composites (Z-100 MP, Filtek Z-250, Sculpt-It and Alert), the organic matrix resin of which is based on different combinations of the above monomers, were studied by thermomechanical analysis (TMA). This study showed the existence of a glass transition temperature at around 35-47 degrees C for the resins and 40-45 degrees C for the composites; then the coefficient of linear thermal expansion (CLTE) was calculated at the temperature intervals 0-60 degrees C, 0-T(g) and T(g)-60 degrees C. The CLTE values of Bis-GMA, TEGDMA and UDMA resins are similar and lower than those of Bis-EMA (4) and PCDMA resins. The CLTE values of the composites indicated that the major factor that affects the CLTE of a composite is the filler content, but it also seems to be affected by the chemical structure of the matrix resin. TMA on water-saturated samples showed that water desorption takes place during the measurement and that the residual water acts as a plasticizer decreasing the T(g) and increasing the CLTE values. Furthermore, TMA on post-heated samples for 1, 3 or 6h showed, only for the resins, an initial decrease of CLTE and increase of the T(g) after 1h that was not significantly changed after 6h of heating.