The Interaction Between N-Isopropylacrylamide-Acrylic Acid-Ethyl Methacrylate Thermosensitive Polymers and Cationic Surfactants

The interaction between cationic surfactants and isopropylacrylamide-acrylic acid-ethyl methacrylate (IPA:AA:EMA) terpolymers has been investigated using steady-state fluorescence and spectrophotometric measurements to assess the effect of the polymer composition on the aggregation process and terpolymers' thermosensitivities. Micropolarity studies using pyrene show that the interaction of cationic surfactants with IPA:AA:EMA terpolymers occurs at surfactant concentrations much smaller than that observed for the pure surfactant in aqueous solution. The critical aggregation concentration (CAC) values decrease with both the hydrocarbon length of the surfactant and the content of ethyl methacrylate. These results were interpreted as a manifestation of the increasing contribution of attractive hydrophobic and electrostatic forces between negatively charged polymer chains and positively charged surfactant molecules. The increase of ethyl methacrylate in the copolymers lowers the CAC due to the larger hydrophobic character of the polymer backbone. The cloud point determination reveals that the lower critical solution temperatures (LCST) depend strongly on the copolymer composition and surfactant nature. The binding of surfactants molecules to the polymer chain screens the electrostatic repulsion between the carboxylic groups inducing a conformational transition and the dehydration of the polymer chain.

Fluorescence probe study of the interaction between acrylic acid-co-ethyl methacrylate copolymers and sodium dodecylsulfate

The interaction between sodium dodecylsulfate (SDS) and acrylic acid (AA)-ethyl methacrylate (EMA) copolymers has been investigated using steady state fluorescence and conductimetric measurements to assess the effect of the polymer composition on the aggregation process. Micropolarity studies using the ratio between the emission intensities of the vibronic bands of pyrene (I-1/I-3) and the shift of the fluorescence emission of pyrene-3-carboxaldehyde show, that the interaction of SDS with AA-EMA copolymers occurs at surfactant concentrations smaller than that observed for the pure surfactant in water and depends on the copolymer composition. The increase of ethyl methacrylate in the copolymers lowers the critical aggregation concentration (CAC) due to the larger hydrophobic character of the polymer backbone. The formation of aggregates on the macromolecule is induced mainly, by hydrophobic interactions, but the process is also influenced by the ionic strength due to the counter-ions of the polyelectrolyte.

Aqueous solution behavior of thermosensitive (N-isopropylacrylamide-acrylic acid-ethyl methacrylate) terpolymers

A series of N-isopropylacrylamide (NIPAM)-acrylic acid-ethyl methacrylate terpolymers with varied monomer compositions was prepared by radical polymerization. The solution behavior of these polymers was studied in dilute aqueous solution using spectrophotometry, fluorescence spectroscopy and high-sensitivity differential scanning calorimetry. The results obtained revealed that the lower critical solution temperatures depend strongly on the copolymer composition, solution pH and ionic strength. At a high pH, the ionization of acrylic acid (AA) units leads to an increase in solution cloud points (T-c). Solutions of polymers containing 10% or less of AA display a constant T-c for pH above 5.5, with 15% there is a continuous increase in T-c with pH and, for higher AA contents, no clouding was observed within the studied temperature range. Fluorescence probe studies were conducted by following the I (1)/I (3) ratio of pyrene vibronic bands and the emission of anilinonaphtalene sulfonic acid, sodium salt (ANS), both approaches revealing the existence of hydrophobic domains for polymers with higher ethyl methacrylate content at temperatures lower than T-c, suggesting some extent of aggregation and/or a coil-to-globule transition. Scanning calorimetry measurements showed an endothermic transition at temperatures agreeing with the previously detected cloud points. Moreover, the transition curves became broader and with a smaller transition enthalpy, as both the AA content and the solution pH were increased. These broader transitions were interpreted to be the result of a wider molecular distribution upon polymer ionization, hence, displaying varied solution properties. The decrease in transition enthalpy was rationalized as a consequence of reminiscent hydration of NIPAM units, even after phase separation, owing to the presence of electric charges along the polymer chain.

One-step glycerol oxidehydration to acrylic acid on multifunctional zeolite catalysts

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Unrestricted linear dimensional changes of two hard chairside reline resins and one heat-curing acrylic resin

The selection and use of hard chairside reline resins must be made with regard to dimensional stability, which will influence the accuracy of fit of the denture base. This study compared the dimensional change of two hard chairside reline resins (Duraliner II and Kooliner) and one heat-curing denture base resin (Lucitone 550). A stainless steel mold with reference dimensions (AB, CD) was used to obtain the samples. The materials were processed according to the manufacturer's recommendations. Measurements of the dimensions were made after processing and after the samples had been stored in distilled water at 37° C for eight different periods of time. The data were recorded and then analyzed with analysis of variance. All materials showed shrinkage immediately after processing (p < 0.05). The only resin that exhibited shrinkage after 60 days of storage in water was Duraliner II; these changes could be clinically significant in regard of tissue fit.

Water sorption, solubility, and bond strength of two autopolymerizing acrylic resins and one heat-polymerizing acrylic resin.

STATEMENT OF PROBLEM: Because water sorption of autopolymerizing acrylic reline resins is accompanied by volumetric change, it is a physical property of importance. As residual monomer leaches into the oral fluids and causes tissue irritation, low solubility of these resins is desired. Another requirement is a satisfactory bond between the autopolymerizing acrylic resins and the denture base acrylic resin. PURPOSE: This study compared the water sorption, solubility, and the transverse bond strength of 2 autopolymerizing acrylic resins (Duraliner II and Kooliner) and 1 heat-polymerizing acrylic resin (Lucitone 550). MATERIAL AND METHODS: The water sorption and solubility test was performed as per International Standards Organization Specification No. 1567 for denture base polymers. Bond strengths between the autopolymerizing acrylic resins and the heat-polymerizing acrylic resin were determine with a 3-point loading test made on specimens immersed in distilled water at 37 degrees C for 50 hours and for 30 days. Visual inspection determined whether failures were adhesive or cohesive. RESULTS: Duraliner II acrylic resin showed significantly lower water sorption than Kooliner and Lucitone 550 acrylic resins. No difference was noted in the solubility of all materials. Kooliner acrylic resin demonstrated significantly lower transverse bond strength to denture base acrylic resin and failed adhesively. The failures seen with Duraliner II acrylic resin were primarily cohesive in nature. CONCLUSIONS: Autopolymerizing acrylic reline resins met water sorption and solubility requirements. However, Kooliner acrylic resin demonstrated significantly lower bond strength to denture base acrylic resin.

Effect of Surface Treatments on the Bond Strength between Composite Resin and Acrylic Resin Denture Teeth

Purpose: This investigation studied the effects of 3 surface treatments on the shear bond strength of a light-activated composite resin bonded to acrylic resin denture teeth. Materials and Methods: The occlusal surfaces of 30 acrylic resin denture teeth were ground flat with up to 400-grit silicon carbide paper. Three different surface treatments were evaluated: (1) the flat ground surfaces were primed with methyl methacrylate (MMA) monomer for 180 seconds; (2) light-cured adhesive resin was applied and light polymerized according to the manufacturer's instructions; and (3) treatment 1 followed by treatment 2. The composite resin was packed on the prepared surfaces using a split mold. The interface between tooth and composite was loaded at a cross-head speed of 0.5 mm/min until failure. Results: Analysis of variance indicated significant differences between the surface treatments. Results of mean comparisons using Tukey's test showed that significantly higher shear bond strengths were developed by bonding composite resin to the surfaces that were previously treated with MMA and then with the bonding agent when compared to the other treatments. Conclusion: Combined surface treatment of MMA monomer followed by application of light-cured adhesive resin provided the highest shear bond strength between composite resin and acrylic resin denture teeth.

Effect of microwave treatments on dimensional accuracy of maxillary acrylic resin denture base

Microwave energy has been used as an alternative method for disinfection and sterilization of dental prostheses. This study evaluated the influence of microwave treatment on dimensional accuracy along the posterior palatal border of maxillary acrylic resin denture bases processed by water-bath curing. Thirty maxillary acrylic bases (3-mm-thick) were made on cast models with Clássico acrylic resin using routine technique. After polymerization and cooling, the sets were deflasked and the bases were stored in water for 30 days. Thereafter, the specimens were assigned to 3 groups (n=10), as follows: group I (control) was not submitted to any disinfection cycle; group II was submitted to microwave disinfection for 3 min at 500 W; and in group III microwaving was done for 10 min at 604 W. The acrylic bases were fixed on their respective casts with instant adhesive (Super Bonder®) and the base/cast sets were sectioned transversally in the posterior palatal zone. The existence of gaps between the casts and acrylic bases was assessed using a profile projector at 5 points. No statistically significant differences were observed between the control group and group II. However, group III differed statistically from the others (p<0.05). Treatment in microwave oven at 604 W for 10 min produced the greatest discrepancies in the adaptation of maxillary acrylic resin denture bases to the stone casts.

Effect of disinfectants on the hardness and roughness of reline acrylic resins

Purpose: Potential effects on hardness and roughness of a necessary and effective disinfecting regimen (1% sodium hypocholorite and 4% chlorhexidine) were investigated for two hard chairside reline resins versus a heat-polymerizing denture base acrylic resin. Materials and Methods: Two standard hard chairside reliners (Kooliner and Duraliner II), one heat-treated chairside reliner (Duraliner II +10 minutes in water at 55°C), and one standard denture base material (Lucitone 550) were exposed to two disinfecting solutions (1% sodium hypochlorite; 4% chlorhexidine gluconate), and tested for two surface properties [Vickers hardness number (VHN, kg/mm2); Roughness (Ra, μm)] for different times and conditions (1 hour after production, after 48 hours at 37 ± 2°C in water, after two disinfection cycles, after 7 days in disinfection solutions, after 7 days in water only). For each experimental condition, eight specimens were made from each material. Data were analyzed by analysis of variance followed by Tukey's test, and Student's t-test (p= 0.05). Results: For Kooliner (from 6.2 ± 0.3 to 6.5 ± 0.5 VHN) and Lucitone 550 (from 16.5 ± 0.4 to 18.4 ± 1.7 VHN), no significant changes in hardness were observed either after the disinfection or after 7 days of immersion, regardless of the disinfectant solution used. For Duraliner II (from 4.0 ± 0.1 to 4.2 ± 0.1 VHN), with and without heat treatment, a small but significant increase in hardness was observed for the specimens immersed in the disinfectant solutions for 7 days (from 4.3 ± 0.2 to 4.8 ± 0.5 VHN). All materials showed no significant change in roughness (Kooliner: from 0.13 ± 0.05 to 0.48 ± 0.24 μm; Duraliner II, with and without heat treatment: from 0.15 ± 0.04 to 0.29 ± 0.07 μm; Lucitone 550: from 0.44 ± 0.19 to 0.49 ± 0.15 μm) after disinfection and after storage in water for 7 days. Conclusions: The disinfectant solutions, 1% sodium hypochlorite and 4% chlorhexidine gluconate, caused no apparent damage on hardness and roughness of the materials evaluated. Copyright © 2006 by The American College of Prosthodontists.

Bond strength of acrylic teeth to denture base resin after various surface conditioning methods before and after thermocycling

This study aimed to evaluate the durability of adhesion between acrylic teeth and denture base acrylic resin. The base surfaces of 24 acrylic teeth were flatted and submitted to 4 surface treatment methods: SM1 (control): No SM; SM2: application of a methyl methacrylate-based bonding agent (Vitacol); SM3: air abrasion with 30-μm silicone oxide plus silane; SM4: SM3 plus SM2. A heat-polymerized acrylic resin was applied to the teeth. Thereafter, bar specimens were produced for the microtensile test at dry and thermocyled conditions (60 days water storage followed by 12,000 cycles). The results showed that bond strength was significantly affected by the SM (P < .0001) (SM4 = SM2 > SM3 > SM1) and storage regimens (P < .0001) (dry > thermocycled). The methyl methacrylate-based adhesive showed the highest bond strength.

The effect of water immersion on the shear bond strength between chairside reline and denture base acrylic resins: Basic science research

Purpose: The effect of water immersion on the shear bond strength (SBS) between 1 heat-polymerizing acrylic resin (Lucitone 550-L) and 4 autopolymerizing reline resins (Kooliner-K, New Truliner-N, Tokuso Rebase Fast-T, Ufi Gel Hard-U) was investigated. Specimens relined with resin L were also evaluated. Materials and Methods: One hundred sixty cylinders (20 × 20 mm) of L denture base resin were processed, and the reline resins were packed on the prepared bonding surfaces using a split-mold (3.5 × 5.0 mm). Shear tests (0.5 mm/min) were performed on the specimens (n = 8) after polymerization (control), and after immersion in water at 37°C for 7, 90, and 180 days. All fractured surfaces were examined by scanning electron microscopy (SEM) to calculate the percentage of cohesive fracture (PCF). Shear data were analyzed with 2-way ANOVA and Tukey's test; Kruskall-Wallis test was used to analyze PCF data (α = 0.05). Results: After 90 days water immersion, an increase in the mean SBS was observed for U (11.13 to 16.53 MPa; p < 0.001) and T (9.08 to 13.24 MPa, p = 0.035), whereas resin L showed a decrease (21.74 MPa to 14.96 MPa; p < 0.001). The SBS of resins K (8.44 MPa) and N (7.98 MPa) remained unaffected. The mean PCF was lower than 32.6% for K, N, and T, and higher than 65.6% for U and L. Conclusions: Long-term water immersion did not adversely affect the bond of materials K, N, T, and U and decreased the values of resin L. Materials L and U failed cohesively, and K, N, and T failed adhesively. © 2007 by The American College of Prosthodontists.

Influence of microwave polymerization method and thickness on porosity of acrylic resin

Purpose: This study evaluated the influence of polymerization cycle and thickness of maxillary complete denture bases on the porosity of acrylic resin. Materials and Methods: Two heat-activated denture base resins - one conventional (Clássico) and one designed for microwave polymerization (Onda-Cryl) - were used. Four groups were established, according to polymerization cycles: A (Onda-Cryl, short microwave cycle), B (Onda-Cryl, long microwave cycle), C (Onda-Cryl, manufacturing microwave cycle), and T (Clássico, water bath). Porosity was evaluated for different thicknesses (2.0, 3.5, and 5.0 mm; thicknesses I, II, and III, respectively) by measurement of the specimen volume before and after its immersion in water. The percent porosity data were submitted to Kruskal-Wallis for comparison among the groups. Results: The Kruskal-Wallis test detected that the combinations of the different cycles and thicknesses showed significant differences, and the mean ranks of percent porosity showed differences only in the thinnest (2.0 mm) microwave-polymerized specimens (A = 53.55, B = 40.80, and C = 90.70). Thickness did not affect the results for cycle T (I = 96.15, II = 70.20, and III = 82.70), because porosity values were similar in the three thicknesses. Conclusions: Microwave polymerization cycles and the specimen thickness of acrylic resin influenced porosity. Porosity differences were not observed in the polymerized resin bases in the water bath cycle for any thickness. © 2007 by The American College of Prosthodontists.

Effectiveness of six different disinfectants on removing five microbial species and effects on the topographic characteristics of acrylic resin

Purpose: The aim of this study was to evaluate the effectiveness of disinfectant solutions (1% sodium hypochlorite, 2% chlorhexidine digluconate, 2% glutaraldehyde, 100% vinegar, tabs of sodium perborate-based denture cleanser, and 3.8% sodium perborate) in the disinfection of acrylic resin specimens (n = 10/group) contaminated in vitro by Candida albicans, Streptococcus mutans, S. aureus, Escherichia coli, or Bacillus subtilis as measured by residual colony-forming unit (CFU). In a separate experiment, acrylic resin was treated with disinfectants to monitor potential effects on surface roughness, Ra (μm), which might facilitate microbial adherence. Materials and Methods: Three hundred fifty acrylic resin specimens contaminated in vitro with 1×10 6 cells/ml suspensions of standard strains of the cited microorganisms were immersed in the disinfectants for 10 minutes; the control group was not submitted to any disinfection process. Final counts of microorganisms per ml were performed by plating method for the evaluation of microbial level reduction. Results were compared statistically by ANOVA and Tukey's test (p ≤ 0.05). In a parallel study aiming to evaluate the effect of the tested disinfectant on resin surface, 60 specimens were analyzed in a digital rugosimeter before and after ten cycles of 10-minute immersion in the disinfectants. Measurements of superficial roughness, Ra (μm), were compared statistically by paired t-test (p ≤ 0.05). Results: The results showed that 1% sodium hypochlorite, 2% glutaraldehyde, and 2% chlorhexidine digluconate were most effective against the analyzed microorganisms, followed by 100% vinegar, 3.8% sodium perborate, and tabs of sodium perborate-based denture cleanser. Superficial roughness of the specimens was higher after disinfection cycles with 3.8% sodium perborate (p = 0.03) and lower after the cycles with 2% chlorhexidine digluconate (p = 0.04). Conclusion: Within the limits of this experiment, it could be concluded that 1% sodium hypochlorite, 2% glutaraldehyde, 2% chlorexidine, 100% vinegar, and 3.8% sodium perborate are valid alternatives for the disinfection of acrylic resin. © 2008 by The American College of Prosthodontists.

Influence of storage period and effect of different brands of acrylic resin on the dimensional accuracy of the maxillary denture base

The aim of this study was to evaluate the dimensional changes of denture bases made from different resins after different storage periods. For this purpose, 25 sets of plaster models/resin bases were prepared using 4 acrylic resins submitted to two types of polymerization: 1- QC-20 submitted to polymerization by microwave energy; 2- QC-20 submitted to polymerization by water hot bath; 3- Vipi Cril submitted to polymerization by water hot bath; 4- Vipi Wave submitted to polymerization by microwave energy; and 5- Onda Cryl submitted to polymerization by microwave energy. After polymerization, the specimens were sectioned for accuracy readings using a comparison microscope. Readings were taken at 3 points: the crests of the right (A) and left (B) ridges, and the median region of the palate, in 4 different periods. The data obtained were submitted to two-way ANOVA and Tukey's test at 5% significance level. The greatest distortions were found in the posterior palatal region of the base (M), with statistically significant difference (p<0.05) for the studied resins. All acrylic resins presented dimensional changes and the storage period influenced these alterations.

Effect of microwave disinfection on physical and mechanical properties of acrylic resins

This study evaluated the effect of microwave energy on the hardness, impact strength and flexural strength of the Clássico, Onda-Cryl and QC-20 acrylic resins. Aluminum die were embedded in metallic or plastic flasks with type III dental stone, in accordance with the traditional packing technique. A mixing powder/liquid ratio was used according to the manufacturer's instructions. After polymerization in water batch at 74°C for 9 h, boiling water for 20 min or microwave energy at 900 W for 10 min, the specimens were deflasked after flask cooling at room temperature, and submitted to finishing. Specimens non-disinfected and disinfected by microwave irradiation were submitted to hardness, impact and flexural strength tests. Each specimen was immersed in distilled water and disinfected in a microwave oven calibrated to 650 W for 3 min. Knoop hardness test was performed with 25 g load for 10 s, impact test was carried out using the Charpy system with 40 kpcm, and 3-point bending test with a crosshead speed of 0.5 mm/min until fracture. Data were submitted to statistical analysis by ANOVA and Tukey's test (α=0.05). Disinfection by microwave energy decreased the hardness of Clássico and Onda-Cryl acrylic resins, but no effect was observed on the impact and flexural strength of all tested resins.