Influence of curing protocol on selected properties of light-curing polymers: Degree of conversion, volume contraction, elastic modulus, and glass transition temperature

Objectives. The purpose of this study was to investigate the effect of light-curing protocol on degree of conversion (DC), volume contraction (C), elastic modulus (E), and glass transition temperature (T(g)) as measured on a model polymer. It was a further aim to correlate the measured values with each other. Methods. Different light-curing protocols were used in order to investigate the influence of energy density (ED), power density (PD), and mode of cure on the properties. The modes of cure were continuous, pulse-delay, and stepped irradiation. DC was measured by Raman micro-spectroscopy. C was determined by pycnometry and a density column. E was measured by a dynamic mechanical analyzer (DMA), and T(g) was measured by differential scanning calorimetry (DSC). Data were submitted to two-and three-way ANOVA, and linear regression analyses. Results. ED, PD, and mode of cure influenced DC, C, E, and T(g) of the polymer. A significant positive correlation was found between ED and DC (r = 0.58), ED and E (r = 0.51), and ED and T(g) (r = 0.44). Taken together, ED and PD were significantly related to DC and E. The regression coefficient was positive for ED and negative for PD. Significant positive correlations were detected between DC and C (r = 0.54), DC and E (r = 0.61), and DC and T(g) (r = 0.53). Comparisons between continuous and pulse-delay modes of cure showed significant influence of mode of cure: pulse-delay curing resulted in decreased DC, decreased C, and decreased T(g). Influence of mode of cure, when comparing continuous and step modes of cure, was more ambiguous. A complex relationship exists between curing protocol, microstructure of the resin and the investigated properties. The overall performance of a composite is thus indirectly affected by the curing protocol adopted, and the desired reduction of C may be in fact a consequence of the decrease in DC. (C) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Dielectric thermal analysis as a tool for quantitative-evaluation of the viscosity and the kinetics of epoxy resin cure

Dielectric thermal analysis has been proved as a valuable tool for monitoring the epoxy curing process and the related rheological properties in the fabrication of polymer-matrix composite materials. This technique also has the potential to be applied in the monitoring of magnet impregnation processes as well as in quality control. In this work we present the quantitative evaluation of the viscosity changing and the curing kinetics for a commercial Stycast epoxy resin system at different temperatures through the impedance analysis. The results showed correlation between the real component of the complex impedance and the isothermal reaction extent. Comparing the dielectric analysis result with the viscosity measured by rotational rheometer we observed a similar behavior reported for dynamic mechanic analysis. The results comparison have shown that the kinetics parameters obtained from DSC and DETA analysis showed different sensitivities related to the characteristics of curing stages. We concluded that the dielectric thermal analysis should be applied in quantitative evaluation of cure kinetics.

The effect of curing light and chemical catalyst on the degree of conversion of two dual cured resin luting cements

The aim of this study was to evaluate the influence of different curing lights and chemical catalysts on the degree of conversion of resin luting cements. A total of 60 disk-shaped specimens of RelyX ARC or Panavia F of diameter 5 mm and thickness 0.5 mm were prepared and the respective chemical catalyst (Scotchbond Multi-Purpose Plus or ED Primer) was added. The specimens were light-cured using different curing units (an argon ion laser, an LED or a quartz-tungsten-halogen light) through shade A2 composite disks of diameter 10 mm and thickness 2 mm. After 24 h of dry storage at 37A degrees C, the degree of conversion of the resin luting cements was measured by Fourier-transformed infrared spectroscopy. For statistical analysis, ANOVA and the Tukey test were used, with p a parts per thousand currency signaEuro parts per thousand 0.05. Panavia F when used without catalyst and cured using the LED or the argon ion laser showed degree of conversion values significantly lower than RelyX ARC, with and without catalyst, and cured with any of the light sources. Therefore, the degree of conversion of Panavia F with ED Primer cured with the quartz-tungsten-halogen light was significantly different from that of RelyX ARC regardless of the use of the chemical catalyst and light curing source. In conclusion, RelyX ARC can be cured satisfactorily with the argon ion laser, LED or quartz-tungsten-halogen light with or without a chemical catalyst. To obtain a satisfactory degree of conversion, Panavia F luting cement should be used with ED Primer and cured with halogen light.

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 degrees C or preheated to 37 degrees C or 50 degrees 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 degrees C (p=0.01830), while no significant difference was observed among groups at 37 degrees C and 50 degrees C. For Variolink, the 3-mm-thick ceramic group showed lower DC than the 1-mm-thick group only at 25 degrees 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 degrees C near 70% reduction and at 50 degrees 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.

Influence of curing rate on softening in ethanol, degree of conversion, and wear of resin composite

Purpose: To investigate the effect of curing rate on softening in ethanol, degree of conversion, and wear of resin composites. Methods: With a given energy density and for each of two different light-curing units (QTH or LED), the curing rate was reduced by modulating the curing mode. Thus, the irradiation of resin composite specimens (Filtek Z250, Tetric Ceram, Esthet-X) was performed in a continuous curing mode and in a pulse-delay curing mode. Wallace hardness was used to determine the softening of resin composite after storage in ethanol. Degree of conversion was determined by infrared spectroscopy (FTIR). Wear was assessed by a three-body test. Data were submitted to Levene`s test, one and three-way ANOVA, and Tukey HSD test (alpha= 0.05). Results: Immersion in ethanol, curing mode, and material all had significant effects on Wallace hardness. After ethanol storage, resin composites exposed to the pulse-delay curing mode were softer than resin composites exposed to continuous cure (P< 0.0001). Tetric Ceram was the softest material followed by Esthet-X and Filtek Z250 (P< 0.001). Only the restorative material had a significant effect on degree of conversion (P< 0.001): Esthet-X had the lowest degree of conversion followed by Filtek Z250 and Tetric Ceram. Curing mode (P= 0.007) and material (P< 0.001) had significant effect on wear. Higher wear resulted from the pulse-delay curing mode when compared to continuous curing, and Filtek Z250 showed the lowest wear followed by Esthet-X and Tetric Ceram. (Am J Dent 2011;24:115-118).

Effect of Different Light-Curing Modes on Degree of Conversion, Staining Susceptibility and Stain's Retention Using Different Beverages in a Nanofilled Composite Resin

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of ceramic shade on the degree of conversion of a dual-cure resin cement analyzed by FTIR

Objectives: The aim of this research was to evaluate the degree of monomer conversion of different resin cement shades when photocured under different feldspathic ceramic shades. The photocuring time was also evaluated as well as the translucency of each ceramic shade. Methods: Three VITA VM7 ceramic shades (Base Dentin 0M1, Base Dentin 2M2 and Base Dentin 5M3) were used to determine the translucency percentage. A spectrophotometer MiniScan was used to measure the opacity percentage of each specimen (2-mm-thick) and then the translucency was calculated. To measure the degree of conversion (DC), the resin cement (Variolink II; A3 Yellow and transparent) specimens (thickness: 100 μm) were photocured under a ceramic block (2-mm-thick) for 20 or 40 s. Specimens photocured without the ceramic block were used as control. Sixteen groups (n = 3) were evaluated. Micro-ATR/FTIR spectrometry was used to evaluate the extent of polymerization of all specimens after 24 h. The %DC was calculated of experimentally polymerized versus maximally polymerized composite. Results: The translucency percentages of 0M1, 2M2 and 5M3 ceramics were 12.41 (1.02)%, 5.75 (1.91)% and 1.07 (0.03)%, respectively. The %DC of both resin cement shades cured under ceramic 5M3 was significantly lower than the other groups (p < 0.05). The %DC of 0M1 groups exhibited no significant difference from 2M2 groups (p > 0.05), with the exception of the transparent cement photocured for 40 s. Conclusion: Photocuring under 2 mm ceramic showed that the increase in chroma saturation significantly decreased Variolink II resin cement %DC (100-μm-thick). © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Time reduction of light curing: Influence on conversion degree and microhardness of orthodontic composites

Introduction: The aim of this study was to assess the influence of curing time and power on the degree of conversion and surface microhardness of 3 orthodontic composites. Methods: One hundred eighty discs, 6 mm in diameter, were divided into 3 groups of 60 samples according to the composite used-Transbond XT (3M Unitek, Monrovia, Calif), Opal Bond MV (Ultradent, South Jordan, Utah), and Transbond Plus Color Change (3M Unitek)-and each group was further divided into 3 subgroups (n = 20). Five samples were used to measure conversion, and 15 were used to measure microhardness. A light-emitting diode curing unit with multiwavelength emission of broad light was used for curing at 3 power levels (530, 760, and 1520 mW) and 3 times (8.5, 6, and 3 seconds), always totaling 4.56 joules. Five specimens from each subgroup were ground and mixed with potassium bromide to produce 8-mm tablets to be compared with 5 others made similarly with the respective noncured composite. These were placed into a spectrometer, and software was used for analysis. A microhardness tester was used to take Knoop hardness (KHN) measurements in 15 discs of each subgroup. The data were analyzed with 2 analysis of variance tests at 2 levels. Results: Differences were found in the conversion degree of the composites cured at different times and powers (P < 0.01). The composites showed similar degrees of conversion when light cured at 8.5 seconds (80.7%) and 6 seconds (79.0%), but not at 3 seconds (75.0%). The conversion degrees of the composites were different, with group 3 (87.2%) higher than group 2 (83.5%), which was higher than group 1 (64.0%). Differences in microhardness were also found (P < 0.01), with lower microhardness at 8.5 seconds (35.2 KHN), but no difference was observed between 6 seconds (41.6 KHN) and 3 seconds (42.8 KHN). Group 3 had the highest surface microhardness (35.9 KHN) compared with group 2 (33.7 KHN) and group 1 (30.0 KHN). Conclusions: Curing time can be reduced up to 6 seconds by increasing the power, with a slight decrease in the degree of conversion at 3 seconds; the decrease has a positive effect on the surface microhardness.

Influence of curing rate on softening in ethanol, degree of conversion, and wear of resin composite

PURPOSE: To investigate the effect of curing rate on softening in ethanol, degree of conversion, and wear of resin composites. METHOD: With a given energy density and for each of two different light-curing units (QTH or LED), the curing rate was reduced by modulating the curing mode. Thus, the irradiation of resin composite specimens (Filtek Z250, Tetric Ceram, Esthet-X) was performed in a continuous curing mode and in a pulse-delay curing mode. Wallace hardness was used to determine the softening of resin composite after storage in ethanol. Degree of conversion was determined by infrared spectroscopy (FTIR). Wear was assessed by a three-body test. Data were submitted to Levene's test, one and three-way ANOVA, and Tukey HSD test (alpha = 0.05). Results: Immersion in ethanol, curing mode, and material all had significant effects on Wallace hardness. After ethanol storage, resin composites exposed to the pulse-delay curing mode were softer than resin composites exposed to continuous cure (P< 0.0001). Tetric Ceram was the softest material followed by Esthet-X and Filtek Z250 (P< 0.001). Only the restorative material had a significant effect on degree of conversion (P< 0.001): Esthet-X had the lowest degree of conversion followed by Filtek Z250 and Tetric Ceram. Curing mode (P= 0.007) and material (P< 0.001) had significant effect on wear. Higher wear resulted from the pulse-delay curing mode when compared to continuous curing, and Filtek Z250 showed the lowest wear followed by Esthet-X and Tetric Ceram.

Light curing through glass ceramics with a second- and a third-generation LED curing unit: effect of curing mode on the degree of conversion of dual-curing resin cements

Objectives The aim of this study was to measure the degree of conversion (DC) of five dual-curing resin cements after different curing modes with a second- and a third-generation light-emitting diode (LED) curing unit. Additionally, irradiance of both light curing units was measured at increasing distances and through discs of two glass ceramics for computer-aided design/manufacturing (CAD/CAM). Materials and methods Irradiance and spectra of the Elipar FreeLight 2 (Standard Mode (SM)) and of the VALO light curing unit (High Power Mode (HPM) and Xtra Power Mode (XPM)) were measured with a MARC radiometer. Irradiance was measured at increasing distances (control) and through discs (1.5 to 6 mm thickness) of IPS Empress CAD and IPS e.max CAD. DC of Panavia F2.0, RelyX Unicem 2 Automix, SpeedCEM, BisCem, and BeautiCem SA was measured with an attenuated total reflectance–Fourier transform infrared spectrometer when self-cured (negative control) or light cured in SM for 40 s, HPM for 32 s, or XPM for 18 s. Light curing was performed directly (positive control) or through discs of either 1.5- or 3-mm thickness of IPS Empress CAD or IPS e.max CAD. DC was analysed with Kruskal–Wallis tests followed by pairwise Wilcoxon rank sum tests (α = 0.05). Results Maximum irradiances were 1,545 mW/cm2 (SM), 2,179 mW/cm2 (HPM), and 4,156 mW/cm2 (XPM), and all irradiances decreased by >80 % through discs of 1.5 mm, ≥95 % through 3 mm, and up to >99 % through 6 mm. Generally, self-curing resulted in the lowest DC. For some cements, direct light curing did not result in higher DC compared to when light cured through ceramic discs. For other cements, light curing through ceramic discs of 3 mm generally reduced DC. Conclusions Light curing was favourable for dual-curing cements. Some cements were more susceptible to variations in curing mode than others. Clinical relevance When light curing a given cement, the higher irradiances of the third-generation LED curing unit resulted in similar DC compared to the second-generation one, though at shorter light curing times.

On the extent of genetic variation for transpiration efficiency in sorghum

A glasshouse study examined 49 diverse sorghum lines for variation in transpiration efficiency. Three of the 49 lines grown were Sorghum spp, native to Australia; one was the major weed Johnson grass (Sorghum halepense), and the remaining 45 lines were cultivars of Sorghum bicolor. All plants were grown under non-limiting water and nutrient conditions using a semi-automatic pot watering system designed to facilitate accurate measurement of water use. Plants were harvested 56-58 days after sowing and dry weights of plant parts were determined. Transpiration efficiency differed significantly among cultivars. The 3 Australian native sorghums had much lower transpiration efficiency than the other 46 cultivars, which ranged from 7.7 to 6.0 g/kg. For the 46 diverse cultivars, the ratio of range in transpiration efficiency to its l.s.d. was 2.0, which was similar to that found among more adapted cultivars in a previous study. This is a significant finding as it suggests that there is likely to be little pay-off from pursuing screening of unadapted material for increased variation in transpiration efficiency. It is necessary, however, also to examine absolute levels of transpiration efficiency to determine whether increased levels have been found. The cultivar with greatest transpiration efficiency in this study (IS9710) had a value 9% greater (P < 0.05) than the accepted standard for adapted sorghum cultivars. The potential impact of such an increase in transpiration efficiency warrants continued effort to capture it. Transpiration efficiency has been related theoretically and experimentally to the degree of carbon isotope discrimination in leaf tissue in sorghum, which thus offers a relatively simple selection index. In this study, the variation in transpiration efficiency was not related simply to carbon isotope discrimination. Significant associations of transpiration efficiency with ash content and indices of photosynthetic capacity were found. However, the associations were not strong. These results suggest that a simple screening technique could not be based on any of the measures or indices analysed in this study. A better understanding of the physiological basis of the observed genetic differences in transpiration efficiency may assist in developing reliable selection indices. It was concluded that the potential value of the improvement in transpiration efficiency over the accepted standard and the degree of genetic variation found warrant further study on this subject. It was suggested that screening for genetic variation under water-limiting conditions may provide useful insights and should be pursued.

Study of the Extent of the Information of Cardiologists from Sao Paulo City, Brazil, Regarding a Low-Prevalence Entity: Brugada Syndrome

Objective: To determine the degree of knowledge that cardiologists from Sao Paulo, Brazil, have regarding a low-prevalent entity associated with a high rate of sudden death-Brugada syndrome. Methods: Two hundred forty-four cardiologists were interviewed by an instrument divided in two parts: in the first, we recorded gender, age, and data related to academic profile. The second-answered only by the professionals that manifested having some degree of knowledge on the syndrome-had 28 questions that evaluated their knowledge. The answers were spontaneous and they did not have a chance to consult. We used uni- and multivariate analysis on the average percentage of right and wrong answers, and the influence of the academic profile. Results: The predominant gender was the male gender (61.1%), the average age was 44.32 +/- 10.83 years, 40% with more than 20 years after obtaining their degree, 44% were educated in public institutions, 69% had a residency in cardiology, 20% had overseas practice, 12% had postdegree, 41% were linked to an educational institution, 24% with publication(s) in an indexed journal, 17.2% were authors of chapters in books, 2.5% had edited books, and 10% were linked to the Brazilian Society of Cardiac Arrhythmias. The average percentage of right answers was 45.7%. Conclusion: The sample studied revealed a little knowledge on the entity. A residency in cardiology was the factor of greater significance in the percentage of right answers. Other significant factors were the link of the interviewed person to an educational institution, or the Brazilian Society of Cardiac Arrhythmias, and having a specialist degree.

Degree of conversion and mechanical properties of a BisGMA : TEGDMA composite as a function of the applied radiant exposure

Objective: Verify the influence of radiant exposure (H) on composite degree of conversion (DC) and mechanical properties. Methods: Composite was photoactivated with 3, 6, 12, 24, or 48 J/cm(2). Properties were measured after 48-h dry storage at room temperature. DC was determined on the flat surfaces of 6 mm x 2 mm disk-shaped specimens using FTIR. Flexural strength (FS) and modulus (FM) were accessed by three-point bending. Knoop microhardness number (KHN) was measured on fragments of FS specimens. Data were analyzed by one-way ANOVA/Tukey test, Student`s t-test, and regression analysis. Results: DC/top between 6 and 12 J/cm(2) and between 24 and 48 J/cm(2) were not statistically different. No differences between DC/top and bottom were detected. DC/bottom, FM, and KHN/top showed significant differences among all H levels. FS did not vary between 12 and 24 J/cm(2) and between 24 and 48 J/cm(2). KHN/bottom at 3 and 6 J/cm(2) was similar. KHN between top and bottom was different up to 12 J/cm(2). Regression analyses having H as independent variable showed a plateau region above 24 J/cm(2). KHN increased exponentially (top) or linearly (bottom) with DC. FS and FM increased almost linearly with DC/bottom up to 55% conversion. Conclusions: DC and mechanical properties increased with radiant exposure. Variables leveled off at high H levels. (C) 2007 Wiley Periodicals, Inc.

Early and 24-hour bond strength and degree of conversion of etch-and-rinse and self-etch adhesives

Purpose: To evaluate early and 24-hour microtensile bond strength (mu TBS) and the degree of conversion (DC) of one representative adhesive system from each of the four current bonding approaches. Methods: 40 human molars were sectioned occluso-gingivally into two halves. Resin composite was bonded incrementally to flat, mid-coronal dentin, using the adhesives Adper Scotchbond MP (MP); Adper Scotchbond 2 (SB); Clearfil SE Bond (SE); and Adper Prompt L-Pop (LP) according to the respective manufacturer`s instructions (n= 10). One half was immediately sectioned into sticks and subjected to mu TBS test. As the sectioning process took approximately 1 hour, the results were designated as 1-hour bond strengths. The other half was stored in distilled water at 37 degrees C for 24 hours before being sectioned and tested. The DC of these systems was measured using Fourier Transform-Raman spectroscopy in three periods: immediately, 1 and 24 hours after polymerization. Data were analyzed with ANOVA and Tukey`s tests. Results: There were no significant differences between the 1-hour and 24-hour bond strengths (P> 0.05), or among the DC measured immediately, 1 hour and 24 hours after polymerization (P> 0.05). However, significant differences were observed among adhesives (P< 0.05). mu TBS values obtained, in MPa (1 hour/24 hour), were: SB (48.6 + 1.3/48.4 + 3.5) = SE (51.9 + 4.7/53.3 +/- 2.9) > MP (35.3 +/- 10.9/38.6 + 6.7) > LP (25.5 + 1.1/26.0 + 1.5). The DC, in percentage (immediately/1 hour/24 hour), were: SE (81/82/87) > MP (79/77/81) > SB (60/63/65) > LP (39/37/42).

Effect of curing protocol on the polymerization of dual-cured resin cements

Objectives. The purpose of this study was to evaluate how curing protocol affects the extent of polymerization of dual-cured resin cements. Methods. Four commercial resin cements were used (DuoLink, Panavia F 2.0, Variolink II and Enforce). The extent of polymerization of the resin cements cured under different conditions was measured using a (1)H Stray-Field MRI method, which also enabled to probe molecular mobility in the kHz frequency range. Results. Resin cements show well distinct behaviours concerning chemical cure. Immediate photo-activation appears to be the best choice for higher filler loaded resin cements (Panavia F 2.0 and Variolink). A photo-activation delay (5 min) did not induce any significant difference in the extent of polymerization of all cements. Significance. The extent of polymerization of dual-cured resin cements considerably changed among products under various curing protocols. Clinicians should optimize the materials choice taking into account the curing characteristics of the cements. (C) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.