Relevance of In-vitro Tests of Adhesive and Composite Dental Materials. A Review in 3 Parts. Part 2: Non-standardized tests of composite materials

Summary The first part of this review examined ISO approval requirements and in vitro testing. In the second part, non-standardized test methods for composite materials are presented and discussed. Physical tests are primarily described. Analyses of surface gloss and alterations, as well as aging simulations of dental materials are presented. Again, the importance of laboratory tests in determining clinical outcomes is evaluated. Differences in the measurement protocols of the various testing institutes and how these differences can in?uence the results are also discussed. Because there is no standardization of test protocols, the values determined by different institutes cannot be directly compared. However, the ranking of the tested materials should be the same if a valid protocol is applied by different institutes. The modulus of elasticity, the expansion after water sorption, and the polishability of the material are all clinically relevant, whereas factors measured by other test protocols may have no clinical correlation. The handling properties of the materials are highly dependent on operators' preferences. Therefore, no standard values can be given.

Relevance of in vitro tests of adhesive and composite dental materials, a review in 3 parts. Part 1: Approval requirements and standardized testing of composite materials according to ISO specifications

The first part of this three-part review on the relevance of laboratory testing of composites and adhesives deals with approval requirements for composite materials. We compare the in vivo and in vitro literature data and discuss the relevance of in vitro analyses. The standardized ISO protocols are presented, with a focus on the evaluation of physical parameters. These tests all have a standardized protocol that describes the entire test set-up. The tests analyse flexural strength, depth of cure, susceptibility to ambient light, color stability, water sorption and solubility, and radiopacity. Some tests have a clinical correlation. A high flexural strength, for instance, decreases the risk of fractures of the marginal ridge in posterior restorations and incisal edge build-ups of restored anterior teeth. Other tests do not have a clinical correlation or the threshold values are too low, which results in an approval of materials that show inferior clinical properties (e.g., radiopacity). It is advantageous to know the test set-ups and the ideal threshold values to correctly interpret the material data. Overall, however, laboratory assessment alone cannot ensure the clinical success of a product.

Direct Adhesive Pin-retained Restorations For Severely Worn Dentition Treatment: A 1.5-year Follow-up Report.

Excessive occlusal surface wear can result in occlusal disharmony, functional and esthetic impairment. As a therapeutic approach, conventional single crowns have been proposed, but this kind of treatment is complex, highly invasive and expensive. This case report describes the clinical outcomes of an alternative minimally invasive treatment based on direct adhesive-pin retained restorations. A 64-year-old woman with severely worn dentition, eating problems related to missing teeth and generalized tooth hypersensitivity was referred for treatment. Proper treatment planning based on the diagnostic wax-up simulation was used to guide the reconstruction of maxillary anterior teeth with direct composite resin over self-threading dentin pins. As the mandibular remaining teeth were extremely worn, a tooth-supported overdenture was installed. A stabilization splint was also used to protect the restorations. This treatment was a less expensive alternative to full-mouth rehabilitation with positive esthetic and functional outcomes after 1.5 years of follow-up.

Dentin Bond Strength Of A Fluoride-releasing Adhesive System Submitted To Ph-cycling.

To evaluate the microtensile bond strength (µTBS) of a fluoride-containing adhesive system submitted to a pH-cycling and storage time regimen for primary outcomes. As secondary outcomes the fluoride released amount was evaluated. Twelve dentin surfaces from sound third molar were divided into 2 groups according to adhesive systems: Clearfil SE Protect (PB) and Clearfil SE Bond (SE). Sticks obtained (1.0 mm2) from teeth were randomly divided into 3 subgroups according to storage regimen model: immediate (24h); 5-month deionized water (W); and pH-cycling model (C). All sticks were tested for µTBS in a universal testing machine. Fluoride concentration was obtained from 1-4 days and 30-day in W and 1-4 days in demineralization (DE)/remineralization (RE) solutions from C, using a fluoride-specific electrode. µTBS and fluoride released data were, respectively, submitted to ANOVA in a split plot design and Tukey, and Friedman' tests (a=0.05). There was no significant interaction between adhesive system and storage regimen for µTBS. W showed the lowest µTBS values. There was no significant difference between 24 h and C models for µTBS. There was no significant difference between adhesive systems. Failure mode was predominantly cohesive within composite for the 24 h and W, for the C group it was mixed for SE and cohesive within composite for PB adhesive system. Fluoride concentrations in the DE/RE solutions were less than 0.03125 ppm and not detected in W. In conclusion, the fluoride-containing adhesive system performed similarly to the regular one. Hydrolytic degradation is the main problem with both adhesive systems, regardless of fluoride contents.

Self-etch Adhesive Systems: A Literature Review.

This paper presents the state of the art of self-etch adhesive systems. Four topics are shown in this review and included: the historic of this category of bonding agents, bonding mechanism, characteristics/properties and the formation of acid-base resistant zone at enamel/dentin-adhesive interfaces. Also, advantages regarding etch-and-rinse systems and classifications of self-etch adhesive systems according to the number of steps and acidity are addressed. Finally, issues like the potential durability and clinical importance are discussed. Self-etch adhesive systems are promising materials because they are easy to use, bond chemically to tooth structure and maintain the dentin hydroxyapatite, which is important for the durability of the bonding.

Influence of different adhesive systems on the pull-out bond strength of glass fiber posts

This in vitro study evaluated the tensile bond strength of glass fiber posts (Reforpost - Angelus-Brazil) cemented to root dentin with a resin cement (RelyX ARC - 3M/ESPE) associated with two different adhesive systems (Adper Single Bond - 3M/ESPE and Adper Scotchbond Multi Purpose (MP) Plus - 3M/ESPE), using the pull-out test. Twenty single-rooted human teeth with standardized root canals were randomly assigned to 2 groups (n=10): G1- etching with 37% phosphoric acid gel (3M/ESPE) + Adper Single Bond + #1 post (Reforpost - Angelus) + four #1 accessory posts (Reforpin - Angelus) + resin cement; G2- etching with 37% phosphoric acid gel + Adper Scotchbond MP Plus + #1 post + four #1 accessory posts + resin cement. The specimens were stored in distilled water at 37°C for 7 days and submitted to the pull-out test in a universal testing machine (EMIC) at a crosshead speed of 0.5 mm/min. The mean values of bond strength (kgf) and standard deviation were: G1- 29.163 ± 7.123; G2- 37.752 ±13.054. Statistical analysis (Student's t-test; a=0.05 showed no statistically significant difference (p<0.05) between the groups. Adhesive bonding failures between resin cement and root canal dentin surface were observed in both groups, with non-polymerized resin cement in the apical portion of the post space when Single Bond was used (G1). The type of adhesive system employed on the fiber post cementation did not influence the pull-out bond strength.

Bond strength of a pit-and-fissure sealant associated to etch-and-rinse and self-etching adhesive systems to saliva-contaminated enamel: individual vs. simultaneous light curing

This study evaluated in vitro the shear bond strength (SBS) of a resin-based pit-and-fissure sealant [Fluroshield (F), Dentsply/Caulk] associated with either an etch-and-rinse [Adper Single Bond 2 (SB), 3M/ESPE] or a self-etching adhesive system [Clearfil S3 Bond (S3), Kuraray Co., Ltd.] to saliva-contaminated enamel, comparing two curing protocols: individual light curing of the adhesive system and the sealant or simultaneous curing of both materials. Mesial and distal enamel surfaces from 45 sound third molars were randomly assigned to 6 groups (n=15), according to the bonding technique: I - F was applied to 37% phosphoric acid etched enamel. The other groups were contaminated with fresh human saliva (0.01 mL; 10 s) after acid etching: II - SB and F were light cured separately; III - SB and F were light cured together; IV - S3 and F were light cured separately; V - S3 and F were light cured simultaneously; VI - F was applied to saliva-contaminated, acid-etched enamel without an intermediate bonding agent layer. SBS was tested to failure in a universal testing machine at 0.5 mm/min. Data were analyzed by one-way ANOVA and Fisher's test (α=0.05).The debonded specimens were examined with a stereomicroscope to assess the failure modes. Three representative specimens from each group were observed under scanning electron microscopy for a qualitative analysis. Mean SBS in MPa were: I-12.28 (±4.29); II-8.57 (±3.19); III-7.97 (±2.16); IV-12.56 (±3.11); V-11.45 (±3.77); and VI-7.47 (±1.99). In conclusion, individual or simultaneous curing of the intermediate bonding agent layer and the resin sealant did not seem to affect bond strength to saliva-contaminated enamel. S3/F presented significantly higher SBS than the that of the groups treated with SB etch-and-rinse adhesive system and similar SBS to that of the control group, in which the sealant was applied under ideal dry, noncontaminated conditions.

Can previous acid etching increase the bond strength of a self-etching primer adhesive to enamel?

Because a greater research effort has been directed to analyzing the adhesive effectiveness of self etch primers to dentin, the aim of this study was to evaluate, by microtensile testing, the bond strength to enamel of a composite resin combined with a conventional adhesive system or with a self-etching primer adhesive, used according to its original prescription or used with previous acid etching. Thirty bovine teeth were divided into 3 groups with 10 teeth each (n= 10). In one of the groups, a self-etching primer (Clearfil SE Bond - Kuraray) was applied in accordance with the manufacturer's instructions and, in the other, it was applied after previous acid etching. In the third group, a conventional adhesive system (Scotchbond Multipurpose Plus - 3M-ESPE) was applied in accordance with the manufacturer's instructions. The results obtained by analysis of variance revealed significant differences between the adhesive systems (F = 22.31). The self-etching primer (Clearfil SE Bond) presented lower enamel bond strength values than the conventional adhesive system (Scotchbond Multipurpose Plus) (m = 39.70 ± 7.07 MPa) both when used according to the original prescription (m = 27.81 ± 2.64 MPa) and with previous acid etching (m = 25.08 ± 4.92 MPa).

Influence of intrapulpal pressure simulation on the bond strength of adhesive systems to dentin

The purpose of this study was to evaluate the influence of intrapulpal pressure simulation on the bonding effectiveness of etch & rinse and self-etch adhesives to dentin. Eighty sound human molars were distributed into eight groups, according to the permeability level of each sample, measured by an apparatus to assess hydraulic conductance (Lp). Thus, a similar mean permeability was achieved in each group. Three etch & rinse adhesives (Prime & Bond NT - PB, Single Bond -SB, and Excite - EX) and one self-etch system (Clearfil SE Bond - SE) were employed, varying the presence or absence of an intrapulpal pressure (IPP) simulation of 15 cmH2O. After adhesive and restorative procedures were carried out, the samples were stored in distilled water for 24 hours at 37°C, and taken for tensile bond strength (TBS) testing. Fracture analysis was performed using a light microscope at 40 X magnification. The data, obtained in MPa, were then submitted to the Kruskal-Wallis test ( a = 0.05). The results revealed that the TBS of SB and EX was significantly reduced under IPP simulation, differing from the TBS of PB and SE. Moreover, SE obtained the highest bond strength values in the presence of IPP. It could be concluded that IPP simulation can influence the bond strength of certain adhesive systems to dentin and should be considered when in vitro studies are conducted.

Do the origins of primary teeth affect the bond strength of a self-etching adhesive system to dentin?

The aim of this in vitro study was to evaluate the tensile bond strength of a self-etching adhesive system to three different dentinal substrates. Primary molar teeth that had been recently exfoliated (RE), with unknown time of exfoliation (UT), and extracted due to prolonged retention (PR) were used for this investigation. Ten primary molar teeth of each group were cut in the middle following the mesio-distal direction, creating a total of twenty specimens per group. The specimens were included in acrylic resin and had a flat dentin surface exposed. The self-etching adhesive system was applied to this surface and a 3-millimeter high cone with diameter of 2 mm in the adhesion area was constructed using composite resin. The specimens were stored in distilled water at 37ºC for 24 hours. Fifteen specimens of each substrate were used for the tensile bond test (n = 15) and 5 had the interface analyzed by scanning electron microscopy (SEM). The data was examined by one-way ANOVA and presented no significant differences between groups (p = 0.5787). The mean values obtained for RE, UT and PR were 18.39 ± 9.70, 19.41 ± 7.80, and 23.30 ± 9.37 MPa, respectively. Any dentinal substrates of primary teeth studied are safe for tensile bond strength tests with adhesive systems.

Effectiveness of sealing active proximal caries lesions with an adhesive system: 1-year clinical evaluation

The objective of this study was to evaluate the effectiveness of a therapeutic sealant to arrest non-cavitated proximal carious lesion progression. The study population comprised 44 adolescents who had bitewing radiographs taken for caries diagnosis. Non-cavitated lesions extending up to half of dentin thickness were included in the sample. In the experimental group (n = 33), the proximal caries-lesion surfaces were sealed with an adhesive (OptiBond Solo, Kerr) after tooth separation. The control group (n = 11) received no treatment, except for oral hygiene instructions including use of dental floss. Follow-up radiographs were taken after one year and were analyzed in comparison with baseline radiographs. In a blind study setting, visual readings were performed by two examiners, blinded to whether the examined radiograph was baseline or follow-up, and whether it concerned a test or control lesion. The efficacy of sealing treatment was evaluated by the McNemar test (0.05). About 22% of the sealed lesions showed reduction, 61% showed no change and 16% showed progression. For the control lesions, the corresponding values were 27%, 36% and 36% respectively. The number of lesions that showed reduction and no changes were merged and therefore 83.3% of the sealed lesions and 63.6% of the control lesions were considered clinically successful. No statistical significance was detected (p > 0.05). In the course of 1 year, sealing proximal caries lesions was not shown to be superior to lesion monitoring.

Long-term quantification of the release of monomers from dental resin composites and a resin-modified glass ionomer cement

This study quantified the release of monomers from polymerized specimens of four commercially available resin composites and one glass ionomer cement immersed in water:ethanol solutions. Individual standard curves were prepared from five monomers: (1) triethylene glycol dimethacrylate (TEGDMA), (2) 2-hydroxy-ethyl methacrylate (HEMA), (3) urethane dimethacrylate (UDMA), (4) bisphenol A glycidyl dimethacrylate (BISGMA), and (5) bisphenol A. The concentration of the monomers was determined at Days 1, 7, 30, and 90 with the use of electrospray ionization/mass spectrometry. Data were expressed in mean mumol per mm(2) surface area of specimen and analyzed with Scheffe's test (P < 0.05). The following monomers were found in water: monomers (1) and (2) from Delton sealant, monomer (5) from ScotchBond Multipurpose Adhesive and Delton sealant, monomer (3) from Definite and monomer (4) from Fuji II LC, ScotchBond Multipurpose Adhesive, Synergy and Definite. All these monomers increased in concentration over time, with the exception of monomer (1) from Delton sealant. Monomers (3) and (5) were found in extracts of materials despite their absence from the manufacturer's published composition. All monomers were released in significantly higher concentrations in water:ethanol solutions than in water. The greatest release of monomers occurred in the first day. The effect of the measured concentrations of monomers (1-5) on human genes, cells, or tissues needs to be considered with the use of a biological model. (C) 2002 Wiley Periodicals, Inc.

Bond strength of an adhesive system irradiated with Nd : YAG laser in dentin treated with Er : YAG laser

The purpose of this in vitro study was to verify through micro tensile bond test the bond strength of an adhesive system irradiated with Nd:YAG laser in dentine previously treated with Er:YAG laser. Twenty caries free extracted human third molars were used. The teeth were divided in four experimental groups (n = 5): (G1) control group; (G2) irradiation of the adhesive system with the Nd:YAG laser; (G3) dentin treatment with Er:YAG laser; (G4) dentin treatment with Er:YAG laser followed by the irradiation of the adhesive system with Nd:YAG laser. The Er:YAG laser fluency parameter for the dentin treatment was of 60 J/cm(2). ne adhesive system was irradiated with the Nd:YAG laser with fluency of 100 J/cm(2). Dental restorations were performed with Adper Single Bond 2/Z250. One tooth from each group was prepared for the evaluation of the adhesive interface under SEM and bond failure tests were also performed and evaluated. The statistical analysis showed statistical significant difference between the groups G1 and G3, G1 and G4, G2 and G3, and G2 and G4; and similarity between the groups G1 and G2, and G3 and G4. The adhesive failures were predominant in all the experimental groups. The SEM analysis showed an adhesive interface with features confirming the results of the mechanical tests. The Nd:YAG laser on the adhesive system did not influence the bond strength in dentin treated or not with the Er:YAG laser.

Erbium, chromium : yttrium scandium gallium garnet laser for caries removal: influence on bonding of a self-etching adhesive system

This study evaluated the influence of the dental substrates obtained after the use of different caries removal techniques on bonding of a self-etching system. Forty, extracted, carious, human molars were ground to expose flat surfaces containing caries-infected dentine surrounded by sound dentine. The caries lesions of the specimens were removed or not (control-G1) either by round steel burs and water-cooled, low speed, handpiece (G2), or by irradiation with an erbium, chromium:yttrium scandium gallium garnet (Er,Cr:YSGG) laser (2W, 20 Hz, 35.38 J/cm(2), fiber G4 handpiece with 0.2826 mm(2), non-contact mode at a 2 mm distance, 70% air/20% water-G3) or using a chemo-mechanical method (Carisolv-G4). Caries-infected, caries-affected and sound dentines were submitted to a bonding system followed by construction of a resin-based composite crown. Hour-glass shaped samples were obtained and submitted to a micro-tensile bond test. The bond strength data were compared by analysis of variance (ANOVA), complemented by Tukey`s test (P <= 0.05). The samples of sound dentine presented higher bond strengths than did samples of caries-affected dentine, except for the groups treated with the Er,Cr:YSGG laser. The highest bond strengths were observed with the sound dentine treated with burs and Carisolv. The bond strengths to caries-affected dentine were similar in all groups. Additionally, bonding to caries-affected dentine of the Er,Cr:YSGG laser and Carisolv groups was similar to bonding to caries-infected dentine. Thus, caries-affected dentine is not an adequate substrate for adhesion. Moreover, amongst the caries removal methods tested, the Er,Cr:YSGG laser irradiation was the poorest in providing a substrate for bonding with the tested self-etching system.

Influence of oil contamination on in vitro bond strength of bonding agents to dental substrates

Purpose: To evaluate the influence of cleaning procedures (pumice, anionic detergent and both procedures together) on the tensile bond strength of etch-and-rinse and self-etch adhesive systems to bovine enamel and dentin in vitro. Methods: Eighty non-carious, bovine incisors were extracted, embedded in acrylic resin to obtain enamel/dentin specimens. Flat bonding surfaces were obtained by grinding. Groups were divided according to substrate (enamel or dentin), adhesive system [etch-and-rinse, Adper Single Bond 2 (SB) or self-etch, Clearfil Protect Bond (PB)]; and cleaning substances (pumice, anionic detergent and their combination). The teeth were randomly divided into 20 groups (n=8): G1 - Enamel (E) + SB; G2 -E + oil (O) + SB; G3 - E + O + Pumice (P) + SB; G4 - E + O + Tergentol (T) + SB; G5 - E + O + P + T + SB; G6 - E + PB; G7 - E + O + PB; G8 - E + O + P + PB; G9 - E + O + T + PB; GIO - E + O + P + T + PB; G11 - Dentin (D) + SB; G12 D + SB + O; G13 - D + SB + O + P; G14 - D + SB + O + T; G15 - D + SB + O + P + T; G16 - D + PB; G17 - D + O + PB +; G18 - D + O + P + PB; G19 - D + O + T + PB; G20 - D + O + P + T + PB. Specimens were contaminated with handpiece oil for 5 seconds before bonding. Adhesive systems and resin composite were applied according to manufacturers` instructions. Specimens were tested in tension after 24 hours of immersion using a universal testing machine at a crosshead speed of 0.5 mm/minute. Bond strengths were analyzed with ANOVA. Failure sites were observed and recorded. Results: Tensile bond strength in MPa were: G1 (23.6 +/- 0.9); G2 (17.3 +/- 2.2); G3 (20.9 +/- 0.9); G4 (20.6 +/- 0.5); G5 (18.7 +/- 2.3); G6 (23.0 +/- 1.0); G7 (21.5 +/- 2.4); G8 (19.9 +/- 1.3); G9 (22.1 +/- 1.2); G10 (19.1 +/- 1.2); G11 (18.8 +/- 1.3); G12 (15.7 +/- 2.1); G13 (17.8 +/- 3.3); G14 (15.3 +/- 2.9); G15 (15.6 +/- 1.9); G16 (14.7 +/- 2.3); G17 (5.5 +/- 0.9); G18 (19.3 +/- 1.8); G19 (15.6 +/- 1.6); G20 (20.3 +/- 3.9). Statistical analysis showed that the main factors substrate and cleaning were statistically significant, as well as the triple interaction between factors of variance. However, the factor adhesive system did not show statistical difference. Oil contamination reduced bond strengths, being less detrimental to enamel than to dentin. Etch-and-rinse (SB) and two-step self-etch (PB) systems had similar bond strengths in the presence of oil contamination. For etch-and-rinse (SB), the cleaning procedures were able to clean enamel, but dentin was better cleaned by pumice. When self-etch (PB) system was used on enamel, anionic detergent was the best cleaning substance, while on dentin the tested procedures were similarly efficient.