Thermal behaviour of intercalated 8-hydroxyquinoline (oxine) in montmorillonite clay

The composite montmorillonite-8-hydroxyquinoline (Swy-1-8-HQ) was prepared by two different processes and studied by using thermogravimetric analysis (TG/DTG and DSC), as well as helpful techniques as fluorescence in the UV-visible region and X-ray diffraction. The composites developed fluorescent appearance, however with quantum poor efficiency and they exhibited distinct TG and DSC thermal behavior. The fluorescence data of spectra associated to the TG/DT curves allowed to suggest that the 8-HQ was present in the composites in two different circumstances: 1 - intercalated in the interlayer spaces (Swy-1-8-HQ2), rigidly associated to the Substrate feasible as a monolayer with the aromatic rings parallel to the silica layer; and/or, 2 - adsorbed on the Surface (Swy-1-8-HQ1), either as a bilayer formation or tilting of the molecules to the silicate layer sheet. All results confirmed above are in agreement with X-ray diffraction patterns, once the interlayer space increases when 8-HQ is incorporated. The experimental results confirm the formation of the composites in agreement with the method used in the preparation.

Repair bond strength of a resin composite to alumina-reinforced feldspathic ceramic

This study compared the microtensile bond strength of a repair resin to an alumina-reinforced feldspathic ceramic (Vitadur-alpha, Vita) after 3 surface conditioning methods: Group 1, etching with 9.6% hydrofluoric acid for 1 minute plus rinsing and drying, followed by application of silane for 5 minutes; group 2, airborne particle abrasion with 110-mm aluminum oxide using a chairside air-abrasion device followed by silane application for 5 minutes; group 3, chairside tribochemical silica coating with 30-mu m SiOx followed by silane application for 5 minutes (N = 30). Group 1 presented the highest mean bond strength (19.7 +/- 3.8 MPa), which was significantly higher than those of groups 2 (10 +/- 2.6 MPa) and 3 (10.4 +/- 4 MPa) (P <.01). Scanning electron microscope analysis of the failure modes demonstrated predominantly mixed types of failures, with adhesive and/or cohesive failures in all experimental groups.

Influence of ceramic surface conditioning and resin cements on microtensile bond strength to a glass ceramic

Statement of problem. It is not clear how different glass ceramic surface pretreatments influence the bonding capacity of various luting agents to these surfaces.Purpose. The purpose of this study was to evaluate the microtensile bond strength (mu TBS) of 3 resin cements to a lithia disilicate-based ceramic submitted to 2 surface conditioning treatments.Material and methods. Eighteen 5 X 6 X 8-mm ceramic (IPS Empress 2) blocks were fabricated according to manufacturer's instructions and duplicated in composite resin (Tetric Ceram). Ceramic blocks were polished and divided into 2 groups (n=9/treatment): no conditioning (no-conditioning/control), or 5% hydrofluoric acid etching for 20 seconds and silanization for 1 minute (HF + SIL). Ceramic blocks were cemented to the composite resin blocks with I self-adhesive universal resin cement (RelyX Unicem) or 1 of 2 resin-based luting agents (Multilink or Panavia F), according to the manufacturer's instructions. The composite resin-ceramic blocks were stored in humidity at 37 degrees C for 7 days and serially sectioned to produce 25 beam specimens per group with a 1.0-mm(2) cross-sectional area. Specimens were thermal cycled (5000 cycles, 5 degrees C-55 degrees C) and tested in tension at 1 mm/min. Microtensile bond strength data (MPa) were analyzed by 2-way analysis of variance and Tukey multiple comparisons tests (alpha=.05). Fractured specimens were examined with a stereomicroscope (X40) and classified as adhesive, mixed, or cohesive.Results. The surface conditioning factor was significant (HF+SIL > no-conditioning) (P<.0001). Considering the unconditioned groups, the mu TBS of RelyX Unicem was significantly higher (9.6 +/- 1.9) than that of Multilink (6.2 +/- 1.2) and Panavia F (7.4 +/- 1.9). Previous etching and silanization yielded statistically higher mu TBS values for RelyX Unicem (18.8 +/- 3.5) and Multilink (17.4 +/- 3.0) when compared to Panavia F (15.7 +/- 3.8). Spontaneous debonding after thermal cycling was detected when luting agents were applied to untreated ceramic surfaces.Conclusion. Etching and silanization treatments appear to be crucial for resin bonding to a lithia disilicate-based ceramic, regardless of the resin cement used.

Efeito da lavagem artificial na eficiência de acaricidas-ovicidas no controle de Brevipalpus phoenicis (Geijskes, 1939) (Acari: Tenuipalpidae) em citros

The objective of this research was to test the control of Brevipalpus phoenicis (Geijskes, 1939) by the hexythiazox and quinometionato products in citrus crop with and without adhesive spread and when submitted to artificial rain. The plants were sprayed at 2, 4, 8, 24 and 48 hours. When dried, the fruits were collected (eight/plants) and half of them were washed in laboratory with artificial rainfall on the basis of 30 mm/h during 15 minutes establishing the following treatments: T1 - hexythiazox + washing; T2 - hexythiazox + agral + washing; T3 - quinometionato + washing; T4 - quinometionato + agral + washing; T5 - control + agral + washing; T6 - hexythiazox; T7 - hexythiazox + agral; T8 - quinometionato; T9 - quinometionato + agral; T10 - control + agral. Thus, all the fruits were inoculated with ten females of B. phoenicis and five days later the mites alive were counted and eliminated. Approximately 15 days later the number of larvae alive were also counted. The results obtained allowed the following conclusions: a) the acaricides were efficient to control B. phoenicis; b) the rainfall (washing) did not alter the efficiency; c) the agral did not change the results.

Study of an organically modified clay: Selective adsorption of heavy metal ions and voltammetric determination of mercury(II)

In this work, a hydrophilic clay, Na-montmorillonite from Wyoming, USA, was rendered organophilic by exchanging the inorganic interlayer cations for hexaclecyltrimethylammonium ions (HDTA), with the formulae of [(CH3)(3)N(C16H33)](+) ion. Based on fact that organo-clay has high affinities for non-ionic organic molecules, 1,3,4-thiadiazole-2,5-dithiol was loaded oil the HDTA-montmorillonite surface, resulting in the 1,3,4-thiadiazole-2,5-dithiol-HDTA-montmorillonite complex (TDD-organo-clay).The following properties of TDD-organo-clay are discussed: selective adsorption of heavy metal ions measured by batch and chromatographic column techniques, and utilization as preconcentration agent in a chemically modified carbon paste electrode (CMCPE) for determination of mercury(II).The main point of this paper is the construction of a selective sensor, a carbon paste electrode modified with TDD-organo-clay, its properties and its application to the determination of mercury(II) ions, as this element belongs to the most toxic metals. The chemical selectivity of this functional group and the selectivity of voltammetry were combined for preconcentration and determination. (c) 2005 Elsevier B.V. All rights reserved.

Effect of surface conditioning methods on the microtensile bond strength of resin composite to composite after aging conditions

Objectives. This study evaluated the effect of two different surface conditioning methods on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite after three aging conditions.Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared (5 mm x 6 mm x 6 mm) and randomly assigned into three groups for aging process: (a) immersion in citric acid (pH 3.0 at 37 degrees C, 1 week) (CA); (b) boiling in water for 8h (BW) and (c) thermocycling (x5000, 5-55 degrees C, dwell time: 30s) (TC). After aging, the blocks were assigned to one of the following surface conditioning methods: (1) silica coating (30 mu m SiOx) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single Bond, 3M ESPE) (PA). Resin composite (Esthet.X (R)) was bonded to the conditioned substrates incrementally and light polymerized. The experimental groups formed were as follows: Gr1:CA + PA; Gr2:CA + CJ Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to obtain non-trimmed bar specimens (sticks, 10 mm x 1 mm x 1 mm) with 1 mm(2) of bonding area. The microtensile test was accomplished in a universal testing machine (crosshead speed: 0.5 mm min(-1)).Results. The means and standard deviations of bond strength (MPa +/- S.D.) per group were as follows: Gr1: 25.5 +/- 10.3; Gr2: 46.3 +/- 10.1; Gr3: 21.7 +/- 7.1; Gr4: 52.3 +/- 15.1; GrS: 16.1 +/- 5.1; Gr6, 49.6 +/- 13.5. The silica coated groups showed significantly higher mean bond values after all three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, alpha = 0.05). The interaction effect revealed significant influence of TC aging on both silica coated and acid etched groups compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging medium.Significance. Chairside silica coating and silanization provided higher resin-resin bond strength values compared to acid etching with phosphoric acid followed by adhesive resin applications. Thermocycling the composite substrates resulted in the lowest repair bond strength compared to citric acid challenge or boiling in water. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The effect of ceramic surface treatment on bonding to densely sintered alumina ceramic

Statement of problem. Ceramic surface treatment is crucial for bonding to resin. High crystalline ceramics are poorly conditioned using traditional procedures.Purpose. The purpose of this study was to evaluate the effect of silica coating on a densely sintered alumina ceramic relative to its bond strength to composite, using a resin luting agent.Material and methods. Blocks (6 X 6 X 5 mm) of ceramic and composite were made. The ceramic (Procera AllCeram) surfaces were polished, and the blocks were divided into 3 groups (n = 5): SB, airborne-particle abrasion with 110-mu m Al(2)O(3); RS, silica coating using Rocatec System; and CS, silica coating using CoJet System. The treated ceramic blocks were luted to the composite (W3D Master) blocks using a resin luting agent (Panavia F). Specimens were stored in distilled water at 37 degrees C for 7 days and then Cut in 2 axes, x and y, to obtain specimens with a bonding area of approximately 0.6 mm(2) (n = 30). The specimens were loaded to failure in tension in a universal testing machine, and data were statistically analyzed using a randomized complete block design analysis of variance and Tukey's test (alpha=.05). Fractured surfaces were examined using light microscopy and scanning electron microscopy to determine the type of failure. Energy-dispersive spectroscopy was used for surface compositional analysis.Results. Mean bond strength values (MPa) of Groups RS (17.1 +/- 3.9) (P = .00015) and CS (18.5 +/- 4.7) (P=.00012) were significantly higher than the values of Group SB (12.7 +/- 2.6). There was no statistical difference between Groups RS and CS. All failures occurred at the adhesive zone.Conclusion. Tribochemical silica coating systems increased the tensile bond strength values between Panavia F and Procera AllCeram ceramic.

Surface conditioning of a composite used for inlay/onlay restorations: Effect on mu TBS to resin cement

Purpose: To assess the effect of the composite surface conditioning on the microtensile bond strength of a resin cement to a composite used for inlay/onlay restorations.Materials and Methods: Forty-two blocks (6 x 6 x 4 mm) of a microfilled composite (Vita VMLC) were produced and divided into 3 groups (N = 14) by composite surface conditioning methods: Gr1 - etching with 37% phosphoric acid, washing, drying, silanization; Gr2 - air abrasion with 50-Im Al203 particles, silanization; Gr3 - chairside tribochemiCal silica coating (CoJet System), silanization. Single-Bond (one-step adhesive) was applied on the conditioned surfaces and the two resin blocks treated with the same method were cemented using RelyX ARC (dual-curing resin cement). The specimens were stored for 7 days in water at 37 degrees C and then sectioned to produce nontrimmed beam samples, which were submitted to microtensile bond strength testing (mu TBS). For statistical analysis (one-way ANOVA and Tukey's test, = 0.05), the means of the beam samples from each luted specimen were calculated (n = 7).Results: mu TBS values (MPa) of Gr2 (62.0 +/- 3.9a) and Gr3 (60.5 +/- 7.9a) were statistically similar to each other and higher than Gr1 (38.2 +/- 8.9b). The analysis of the fractured surfaces revealed that all failures occurred at the adhesive zone.Conclusion: Conditioning methods with 50-Im Al203 or tribochemical silica coating allowed bonding between resin and composite that was statistically similar and stronger than conditioning with acid etching.

Microleakage and nanoleakage: Influence of laser in cavity preparation and dentin pretreatment

Objective: the purpose of this study was to verify if the application of the Nd:YAG laser following pretreatment of dentin with adhesive systems that were not light cured in class V cavities and were prepared with Er:YAG laser would promote better sealing of the gingival margins when compared to cavities prepared the conventional way. Background Data: Previous studies had shown that the pretreatment of dentin with laser irradiation after the application of an adhesive system is efficient in achieving higher shear bond and tensile bond strength. Materials and Methods: Er:YAG laser (Kavo-Key, Germany) with 350 mJ, 4 Hz, and 116.7 J/cm(2) was used for cavity preparation. The conventional preparation was made with diamond bur mounted in high-speed turbine. Dentin treatment was accomplished using an Nd:YAG laser (Pulse Master 1000, ADT. USA) at 60 mJ, 10 Hz, and 74.65/cm(2) following application of the adhesive system. The cavities were stored with Single Bond/Z100 and Prime & Bond NT/TPH. Eighty bovine incisors were used, and class V preparations were done at buccal and lingual surfaces divided into eight groups: (1) Er:YAG preparation + Prime & Bond NT + TPH; (2) Er:YAG preparation + Single Bond + Z100; (3) Er:YAG preparation + Single Bond + Nd:YAG + Z100; (4) Er:YAG preparation + Prime & Bond NT + Nd:YAG + TPH; (5) conventional preparation + Prime & Bond NT + TPH; (6) conventional preparation + Single Bond + Z100; (7) conventional preparation + Single Bond + Nd:YAG + Z100; (8) conventional preparation + Prime & Bond NT + Nd:YAG + TPH. All specimens were thermocycled for 300 full cycles between 5 degreesC +/- 2 degreesC and 55 degreesC +/- 2 degreesC (dwell time of 30 sec), and stored in 50% silver nitrate solution for 24 h soaked in photodeveloping solution and exposed to fluorescent light for 6 h. After this procedure, the specimens were sectioned longitudinally in 3 portions and the extension of microleakage at the gingival wall was determined following a criteria ranging from 0 to 4 using scanning electron microscopy (SEM). The medium portion sectioned of each specimen was polished and prepared for nanoleakage avaliation by SEM. Results: Kruskall-Wallis and Miller statistical tests determined that group 3 presented less microleakage and nanoleakage. Conclusion: Application of the Nd:YAG laser following pretreatment of dentin with adhesive Single Bond non-photocured Single Bond adhesive in cavities prepared with Er:YAG promote better sealing of the gingival margins.

Microtensile bond strength of a resin cement to feldpathic ceramic after different etching and silanization regimens in dry and aged conditions

Objectives. This study evaluated the durability of bond strength between resin cement and a feldspathic ceramic submitted to different etching regimens with and without silane coupling agent application.Methods. Thirty-two blocks (6.4 mm x 6.4 mm x 4.8 mm) were fabricated using a microparticulate feldspathic ceramic (Vita VM7), ultrasonically cleaned with water for 5 min and randomly divided into four groups, according to the type of etching agent and silanization method: method 1, etching with 10% hydrofluoric (HF) acid gel for I min + silanization; method 2, HF only; method 3, etching with 1.23% acidulated phosphate fluoride (APF) for 5 min + silanization; method 4, APF only. Conditioned blocks were positioned in their individual silicone molds and resin cement (Panavia F) was applied on the treated surfaces. Specimens were stored in distilled water (37 degrees C) for 24 h prior to sectioning. After sectioning the ceramic-cement blocks in x- and Y-axis with a bonded area of approximately 0.6 mm(2), the microsticks of each block were randomly divided into two storage conditions: Dry, immediate testing; TC, thermal cycling (12,000 times) + water storage for 150 d, yielding to eight experimental groups. Microtensile bond strength tests were performed in universal testing machine (cross-head speed: 1 mm/min) and failure types were noted. Data obtained (MPa) were analyzed with three-way ANOVA and Tukey's test (alpha = 0.05).Results. Significant influence of the use of silane (p < 0.0001), storage conditions (p = 0.0013) and surface treatment were observed (p = 0.0014). The highest bond strengths were achieved in both dry and thermocycled conditions when the ceramics were etched with HF acid gel and silanized (17.4 +/- 5.8 and 17.4 +/- 4.8 MPa, respectively). Silanization after HF acid gel and APT treatment increased the results dramatically (14.5 +/- 4.2-17.4 +/- 4.8 MPa) compared to non-silanized groups (2.6 +/- 0.8-8.9 +/- 3.1 MPa) where the failure type was exclusively (100%) adhesive between the cement and the ceramic.Significance. Silanization of the feldspathic ceramic surface after APF or HF acid etching increased the microtensile bond strength results significantly, with the latter providing higher results. Long-term thermocycling and water storage did not decrease the results in silanized groups. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Synthesis, characterization and electrochemical study of layered double hydroxides intercalated with 2-thiophenecarboxylate anions

The synthesis, characterization, and electrochemical study of the Zn(II)-Al(III) and Zn(II)-Cr(III) Layered Double Hydroxides (LDHs) containing 2-thiopenecarboxylate as the interlayer anions are described. The LDHs were prepared by the constant pH coprecipitation technique followed by hydrothermal treatment for 72 h. The materials were analyzed by PXRD, FT-IR, C-13 CP-MAS, EDX, TEM, and CV. The presence of the organic heterocyclic anions was confirmed by FT-IR and the related solid-state C-13 NMR data strongly suggested that these were dimerised during coprecipitation. Accordingly, the basal spacing found by the X-ray technique was similar to 15.3 Angstrom, a distance coincident with the formation of bilayers of the intercalated anions. The structural organization of all the new materials was greatly enhanced by hydrothermal treatment, as shown by PXRD. The improved organization of the bilayered structures had a strong influence in the electrochemical behaviour of clay-modified electrodes produced with these materials, such as the diminished resistance to the ionic flow through the LDHs films. (C) 2003 Elsevier Ltd. All rights reserved.

Ultrastructure of the ovariole sheath in Diatraea saccharalis (Lepidoptera : Pyralidae)

The ultrastructure of the ovariole sheath along the Diatraea saccharalis ovariole was studied by scanning and transmission electron microscopy. Each ovariole is surrounded by an epithelial sheath, a tunica propria and scattered lumen cells. These three components of the ovariole sheath show different ultrastructural features along the ovariole, in the germarium or in the vitellarium; these differences are more evident in the epithelial sheath cells. The epithelial sheath is composed by two layers of cells, the external one running longitudinally and the internal one running circularly in the ovariole. These cells, in vitellarium, present cytoplasmic bundles of myofilaments that are arranged parallel to the long axis of the cells; these myofilaments are apparently related to the contraction movements of the follicles within the ovariole. The acellular tunica propria, composed of finely filamentous material, is attached to the adjacent follicle cells by adhesive dense plates. Between the epithelial sheath and the tunica propria there is a population of lumen cells, with morphological features of secretory activity.

An In Vitro Comparison of Different Cementation Strategies on the Pull-out Strength of a Glass Fiber Post

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

The slippery slope - Critical perspectives on in vitro research methodologies

Objectives. This paper attempts to provide critical perspectives on common in vitro research methodologies, including shear bond testing, wear testing, and load-to-failure tests. Origins of interest in high-quality laboratory data is reviewed, in vitro data is categorized into property and simulation protocols, and two approaches are suggested for establishing clinical validity. It is hoped that these insights will encourage further progress toward development of in vitro tests that are validated against clinical performance and/or by producing clinically validated failure or damage mechanisms.Materials and methods. Published shear and tensile bond data (macro and micro) is examined in light of published finite element analyses (FEA). This data is subjected to a Weibull scaling analysis to ascertain whether scaling is consistent with failure from the bonded interface or not. Wear tests results are presented in light of the damage mechanism(s) operating. Quantitative wear data is re-examined as being dependent upon contact pressure. Load-to-failure test results are re-analyzed by calculating contact stresses at failure for 119 tests from 54 publications over more than 25 years.Results. FEA analyses and reported failure modes (adhesive, mixed, cohesive) are consistent with failure not involving interfacial "shear stresses" as calculated in published work. Weibull scaling clearly suggests failure involving external surfaces of specimens, not interfacial origins. Contact stresses (pressures) are clearly an important variable in wear testing and are not well-controlled in published work. Load-to-failure tests create damage not seen clinically due to excessively high contact stresses. Most contact stresses in the 119 tests examined were calculated to be between 1000 MPa and 5000 MPa, whereas clinical contact stresses at wear facets have been measured not to exceed 40 MPa.Conclusions. Our community can do a much better job of designing in vitro tests that more closely simulate clinical conditions, especially when contact is involved. Journals are encouraged to thoughtfully consider a ban on publishing papers using bond tests and load-to-failure methods that are seriously flawed and have no clinical relevance. (C) 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Partially exchanged organophilic bentonites

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)