Preparation of a silica gel modified with 2-amino-1,3,4-thiadiazole for adsorption of metal ions and electroanalytical application

Silica gel with a specific area of 382 m2 g-1 and an average pore diameter of 60 Å was chemically modified with 2-amino-1,3,4-thiadiazole, for the purpose of selective adsorption of heavy metals ions and possible use as a chemically modified carbon paste electrode (CMCPE). The following properties of this functionalized silica gel 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 chemical selectivity of this functional group and the selectivity of voltammetry were combined for preconcentration and determination. ©2006 Sociedade Brasileira de Química.

Bond strength of a resin cement to high-alumina and zirconia-reinforced ceramics: The effect of surface conditioning

Purpose: The aim of this study was to evaluate the effect of two surface conditioning methods on the microtensile bond strength of a resin cement to three high-strength core ceramics: high alumina-based (In-Ceram Alumina, Procera AllCeram) and zirconia-reinforced alumina-based (In-Ceram Zirconia) ceramics. Materials and Methods: Ten blocks (5 ×6 × 8 mm) of In-Ceram Alumina (AL), In-Ceram Zirconia (ZR), and Procera (PR) ceramics were fabricated according to each manufacturer's instructions and duplicated in composite. The specimens were assigned to one of the two following treatment conditions: (1) airborne particle abrasion with 110-μm Al2O3 particles + silanization, (2) silica coating with 30 μm SiOx particles (CoJet, 3M ESPE) + silanization. Each ceramic block was duplicated in composite resin (W3D-Master, Wilcos, Petrópolis, RJ, Brazil) using a mold made out of silicon impression material. Composite resin layers were incrementally condensed into the mold to fill up the mold and each layer was light polymerized for 40 s. The composite blocks were bonded to the surface-conditioned ceramic blocks using a resin cement system (Panavia F, Kuraray, Okayama, Japan). One composite resin block was fabricated for each ceramic block. The ceramic-composite was stored at 37°C in distilled water for 7 days prior to bond tests. The blocks were cut under water cooling to produce bar specimens (n = 30) with a bonding area of approximately 0.6 mm2. The bond strength tests were performed in a universal testing machine (crosshead speed: 1 mm/min). Bond strength values were statistically analyzed using two-way ANOVA and Tukey's test (≤ 0.05). Results: Silica coating with silanization increased the bond strength significantly for all three high-strength ceramics (18.5 to 31.2 MPa) compared to that of airborne particle abrasion with 110-μm Al2O3 (12.7-17.3 MPa) (ANOVA, p < 0.05). PR exhibited the lowest bond strengths after both Al2O3 and silica coating (12.7 and 18.5 MPa, respectively). Conclusion: Conditioning the high-strength ceramic surfaces with silica coating and silanization provided higher bond strengths of the resin cement than with airborne particle abrasion with 110-μm Al2O3 and silanization.

Scanning electron microscopic analysis of the effect of Carisolv TM gel on periodontally compromised human root surfaces

The aim of this study was to analyze, under scanning electron microscopy (SEM), the morphologic characteristics of root surfaces after application of CarisolvTM gel in association with scaling and root planing (SRP). Sixty periodontally compromised extracted human teeth were randomly assigned to 6 groups: 1) SRP alone; 2) passive topical application of CarisolvTM + SRP; 3) active topical application of CarisolvTM + SRP; 4) multiple applications of CarisolvTM + SRP; 5) SRP + 24% EDTA; 6) topical application of CarisolvTM + SRP + 24% EDTA. CarisolvTM gel was applied to root surfaces for 30 s, followed by scaling and root planing, consisting of 50 strokes with Gracey curettes in an apical-coronal direction, parallel to the long axis of the tooth. The only exception was group 4, in which the roots were instrumented until a smooth, hard and glass-like surface was achieved. All specimens were further analyzed by SEM. The results showed that the treatment with CarisolvTM caused significant changes in root surface morphology of periodontally compromised teeth only when the chemical agent was actively applied (burnishing technique). CarisolvTM failed to remove the smear layer completely, especially with a single application, independently of the method of application. Multiple applications of CarisolvTM were necessary to achieve a smear layer reduction comparable to that obtained with 24% EDTA conditioning.

Microtensile bond strength of a resin cement to silica-coated and silanized in-ceram zirconia before and after aging

Purpose: This study compared the microtensile bond strength of resin-based cement (Panavia F) to silica-coated, silanized, glass-infiltrated high-alumina zirconia (In-Ceram Zirconia) ceramic in dry conditions and after various aging regimens. Materials and Methods: The specimens were placed in 1 of 4 groups: group 1: dry conditions (immediate testing without aging); group 2: water storage at 37°C for 150 days; group 3: 150 days of water storage followed by thermocycling (× 12,000, 5°C to 55°C); group 4: water storage for 300 days; group 5: water storage for 300 days followed by thermocycling. Results: Group 1 showed a significantly higher microtensile bond strength value (26.2 ± 1 MPa) than the other aging regimens (6.5 ± 1, 6.2 ± 2, 4.5 ± 1, 4.3 ± 1 MPa for groups 2, 3, 4, and 5, respectively) (P < .01). Conclusion: Satisfactory results were seen in dry conditions, but water storage and thermocycling resulted in significantly weaker bonds between the resin cement and the zirconia.

Effects of basic fibroblast growth factor on density and morphology of fibroblasts grown on root surfaces with or without conditioning with tetracycline or EDTA.

A study was conducted to evaluate in vitro the effect of root surface conditioning with basic fibroblast growth factor (b-FGF) on morphology and proliferation of fibroblasts. Three experimental groups were used: non-treated, and treated with 50 microg or 125 microg b-FGF/ml. The dentin samples in each group were divided into subgroups according to the chemical treatment received before application of b-FGF: none, or conditioned with tetracycline-HCl or EDTA. After contact with b-FGF for 5 min, the samples were incubated for 24 h with 1 ml of culture medium containing 1 x 10(5) cells/ml plus 1 ml of culture medium alone. The samples were then subjected to routine preparation for SEM, and random fields were photographed. Three calibrated and blind examiners performed the assessment of morphology and density according to two index systems. Classification and regression trees indicated that the root surfaces treated with 125 microg b-FGF and previously conditioned with tetracycline-HCl or EDTA presented a morphology more suggestive of cellular adhesion and viability (P = 0.004). The density of fibroblasts on samples previously conditioned with EDTA, regardless of treatment with b-FGF, was significantly higher than in the other groups (P < 0.001). The present findings suggest that topical application of b-FGF has a positive influence on both the density and morphology of fibroblasts.

Resin microtensile bond strength to feldspathic ceramic: Hydrofluoric acid etching vs tribochemical silica coating

This study aimed to compare the microtensile bond strength of resin cement to alumina-reinforced feldspathic ceramic submitted to acid etching or chairside tribochemical silica coating. Ten blocks of Vitadur-α were randomly divided into 2 groups according to conditioning method: (1) etching with 9.6% hydrofluoric acid or (2) chairside tribochemical silica coating. Each ceramic block was luted to the corresponding resin composite block with the resin cement (Panavia F). Next, bar specimens were produced for microtensile testing. No significant difference was observed between the 2 experimental groups (Student t test, P> .05). Both surface treatments showed similar microtensile bond strength values.

Microtensile bond strength of a repair composite to leucite-reinforced feldspathic ceramic

The purpose of this study was to evaluate the microtensile bond strength of a repair composite resin to a leucite-reinforced feldspathic ceramic (Omega 900, VITA) submitted to two surface conditionings methods: 1) etching with hydrofluoric acid + silane application or 2) tribochemical silica coating. The null hypothesis is that both surface treatments can generate similar bond strengths. Ten ceramic blocks (6x6x6 mm) were fabricated and randomly assigned to 2 groups (n=5), according to the conditioning method: G1- 10% hydrofluoric acid application for 2 min plus rinsing and drying, followed by silane application for 30 s; G2- airborne particle abrasion with 30 μm silica oxide particles (CoJet-Sand) for 20 s using a chairside air-abrasion device (CoJet System), followed by silane application for 5 min. Single Bond adhesive system was applied to the surfaces and light cured (40 s). Z-250 composite resin was placed incrementally on the treated ceramic surface to build a 6x6x6 mm block. Bar specimens with an adhesive area of approximately 1 ± 0.1 mm2 were obtained from the composite-ceramic blocks (6 per block and 30 per group) for microtensile testing. No statistically significant difference was observed between G1 (10.19 ± 3.1 MPa) and G2 (10.17 ± 3.1 MPa) (p=0.982) (Student's t test; á = 0.05). The null hypothesis was, therefore, accepted. In conclusion, both surface conditioning methods provided similar microtensile bond strengths between the repair composite resin and the ceramic. Further studies using long-term aging procedures should be conducted.

Surface conditioning of a composite used for inlay/onlay restorations: Effect on μTBS 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 × 6 × 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-l̀m Al2O3 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°C and then sectioned to produce nontrimmed beam samples, which were submitted to microtensile bond strength testing (μTBS). 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: μTBS 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-l̀m Al2O3 or tribochemical silica coating allowed bonding between resin and composite that was statistically similar and stronger than conditioning with acid etching.

In vitro evaluation of the abrasiveness of a commercial low-abrasive dentifrice and an experimental dentifrice containing vegetable oil

Toothpastes usually contain detergents, humectants, water colorant, fluoride and thickeners (e.g. silica). Tooth wear has a multi-factorial etilology and the use of abrasive dentifrices is related to abrasion of dental tissues during toothbrushing. This study evaluated in vitro the abrasiveness of a commercial silica gel low-abrasive dentrifice compared to an experimental dentifrice containing vegetable (almond) oil. Distilled water served as a control group. Acrylic specimens (8 per group) were submitted to simulated toothbrushing with slurries of the commercial dentifrice experimental dentifrice, almond oil and water in an automatic brushing machine programmed to 30,000 brush strokes for each specimen which is equivalent to 2 years of manual toothbrushing. Thereafter, surface roughness (Ra) of the specimens was analyzed with a Surfcorder SE 1700 profilometer. Data were analyzed statistically by ANOVA and Tukey's test at 5% significance level. There was no statistically significant differences (p>0.05) in the surface roughness after brushing with water almond oil experimental dentifrice. The commercial dentifrice produced rougher surfaces compared to the control and abrasive free products (p<0.05). Further studies are necessary in confirm the potential benefits of using vegetable oil in toothpaste as an alternative in abrasives in an attempt to minimize the tooth wear caused by toothbrushing.

Defect-induced photoluminescence of powdered silica glass

Visible photoluminescence was generated in standard soda-lime-silica glass powder, mechanically milled in a high-energy attrition mill. The broad emission band maximum shows a linear dependence on the exciting wavelength, suggesting the possibility to tune the PL emission. The photoluminescence was attributed to defect generation related to unsatisfied chemical bonds due to the high surface area. Raman scattering and ultraviolet-visible optical reflectance measurements corroborate this assertion. Transmission electron microscopy measurements indicate that the powder is composed by nanocrystallites with about 10-20 nanometers immersed in an amorphous media.

Evaluation of blood compatibility of plasma deposited heparin-like films and SF6 plasma treated surfaces

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Effect of surface treatments on the bond strength of a resin cement to commercially pure titanium

Investigation of the effectiveness of surface treatments that promote a strong bond strength of resin cements to metals can contribute significantly to the longevity of metal-ceramic restorations. This study evaluated the effect of surface treatments on the shear bond strength (SBS) of a resin cement to commercially pure titanium (CP Ti). Ninety cast CP Ti discs were divided into 3 groups (n=30), which received one of the following airborne-particle abrasion conditions: (1) 50 μm Al2O3 particles; (2) 30 μm silica-modified Al2O3 particles (Cojet Sand); (3) 110 μm silica-modified Al2O3 particles (Rocatec). For each airborne-particle abrasion condition, the following post-airborne-particle abrasion treatments were used (n=10): (1) none; (2) adhesive Adper Single Bond 2; (3) silane RelyX Ceramic Primer. RelyX ARC resin cement was bonded to CP Ti surfaces. All specimens were thermally cycled before being tested in shear mode. Failure mode was determined. The best association was Rocatec plus silane. All groups showed 100% adhesive failure. There were combinations that promote higher SBS than the protocol recommended by the manufacturer of RelyX ARC.

Concentration of Cu(II) and Cd(II) from natural river water by Adsorption on a Modified Silica Surface

A high surface area silica gel (737 ± m2 g-1) was synthesized modified through a two-step reaction with a 4-amino-2-mercaptopyrimidine ligand and applied to Cu(II) and Cd(II) adsorption from an aqueous medium. The modified material was characterized by FTIR, which showed that attachment of the molecule occurred via thiol groups at 2547 and 2600 cm-1, and by elemental analysis that indicated the presence of 0.0102 mmol of ligand. The data from adsorption experiments were adjusted to a modified Langmuir equation and the maximum adsorption capacity was 6.6 and 3.8 μmol g-1 for Cu(II) and Cd(II), respectively. After adjusting several parameters, the material was applied in the preconcentration of natural river water using a continuous flow system before and after sample mineralization, and the results showed a 10-fold enrichment factor. The proposed method was validated through preconcentration and analysis of certified standard reference material (1643e), whose results were in agreement with the values provided by the manufacturer.

Effect of instrumentation using curettes, piezoelectric ultrasonic scaler and er,cr:Ysgg laser on the morphology and adhesion of blood components on root surfaces - A SEM study

This study used scanning electron microscopy (SEM) to evaluate the morphology and adhesion of blood components on root surfaces instrumented by curettes, piezoelectric ultrasonic scaler and Er,Cr:YSGG laser. One hundred samples from 25 teeth were divided into 5 groups: 1) Curettes; 2) Piezoelectric ultrasonic scaler; 3) Curettes plus piezoelectric ultrasonic scaler; 4) Er,Cr:YSGG laser; 5) Curettes plus Er,Cr:YSGG laser. Ten samples from each group were used for analysis of root morphology and the other 10 were used for analysis of adhesion of blood components on root surface. The results were analyzed statistically by the Kruskall-Wallis and Mann-Whitney tests with a significance level of 5%. The group treated with curettes showed smoother surfaces when compared to the groups were instrumented with piezoelectric ultrasonic scaler and the Er,Cr:YSGG laser. The surfaces instrumented with piezoelectric ultrasonic scaler and Er,Cr:YSGG laser, alone or in combination with hand scaling and root planing, did not differ significantly (p>0.05) among themselves. No statistically significant differences (p>0.05) among groups were found as to the adhesion of blood components on root surface. Ultrasonic instrumentation and Er,Cr:YSGG irradiation produced rougher root surfaces than the use of curettes, but there were no differences among treatments with respect to the adhesion of blood components.

Shear bond strength of resin cement bonded to alumina ceramic after treatment by aluminum oxide sandblasting or silica coating

Purpose: To evaluate the shear bond strength and bond durability between a dual-cured resin cement (RC) and a high alumina ceramic (In-Ceram Alumina), subjected to two surface treatments. Materials and Methods: Forty disc-shaped specimens (sp) (4-mm diameter, 5-mm thick) were fabricated from In-Ceram Alumina and divided into two groups (n = 20) in accordance with surface treatment: (1) sandblasting by aluminum oxide particles (50 μm Al 2O 3) (SB) and (2) silica coating (30 μm SiO x) using the CoJet system (SC). After the 40 sp were bonded to the dual-cured RC, they were stored in distilled water at 37°C for 24 hours. After this period, the sp from each group were divided into two conditions of storage (n = 10): (a) 24 h-shear bond test 24 hours after cementation; (b) Aging-thermocycling (TC) (12,000 times, 5 to 55°C) and water storage (150 days). The shear test was performed in a universal test machine (1 mm/min). Results: ANOVA and Tukey (5%) tests noted no statistically significant difference in the bond strength values between the two surface treatments (p= 0.7897). The bond strengths (MPa) for both surface treatments reduced significantly after aging (SB-24: 8.2 ± 4.6; SB-Aging: 3.7 ± 2.5; SC-24: 8.6 ± 2.2; SC-Aging: 3.5 ± 3.1). Conclusion: Surface conditioning using airborne particle abrasion with either 50 μm alumina or 30 μm silica particles exhibited similar bond strength values and decreased after long-term TC and water storage for both methods. © 2011 by The American College of Prosthodontists.