Carlos Eduardo Saraiva Miranda

Changes in the surface of four calcium silicate-containing endodontic materials and an epoxy resin-based sealer after a solubility test

AIM To compare the changes in the surface structure and elemental distribution, as well as the percentage of ion release, of four calcium silicate-containing endodontic materials with a well-established epoxy resin-based sealer, submitted to a solubility test. METHODOLOGY Solubility of AH Plus, iRoot SP, MTA Fillapex, Sealapex and MTA-Angelus (MTA-A) was tested according to ANSI/ADA Specification 57. The deionized water used in the solubility test was submitted to atomic absorption spectrophotometry to determine and quantify Ca(2+), Na(+), K(+), Zn(2+), Ni(2+) and Pb(2+) ions release. In addition, the outer and inner surfaces of nonsubmitted and submitted samples of each material to the solubility test were analysed by means of scanning electron microscopy and energy-dispersive spectroscopy (SEM/EDX). Statistical analysis was performed by using one-way anova and Tukeys post hoc tests (α = 0.05). RESULTS Solubility results, in percentage, sorted in an increasing order were -1.24 ± 0.19 (MTA-A), 0.28 ± 0.08 (AH Plus), 5.65 ± 0.80 (Sealapex), 14.89 ± 0.73 (MTA Fillapex) and 20.64 ± 1.42 (iRoot SP). AH Plus and MTA-A were statistically similar (P > 0.05), but different from the other materials (P < 0.05). High levels of Ca(2+) ion release were observed in all groups except AH Plus sealer. MTA-A also had the highest release of Na(2+) and K(+) ions. Zn(+2) ion release was observed only with AH Plus and Sealapex sealers. After the solubility test, all surfaces had morphological changes. The loss of matrix was evident and the filler particles were more distinguishable. EDX analysis displayed high levels of calcium and carbon at the surface of Sealapex, MTA Fillapex and iRoot SP. CONCLUSIONS AH Plus and MTA-A were in accordance with ANSI/ADAs requirements regarding solubility whilst iRoot SP, MTA Fillapex and Sealapex did not fulfil ANSI/ADAs protocols. High levels of Ca(2+) ion release were observed in all materials except AH Plus. SEM/EDX analysis revealed that all samples had morphological changes in both outer and inner surfaces after the solubility test. High levels of calcium and carbon were also observed at the surface of all materials except AH Plus and MTA-A.

Push-out strength of root fillings with or without thermomechanical compaction

AIM To evaluate the influence of thermomechanical compaction (Taggers hybrid technique - THT) on the push-out strength of several root filling materials to root dentine. METHODOLOGY Root canals of eighty roots in human canines were prepared with the ProTaper system and filled with one of the following materials, using either lateral compaction (LC) (n = 40) or THT (n = 40): AH Plus/gutta-percha (GP) (n = 10), Sealer 26/GP (n = 10), Epiphany SE/Resilon (n = 10) and Epiphany SE/GP (n = 10). Three 2-mm-thick dentine slices were obtained from each third of each root. The root filling in the first slice was subjected to a push-out test to evaluate the bond strength of the materials to intraradicular dentine. Data (in MPa) were analysed using anova and post hoc Tukeys test (P < 0.05). Failure mode was determined at × 25 magnification. The other two slices were prepared for scanning electron microscopy (SEM) to examine the surface of the filling materials. RESULTS Lateral compaction (1.34 ± 1.14 MPa) was associated with a significantly higher bond strength (P < 0.05) than the THT (0.97 ± 0.88 MPa). AH Plus/GP (2.23 ± 0.83 MPa) and Sealer 26/GP (1.86 ± 0.50 MPa) had significantly higher bond strengths than the other materials and differed significantly from each other (P < 0.05). There was a significant difference (P < 0.05) between the coronal (1.36 ± 1.15 MPa), middle (1.14 ± 1.05 MPa) and apical thirds (0.95 ± 0.83 MPa). Considering the technique and root filling material interaction, AH Plus/GP-LC was associated with the highest mean values (2.65 ± 0.66 MPa) (P < 0.05). Sealer 26/GP-LC (2.10 ± 0.46 MPa), AH Plus/GP-THT (1.81 ± 0.78 MPa) and Sealer 26/GP-TH (1.63 ± 0.44 MPa) had intermediate values that were not significantly different from each other (P > 0.05). Epiphany SE was associated with the lowest mean values (3.70 ± 0.86 MPa) (P < 0.05), regardless of the root filling technique and type of solid material (cone). Adhesive failures predominated in the specimens filled with Epiphany SE, whilst mixed and cohesive failures were more frequent in those filled with AH Plus and Sealer 26, regardless of the root filling technique. SEM analysis revealed that LC produced a dense and well-compacted filling whilst the use of a hybrid thermomechanical technique resulted in the solid material (GP or Resilon) intermingled within sealer to form a nonhomogenous mass. CONCLUSION Lateral compaction was associated with higher bond strengths of the materials to intraradicular dentine than a hybrid technique using thermomechanical compaction. The greatest push-out strengths were obtained when the canals were filled with LC of AH Plus and GP cones.

Physicochemical Properties of Methacrylate Resin–based Root Canal Sealers

INTRODUCTION This study assessed in vitro the physicochemical properties of 2 methacrylate resin-based sealers (Epiphany SE and Hybrid Root SEAL), comparing the results with a well-established epoxy resin-based sealer (AH Plus). METHODS Five samples of each material were used for each test (setting time, flow, radiopacity, dimensional change after setting, and solubility) according to American National Standards Institute/American Dental Association (ANSI/ADA) Specification 57. The samples were assigned to 3 groups: I, AH Plus; II, Epiphany SE; and III, Hybrid Root SEAL. The distilled and deionized water used at the solubility test was submitted to atomic absorption spectrometry to observe the presence of Ca2+, K+, Ni2+, and Zn2+ ions. In addition, the surface morphology of the specimens was analyzed by means of scanning electron microscopy (SEM). Statistical analysis was performed by using one-way analysis of variance and Tukey-Kramer test (P < .05). RESULTS Flow, radiopacity, and solubility of all sealers were in accordance with ANSI/ADA. The setting time of Hybrid Root SEAL did not agree with ANSI/ADA requirements. The dimensional change of all sealers was greater than the values considered acceptable by ANSI/ADA. The spectrometry analysis showed significant Ca(2+) ions release for AH Plus. In SEM analysis, Hybrid Root SEAL presented spherical monomers with inferior size than AH Plus and Epiphany SE. CONCLUSIONS It might be concluded that physicochemical properties of the tested sealers conformed to ANSI/ADA (2000) standardization, except for the setting time of Hybrid Root SEAL and the dimensional change of all sealers, which did not fulfill the ANSI/ADA requirements.

Bond Strength of Epiphany Sealer Prepared with Resinous Solvent

This study evaluated in vitro the bond strength of Epiphany sealer prepared with resinous solvent of Epiphany system (Thinning resin) by using a push-out test. Forty maxillary canines were sectioned transversally below the cementoenamel junction to provide 4-mm-thick dentin disks that were centered in aluminum rings and embedded in acrylic resin. Root canals were prepared with tapered diamond bur. Intraradicular dentin was treated with 1% NaOCl for 30 minutes, 17% ethylenediaminetetraacetic acid for 5 minutes, and flushed with distilled water for 1 minute. The specimens were randomly distributed into 4 groups (n = 10) according to the filling material: GI, Epiphany without photoactivation; GII, Epiphany prepared with solvent without photoactivation; GIII, Epiphany followed by photoactivation; and GIV, Epiphany prepared with solvent followed by photoactivation. After the setting time, the specimens were submitted to the push-out test. The highest mean value (14.91 +/- 2.82 MPa) was obtained with Epiphany prepared with solvent followed by photoactivation (GIV), which was statistically different (P < .01) from the other groups. Groups I (8.15 +/- 2.47 MPa), II (9.46 +/- 2.38 MPa), and III (9.80 +/- 2.51 MPa) had inferior bond strength values and were statistically similar among themselves (P > .01). The resinous solvent of Epiphany system increased the bond strength of Epiphany sealer to dentin walls when followed by photoactivation.

Physicochemical properties of endodontic sealers of different bases

Objective To assess the setting time (ST), flow (FL), radiopacity (RD), solubility (SB) and dimensional change following setting (DC) of different sealers (AH Plus®, Polifil, Apexit Plus®, Sealapex®, Endométhasone® and Endofill® according to American National Standards Institute/American Dental Association (ANSI/ADA) Specification 57. Material and methods Five samples of each material were used for each test. For ST, cast rings were filled with sealers and tested with a Gilmore needle. For FL, the sealer was placed on a glass plate. After 180 s, another plate with 20 g and a load of 100 g were applied on the material, and the diameters of the discs formed were measured. In RD, circular molds were filled with the sealers, radiographed and analyzed using Digora software. For SB, circular molds were filled with the sealers, a nylon thread was placed inside the material and another glass plate was positioned on the set, pressed and stored at 37ºC. Samples were weighed, placed in water, dried and reweighed. The water used for SB was analyzed by atomic absorption spectrometry. For DC, circular molds were filled with the sealers, covered by glass plates and stored at 37ºC. Samples were measured and stored in water for 30 days. After this period, they were dryed and measured again. Results Regarding ST, AH Plus®, Apexit® and Endofil® sealers are in accordance with ANSI/ADA standards. Endométhasones manufacturer did not mention the ST; Polifil is an experimental sealer and Sealapex® did not set. Considering RD, SB and DC, all sealers were in accordance with ANSI/ADA. The spectrometric analysis showed that a significant amount of K+ and Zn2+ ions was released from Apexit Plus® and Endofill®, respectively. Conclusion Except for DC, all other physicochemical properties of the tested sealers conformed to ANSI/ADA requirements.

Automated On-line Preconcentration for Trace Metals Determinationin Water Samples by Inductively Coupled Plasma Mass Spectrometry

A preconcentration flow system using the cationic resin AG50W-X8 for multielement determinations of trace constituents in water samples to work on-line with ICP-MS is described. The flow network comprises two small resin columns inserted in parallel channels of the injector port. Sample loading onto the columns occurs simultaneously and independently. Elution takes place intermittently through each column, releasing eluent fractions containing similar concentrations of the analytes, which are merged downstream. The volume of eluent in the alternate aliquots sent through the columns was adjusted to attain precise transient signals. Enrichment factors from 10 to 95 for sample loading times of 0.5 to 5 min were attained. The eluted band produced a transient peak with width at half peak maximum of approximately 20 s, enough to scan several masses for multielement determinations by ICP-MS. The feasibility of the proposed system was demonstrated by determination of Cd, Pb, Ni, Cu and Zn in the certified reference water sample SLRS-1. Accurate results were obtained using a preconcentration factor of 30 fold and a sample throughput of 20 samples per hour.

Interfacing flow injection with capillary electrophoresis and inductively coupled plasma mass spectrometry for Cr speciation in water samples

A hyphenated system coupling flow injection (FI), capillary electrophoresis (CE) and inductively coupled plasma mass spectrometry (ICP-MS) is proposed. Two interfaces were developed in order to couple all three systems: the first to couple FI to CE and the second to couple CE to ICP-MS. The first interface was a chamber with micro channels connecting the FI system to the electrophoresis capillary inlet. The capillary outlet was coupled to a concentric nebulizer in the ICP-MS by using the second interface with an electrolyte sheath flow and grounding electrode. Sample aliquots were sequentially introduced by the FI system with a few nanolitres being electrokinetically injected into the electrophoresis capillary in a reproducible manner. The system performed analysis of a continuous sequence of samples with no interruption of the applied voltage during sample replacement or column conditioning. The feasibility of this system was evaluated for Cr speciation. The separation time was improved by forming an anionic complex between Cr(III) and DTPA. Therefore, the analysis of both Cr species, Cr(III)-DTPA2− and CrO42−, attained compatible sample processing between CE and the interfaced techniques FI and ICP-MS. The anionic chromium species were separated in less than 2 min by applying 20 kV in a phosphate electrolyte with TTAOH (tetradecyltrimethylammonium hydroxide) as electroosmotic flow modifier adjusted to pH 8. The transient signals from both species monitored at m/z 53 were characterized by excellent resolution and precision. Peaks obtained using Cr(VI) and Cr(III) standard solutions with concentration ranging from 50 to 200 µg L−1 presented good correlation.

Evaluation of physico-chemical properties of Portland cements and MTA

The purpose of this study was to evaluate the hydrogenionic potential and electrical conductivity of Portland cements and MTA, as well as the amount of arsenic and calcium released from these materials. In Teflon molds, samples of each material were agitated and added to plastic flasks containing distilled water for 3, 24, 72 and 168 h. The results were analyzed with a Kruskal-Wallis non-parametric test for global comparisons and a Dunn-Tukey test for pairwise comparisons. The results revealed no significant differences in the pH of the materials (p > 0.05). The electrical conductivity of the cements were not statistically different (p > 0.05). White non-structural cement and MTA BIO released the largest amount of calcium ions into solution (p < 0.05), while arsenic release was insignificant in all of the materials (p > 0.05). The results indicated that the physico-chemical properties of Portland cements and MTA were similar. Furthermore, all materials produced an alkaline environment and can be considered safe for clinical use because arsenic was not released. The electrical conductivity and the amount of calcium ions released into solution increased over time.

An improved flow-injection system for spectrophotometric determination of molybdenum and tungsten in tool steels.

A flow-injection procedure for simultaneous spectrophotometric determination of tungsten and molybdenum in steel alloys is proposed. The method exploits the catalytic effects of Mo(VI) and W(VI) on the rate of iodide oxidation by hydrogen peroxide under acidic conditions. A novel strategy for ion-exchange separation of the potential interfering species is proposed, and an AG50W-X8 cationic resin mini-column is used. The sample is injected twice, originating two sequential plugs, citrate being added to one of them in order to suppress the W(VI) catalytic activity thus providing the kinetic discrimination. The system handles 70 samples per hour and requires 1.6mg KI per determination. A linear response is verified up to 10mgl(-1) Mo (or W) in the injectate, and signal additivity is 98-103%. Results are precise (R.S.D.<0.04) and in agreement with ICP-OES. Running a standard reference material (IPT-50) assessed also accuracy.

Radiopacity evaluation of Portland and MTA-based cements by digital radiographic system

Objective The aim of the present study was to evaluate the radiopacity of Portland and MTA-based cements using the Digora TM digital radiographic system. Material and Methods The performed tests followed specification number 57 from the American National Standard Institute/American Dental Association (2000) for endodontic sealing materials. The materials were placed in 5 acrylic plates, especially designed for this experiment, along with a graduated aluminum stepwedge varying from 1 to 10 mm in thickness. The set was radiographed at a 30 cm focus-object distance and with 0.2 s exposure time. After the radiographs were taken, the optical laser readings of radiographs were performed by Digora TM system. Five radiographic density readings were performed for each studied material and for each step of the aluminum scale. Results White ProRoot MTA (155.99±8.04), gray ProRoot MTA (155.96±16.30) and MTA BIO (143.13±16.94) presented higher radiopacity values (p<0.05), while white non-structural Portland (119.76±22.34), gray Portland (109.71±4.90) and white structural Portland (99.59±12.88) presented lower radiopacity values (p<0.05). Conclusions It was concluded that MTA-based cements were the only materials presenting radiopacity within the ANSI/ADA specifications.