Application of impedance spectroscopy to evaluate the effect of different setting accelerators on the developed microstructures of calcium phosphate cements

The main goal of the present study was to evaluate the effect of different setting accelerator agents on the developed microstructures of calcium phosphate cements (CPCs) by employing the impedance spectroscopy (IS) technique. Six compositions of CPCs were prepared from mixtures of commercial dicalcium phosphate anhydrous (DCPA) and synthesized tetracalcium phosphate (TTCP) as the solid phases. Two TTCP/DCPA molar ratios (1/1 and 1/2) and three liquid phases (aqueous solutions of Na(2)HPO(4), tartaric acid (TA) and oxalic acid (OA), 5% volume fraction) were employed. Initial (I) and final (F) setting times of the cement pastes were determined with Gillmore needles (ASTM standard C266-99). The hardened samples were characterized by X-ray powder diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and apparent density measurements. The IS technique was employed as a non-destructive tool to obtain information related to porosity, tortuosity and homogeneity of the cement microstructures. The formulation prepared from a TTCP/DCPA equimolar mixture and OA as the liquid phase presented the shortest I and F (12 and 20 min, respectively) in comparison to the other studied systems. XRD analyses revealed the formation of low-crystallinity hydroxyapatite (HA) (as the main phase) as well as the presence of little amounts of unreacted DCPA and TTCP after 24 h hardening in 100% relative humidity. This was related to the proposed mechanisms of dissolution of the reactants. The bands observed by FTIR allowed identifying the presence of calcium tartrate and calcium oxalate in the samples prepared from TA and OA, in addition to the characteristic bands of HA. High degree of entanglement of the formed crystals was observed by SEM in samples containing OA. SEM images were also correlated to the apparent densities of the hardened cements. Changes in porosity, tortuosity and microstructural homogeneity were determined in all samples, from IS results, when the TTCP/DCPA ratio was changed from 1/1 to 1/2. The cement formulated from an equimolar mixture of TTCP/DCPA and OA as the liquid phase presented setting times, degree of conversion to low-crystallinity HA and microstructural features suitable to be used as potential bone cement in clinical applications. The IS technique was shown to be a very sensitive and non-destructive tool to relate the paste composition to the developed microstructures. This approach could be very useful to develop calcium phosphate bone cements for specific clinical demands.

Apical leakage following root canal dressing with calcium hydroxide.

The purpose of this study was to analyse the apical leakage in teeth filled by the lateral condensation technique following medication with calcium hydroxide. One hundred and twenty extracted human teeth were biomechanically prepared by using exclusively reaming motion with files up to #40. Half of the teeth received a calcium hydroxide dressing for 3 days. The medication was removed by irrigation and reaming motion with files #40 up to #70. The teeth were divided in 6 experimental groups, according to the dimension of the utilized instrument. The root canals were filled and posteriorly the teeth were placed into a 2% methylene blue dye solution inside a flask, which was attached to a vacuum pump. Leakage was measured linearly, and the results showed significantly (p<0.01) less leakage in the experimental groups that received calcium hydroxide dressings than in the control groups. The results persisted even after the removal of 300 micrometers of dentin from the root canal dentinal walls.

Apical leakage after root canal filling with an experimental calcium hydroxide gutta-percha point

This study was an in vitro analysis of the apical seal of root canals filled with an experimental calcium hydroxide gutta-percha point. One hundred and ten recently extracted human permanent teeth with a single root were used. The root canals were biomechanically prepared, and some received a dressing of calcium hydroxide for 7 days. Root canals not dressed were filled by the lateral condensation technique with either regular gutta-percha or calcium hydroxide gutta-percha points. The dressed root canals were filled with the same sealers and regular gutta-percha points. The specimens were placed into a 2% methylene blue dye solution under vacuum, and the apical leakage was linearly evaluated. The experimental groups with calcium hydroxide dressing and the one with calcium hydroxide gutta-percha points exhibited significantly (p < 0.05) less leakage than the groups filled with regular gutta-percha points. The results obtained indicated that calcium hydroxide guttapercha points produced an improvement in the apical sealing quality of the root canal filling. Copyright © 1996 by The American Association of Endodontists.

Calcium hydroxide and a corticosteroid-antibiotic association as dressings in cases of biopulpectomy. A comparative study in dogs' teeth.

The subject of this paper was to study the behavior of the periapical tissues of dogs' teeth after biopulpectomy and dressing with calcium hydroxide or a corticosteroid-antibiotic association, before root canal filling with zinc oxide eugenol (ZOE) or Sealapex sealers. The teeth were overinstrumented and dressed for 7 days before the root canal filling. The animals were sacrificed 180 days after treatment and the specimens were prepared for morphological analysis. Specimens treated with Sealapex presented a higher number of cases with biological closure than ZOE. When the root canals were filled with ZOE, better results were observed with the use of the Ca(OH)2 dressing.

Healing process of dog dental pulp after pulpotomy and pulp covering with mineral trioxide aggregate or Portland cement.

Considering several reports about the similarity between the chemical compositions of the mineral trioxide aggregate (MTA) and Portland cement (PC), the subject of this investigation was to analyze the behavior of dog dental pulp after pulpotomy and direct pulp protection with these materials. After pulpotomy, the pulp stumps of 26 roots of dog teeth were protected with MTA or PC. Sixty days after treatment, the animal was sacrificed and the specimens removed and prepared for histomorphological analysis. There was a complete tubular hard tissue bridge in almost all specimens. In conclusion, MTA and PC show similar comparative results when used in direct pulp protection after pulpotomy.

Physico-chemical properties of MTA and a novel experimental cement

Aim: To evaluate the release of calcium ions, pH and conductivity of a new experimental dental cement (EC) and to compare them with those of mineral trioxide aggregate (MTA-Angelus). Methodology: Five samples of each cement were prepared using plastic tubes 1 mm in diameter and 10 mm long. Each sample was sealed in a test tube containing 10 mL deionized water which was analysed after 24, 48, 72, 96, 192, 240 and 360 h for pH, electrical conductivity and calcium release. The concentration of calcium ions was obtained through atomic absorption spectroscopy technique. The data were analysed statistically using the analysis of variance (ANOVA) and the Student's test (t-test). Results: The pH of the storage solutions was not affected by the material and the interaction of material with time (P > 0.05). However, the time of immersion was significant (P < 0.01) for both materials. For the electric conductivity and calcium release, the interaction of material with time was statistically significant (P < 0.01), indicating that EC and MTA-Angelus did not behave in a similar manner. Conclusions: The experimental cement released calcium and increased the pH of the storage solutions in a similar manner to MTA-Angelus. However, EC showed significantly higher calcium release than commercial MTA-Angelus after 24 h. © 2005 International Endodontic Journal.

Effect of rotary instrumentation and of the association of calcium hydroxide and chlorhexidine on the antisepsis of the root canal system in dogs

This study aimed at evaluating the antisepsis of the root canal system (RCS) and periapical region (PR) provided by rotary instrumentation associated with chlorhexidine + calcium hydroxide as intracanal medicament. Chronic periapical lesions were induced in 26 pre-molar roots in two dogs. After microbiological sampling, automatic instrumentation using the Profile system and irrigation with 5.25% sodium hypochlorite solution, with a final rinse of 14.3% EDTA followed by profuse irrigation with physiological saline were carried out in 18 root canals. After drying the canals, a paste based on calcium hydroxide associated with a 2% chlorhexidine digluconate solution was placed inside them. After 21 days, the medication was removed, leaving the root canals empty and coronally sealed. After 96 hours, a final microbiological sample was obtained, followed by histomicrobiological processing by the Brown & Brenn method. Eight untreated root canals represented the control group (C-G). Based on the Mann-Whitney test at a confidence level of 5% (p < 0.05), the procedures of antisepsis used offered significant efficacy (p < 0.05) resulting in 100.0% of the canals free of microorganisms. In the C-G, an elevated incidence of various microbial morphotypes was confirmed in all sites of the RCS, with the presence of microbial colonies in the periapical region. In contrast, the experimental group showed a similar pattern of infection in the RCS, although less intense and a reduced level of periapical infection (p < 0.05). It was concluded that adequate instrumentation followed by the application of calcium hydroxide + chlorhexidine offered significant elimination of microorganisms.

Effects of hemostatic agents on the histomorphologic response of human dental pulp capped with calcium hydroxide

Objective: To evaluate the response of human pulps capped with a calcium hydroxide [Ca(OH)2] cement after bleeding control with 2 hemostatic agents. Method and Materials: Pulps were exposed on the occlusal floor, and the bleeding was controlled either with saline solution (SS) or 2.5% sodium hypochlorite (NaOCI) (SH). After that, the pulp was capped with Ca(OH) 2 cement and restored with resin composite. After 30 (groups SS30 and SH30) and 60 (groups SS60 and SH60) days, the teeth were extracted and processed with hematoxylin-eosin and categorized in a histologic score system. The data were subjected to Kruskal-Wallis and Mann-Whitney tests (α = .05). Results: Regarding dentin bridge formation, an inferior response of SH60 group was observed when compared to SS60 (P < .05). The response of the SH30 group generally was similar to that of the groups treated with saline solution. However, after 60 days, 2.5% NaOCl showed a trend toward having an inferior response. Conclusion: Using saline solution as a hemostatic agent before pulp capping with Ca(OH)2 resulted in a significantly better histomorphologic response than using 2.5% NaOCl as a hemostatic agent before capping with Ca(OH)2.

Antimicrobial activity of endodontic sealers based on calcium hydroxide and MTA.

The aim of this study was to evaluate the antimicrobial activity of a new root canal sealer containing calcium hydroxide (Acroseal) and the root canal sealer based on MTA (Endo CPM Sealer), in comparison with traditional sealers (Sealapex, Sealer 26 and Intrafill) and white MTA-Angelus, against five different microorganism strains. The materials and their components were evaluated after manipulation, employing the agar diffusion method. A base layer was made using Müller-Hinton agar (MH) and wells were made by removing agar. The materials were placed into the wells immediately after manipulation. The microorganisms used were: Micrococcus luteus (ATCC9341), Staphylococcus aureus (ATCC6538), Pseudomonas aeruginosa (ATCC27853), Candida albicans (ATCC 10231), and Enterococcus faecalis (ATCC 10541). The plates were kept at room temperature for 2 h for prediffusion and then incubated at 37 degrees C for 24 h. The results showed that Sealapex and its base paste, Sealer 26 and its powder, Endo CPM Sealer and its powder, white MTA and its powder all presented antimicrobial activity against all strains. Intrafill and its liquid presented antimicrobial activity against all strains except P. aeruginosa and Acroseal was effective only against M. luteus and S. aureus.

In vivo biological behavior of calcium phosphate cements with different Ca/P ratio

Bioceramics with different Ca/P ratio were prepared from a mechanical mixture of NaPO3, CaCO3, Ca(OH)2 and phosphate buffer solution and implanted in rats subcutaneous tissues. The cements were characterized by Thermo gravimetric analysis (TG-TDA), X-ray diffraction and 31P-NMR. The implant sites were excised after 1, 4 and 16 weeks, fixed, dehydrated, included in paraffin wax for serial cutting and examined under the light transmitted microscope. They were biocompatible and biodegradable when implanted in rat subcutaneous. None of the materials induced ectopic osteogenesis. According to the results, the studied materials seem to be able for manufacturing reabsorbable bone implants.

Radiopacity evaluation of root canal sealers containing calcium hydroxide and MTA

The purpose of this study was to evaluate the radiopacity of root canal sealers containing calcium hydroxide and MTA (Acroseal, Sealer 26, Sealapex, Endo CPM Sealer, Epiphany and Intrafill). Five disc-shaped specimens (10 x 1 mm) were fabricated from each material, according to the ISO 6876/2001 standard. After setting of the materials, radiographs were taken using occlusal film and a graduated aluminum stepwedge varying from 2 to 16 mm in thickness. The dental X-ray unit (GE1000) was set at 50 kVp, 10 mA, 18 pulses/s and distance of 33.5 cm. The radiographs were digitized and the radiopacity compared to that of the aluminum stepwedge using VIXWIN-2000 software (Gendex). The data (mmAl) were analyzed statistically by ANOVA and Tukey's test at the 5% significance level. Epiphany and Intrafill presented the highest radiopacity values (8.3 mmAl and 7.5 mmAl respectively, p < 0.05) followed by Sealer 26 (6.3 mmAl), Sealapex (6.1 mmAl) and Endo CPM Sealer (6 mmAl). Acroseal was the least radiopaque material (4 mmAl, p < 0.05). In conclusion, the calcium hydroxide- and MTA-containing root canal sealers had different radiopacities. However, all materials presented radiopacity values above the minimum recommended by the ISO standard. © 2009 Sociedade Brasileira de Pesquisa Odontológica.

Sealing ability of retrograde obturation materials containing calcium hydroxide or MTA

Newly available materials for retrograde obturation should have their sealing properties evaluated. The goal of this study was to evaluate the sealing ability of Endo CPM sealer, an MTA-based endodontic cement. Single-rooted extracted human teeth were endodontically treated. After apical sectioning, retrograde cavities were prepared. Teeth were divided into five experimental groups (n=12), in which the following materials were used: Sealer 26 (S26), white Mineral Trioxide Aggregate (MTA), Endo CPM Sealer (CPM1), Endo CPM Sealer in thicker consistency (CPM 2), and zinc oxide and eugenol cement (ZOE), and two control groups (n=3). After retrograde obturation, the teeth were immersed in 0.2% rhodamine B dye for 48 hours in a vacuum chamber Marginal leakage data were subjected to ANOVA and Tukey tests at 5% significance level. S26 presented greater sealing ability (p<0.05) than ZOE, MTA, CPM1, and CPM2, all of which had similar results (p>0.05). We concluded that Sealer 26 has the greatest sealing ability. Endo CPM Sealer, with sealing ability similar to MTA, could be used as a retrograde obturation material.

Effect of different radiopacifying agents on the physicochemical properties of white portland cement and white mineral trioxide aggregate

Introduction: The aim of this study was to evaluate the pH, calcium ion release, setting time, and solubility of white mineral trioxide aggregate (WMTA) and white Portland cement (WPC) combined with the following radiopacifying agents: bismuth oxide (BO), calcium tungstate (CT), and zirconium oxide (ZO). Methods: Fifty acrylic teeth with root-end filling material were immersed in ultrapure water for measurement of pH and calcium release (atomic absorption spectrophotometry) at 3, 24, 72, and 168 hours. For evaluation of setting time, each material was analyzed according to the American Society for Testing and Materials guidelines 266/08. The solubility test was performed according to American National Standards Institute/American Dental Association specification no. 57/2000. Solubility, setting time, and pH values were compared by using analysis of variance and Tukey test, and the values of calcium release were compared by the Kruskal-Wallis and Miller tests. The significance level was set at 5%. Results: The pH and calcium release were higher at 3 and 24 hours. WPC was the material with the higher values for both properties. WMTA had the greatest solubility among all materials (P <.05). All radiopacifiers increased the setting time of WPC, and WMTA had the shortest setting time among all materials (P < .05). Conclusions: All materials released calcium ions. Except for WPC/CT at 168 hours, all materials promoted an alkaline pH. On the basis of the obtained results, ZO and CT can be considered as potential radiopacifying agents to be used in combination with Portland cement. Copyright © 2012 American Association of Endodontists.

Effects of calcium hydroxide addition on the physical and chemical properties of a calcium silicate-based sealer

Recently, various calcium silicate-based sealers have been introduced for use in root canal filling. The MTA Fillapex is one of these sealers, but some of its physicochemical properties are not in accordance with the ISO requirements. Objective: The aim of this study was to evaluate the flowability, pH level and calcium release of pure MTA Fillapex (MTAF) or containing 5% (MTAF5) or 10% (MTAF10) calcium hydroxide (CH), in weight, in comparison with AH Plus sealer. Material and Methods: The flowability test was performed according to the ISO 6876: 2001 requirements. For the pH level and calcium ion release analyses, the sealers were placed individually (n=10) in plastic tubes and immersed in deionized water. After 24 hours, 7 and 14 days, the water in which each specimen had been immersed was evaluated to determine the pH level changes and calcium released. Flowability, pH level and calcium release data were analyzed statistically by the ANOVA test (alpha=5%). Results: In relation to flowability: MTAF>AH Plus>MTAF5>MTAF10. In relation to the pH level, for 24 h: MTAF5=MTAF10=MTAF>AH Plus; for 7 and 14 days: MTAF5=MTAF10>MTAF>AH Plus. For the calcium release, for all periods: MTAF>MTAF5=MTAF10>AH Plus. Conclusions: The addition of 5% CH to the MTA Fillapex (in weight) is an alternative to reduce the high flowability presented by the sealer, without interfering in its alkalization potential.

Effect of colloidal silica on the mechanical properties of fiber-cement reinforced with cellulosic fibers

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)