Renata Antoun Simão

High temperature AFM study of CAP 30/45 pen grade bitumen

Bitumen is a complex mixture of hydrocarbons for which microstructural understanding is incomplete. In an effort to detail this microstructure, a asphalt cement sample (CAP 30/45) was analysed by thermal phase detection atomic force microscopy. Phase contrast and topography images showed that sample morphology is highly dependent on temperature. The ‘bee structure’ changed considerably at temperatures between 50°C and 56°C. A decrease of the oscillation amplitude was observed upon heating and the ‘bees’ completely disappeared at temperatures above 57°C. When the temperature was decreased after melting at 170°C, the ‘bees’ began to nucleate gradually at temperatures of 57°C and its evolution with time was followed. Changes in morphology were compared to thermal analysis results and a model for the ‘bee’ structure was proposed.

High resolution imaging of the microstructure of maize starch films

Glycerol-plasticised and non-plasticised cast films were prepared from maize starch suspensions that had been heated under reflux for different periods of time. Light microscopy (LM) and atomic force microscopy (AFM) have been used to observe the morphology of the starch films. In general, LM and AFM topographic images of corresponding non-plasticised films were similar. AFM topographic images of plasticised films revealed differences associated with the retarding effect of glycerol on the gelatinisation process. Relatively high B-type crystallinity indices were determined for plasticised films, independently of the heating conditions to which the suspensions had been submitted. AFM topographic images of plasticised films at higher magnifications revealed smooth and rough domains, that were detailed by phase contrast imaging.

Scanning Electron Microscopic Investigation of the Effectiveness of Phosphoric Acid in Smear Layer Removal When Compared with EDTA and Citric Acid

INTRODUCTION The smear layer adheres to dentinal surface, thus occluding the dentinal tubules. Because this layer disfavors the penetration of irrigant solutions and root canal fillings, it should be removed. The aim of this study was to compare the effectiveness of 37% phosphoric acid with that of 17% EDTA and 10% citric acid in the removal of smear layer. MATERIALS AND METHODS Fifty-two maxillary single-rooted human canines were accessed and instrumented. Between each instrument used, the canals were irrigated with sodium hypochlorite. After instrumentation, the teeth were irrigated with distilled water and then divided into groups according to the time and substances employed. The substances used were 17% EDTA, 10% citric acid, and 37% phosphoric acid solution and gel. The experimental time periods were of 30 seconds, 1 minute, and 3 minutes. The samples were prepared and observed by means of scanning electron microscopy. Three photomicrographs (2,000×) were recorded for each sample regarding the apical, middle, and cervical thirds. A score system was used to evaluate the images. RESULTS None of the substances analyzed in this study was effective for removing the smear layer at 30 seconds. In the 1-minute period, the phosphoric acid solution showed better results than the other substances evaluated. In the 3-minute period, all the substances worked well in the middle and cervical thirds although phosphoric acid solution showed excellent results even in the apical third. CONCLUSIONS These findings point toward the possibility that phosphoric acid solution could be a promising agent for smear layer removal.

Effect of Different Irrigation Protocols on Resin Sealer Bond Strength to Dentin

INTRODUCTION The aim of this study was to evaluate the influence of different irrigation protocols on resin-based sealer bond strength to dentin and the associated failure pattern. METHODS One hundred eighty single-rooted premolars were used. Roots were divided into 18 groups according to the irrigation protocol used and instrumented using 5.25% NaOCl or 2% chlorhexidine (CHX) gel as chemical auxiliary substances and 17% EDTA or 37% phosphoric acid for smear layer removal. Finally, CHX solution was used as the final irrigant in some groups. Root canals were filled with either gutta-percha and AH Plus (Dentsply, Petropolis, RJ, Brazil) (GP/AH) or Resilon/Real Seal SE (SybronEndo, Orange, CA). Bond strength was measured by the push-out test. Additionally, failure patterns were classified as adhesive, cohesive, and mixed. Data were statistically analyzed by Kruskal-Wallis and Mann-Whitney U tests. RESULTS In the GP/AH groups, high bond strength values were obtained when NaOCl was associated with phosphoric acid with (6.9 ± 3.9) and without (7.4 ± 3.8) a final flush with CHX. However, when CHX gel was used, the association with EDTA with (7.5 ± 3.2) and without (6.0 ± 2.3) a final flush with CHX solution showed better results. The GP/AH groups mainly showed a cohesive failure pattern. Evaluation of Resilon/Real Seal SE showed that higher bond strength values were reached when CHX was associated with phosphoric acid with (5.2 ± 3.0) and without (4.2 ± 2.0) a final flush with CHX solution. The failure patterns were mainly adhesive. CONCLUSIONS Irrigation protocols influenced the bond strength of resin sealers to dentin.

Mechanical properties of asphalt binders evaluated by atomic force microscopy.

Atomic Force Microscopy was employed in order to relate the features observed on the surface of a 50/70 asphalt binder according to its local stiffness and elastic recovery. Indentations were performed in different points of the surface and a significant variation of elasticity was observed between the points on the so‐called bee structure and the matrix. Also, indentations varying the maximum force were performed on similar white spots in the bee structure and the recovery was followed up to 1 h after indentation. It was observed that the elastic recovery is very much dependent on the colloidal structure of the bee. The final surface state of the binder, close to the bee for usual bees is not the same as the initial one indicating severe plastic deformation. Also, permanent phase change could be observed for bright spots presented in not well‐structured bee arrangements. A surface hardening was observed in the bee region.

Interactions between Irrigants Commonly Used in Endodontic Practice: A Chemical Analysis

INTRODUCTION The aim of this work was to characterize the by-products formed in the associations between the most commonly used irrigants in endodontic practice through electrospray ionization quadrupole time-of-flight mass spectrometry analyses. METHODS Sodium hypochlorite (NaOCl) (0.16%, 1%, 2.5%, and 5.25%) was associated with 2% chlorhexidine (CHX) solution and gel, 17% EDTA, 10% citric acid, 37% phosphoric acid, saline solution, ethanol, and distilled water. CHX solution and gel were also associated with all above mentioned irrigants. The solutions were mixed in a 1:1 ratio, and electrospray ionization quadrupole time-of-flight mass spectrometry was used to characterize the precipitates when formed. RESULTS CHX produced an orange-brown precipitate when associated with NaOCl from 1%-5.25% and an orange-white precipitate when associated with 0.16% NaOCl. When associated with EDTA, CHX produced a white milky precipitate, and when associated with saline solution and ethanol, a salt precipitation was produced. No precipitation was observed when CHX was associated with citric acid, phosphoric acid, or distilled water. In the NaOCl associations, precipitation occurred only when CHX was present. CONCLUSION The orange-brown precipitate observed in the association between CHX and NaOCl occurs because of the presence of NaOCl, an oxidizing agent causing chlorination of the guanidino nitrogens of the CHX. The precipitates formed in the reaction of CHX with EDTA, saline solution, and ethanol were associated with acid-base reactions, salting-out process, and lower solubility, respectively. NaOCl associated with EDTA, citric acid, and phosphoric acid leads mainly to chlorine gas formation. Intermediate flushes with distilled water seem to be appropriate to prevent or at least reduce formation of by-products.

Hydrophobic corn starch thermoplastic films produced by plasma treatment.

Polymer coating technology is currently an important field in science as it can lead to final products with enhanced characteristics characterized by desired bulk and surface properties. Low power plasmas can induce the polymerization of a precursor gas on the substrate surface as well as introduce functional groups under specific plasma conditions. In the present work, we studied the possibility of reducing water sensitivity of corn starch films by sulfur hexafluoride (SF(6)) plasma treatment. Confocal laser microscopy as well as atomic force microscopy was used to observe the main surface modifications and results indicated starch cross-linking. Fluoride was incorporated to the surface and the relationship between fluoride and sulfur incorporation to the surface was very much dependent on plasma power. Results indicate that fluoride could be preferentially incorporated on polymeric surfaces at -100V self-bias and the overall surface morphology determined the measured contact angle. The dynamic behavior of surface contact angle was observed to be very much dependent on the treatment time and force-distance curves were used to further characterize the chemical surface modifications locally. Optimized treatment conditions led to water contact angles up to 130 degrees . Even after being in contact with water for 10min, surfaces remained hydrophobic, presenting contact angles over 100 degrees .

Evaluation of the interaction between endodontic sealers and dentin treated with different irrigant solutions.

INTRODUCTION Dentin surface treatment with different substances might cause alterations in chemical and structural compositions of the human dentin. The aim of this study was to investigate the wettability of endodontic sealers in contact with dentin treated with 5.25% sodium hypochlorite (NaOCl) and 2% chlorhexidine (CHX) in the presence or absence of smear layer. METHODS Thirty-six dentin slices were used. They were irrigated with NaOCl and washed with distilled water (DW) to simulate irrigation during chemomechanical preparation. After this procedure, the samples were divided into 6 groups: group 1, DW (control); group 2, NaOCl + DW; group 3, CHX + DW; group 4, ethylenediaminetetraacetic acid (EDTA) + DW; group 5, EDTA + DW + NaOCl + DW; group 6, EDTA + DW + CHX + DW. The Ramé-Hart goniometer was used to measure the contact angle between the dentin surfaces and the AH Plus and Real Seal SE sealers. Data were statistically analyzed. RESULTS With regard to the contact angle between AH Plus and treated surfaces, the values of contact angle were lower when CHX was used, regardless of the presence or absence of smear layer. When Real Seal SE was evaluated, in the absence of smear layer, CHX presented lower values of contact angle. In the presence of smear layer, the use of NaOCl and CHX did not favor the spread of the sealer. CONCLUSIONS The present study has revealed that smear layer removal and final flush with CHX favor the wettability of AH Plus and Real Seal SE sealers.

Surface modification of porous polymeric membranes by RF-plasma treatment

Abstract Polymeric membranes can be modified by surface treatment with glow discharge created by non-polymerizable gases, with low power radio-frequency (rf) plasma. The purpose of this work is to study the influence of the exposure time, the supplied power and the nature of the gas on the permeability of the treated membranes. Asymmetric porous substrates of polysulfone (PSf) were used and their surfaces were modified with inorganic gas plasma (ammonia). Three rf power levels, respectively 5, 10 and 15 W were used. Treatment time ranged from 1 to 50 min. The chemical and structural characterization of the membranes before and after the surface modification was done by means of Atomic Force Microscopy (AFM), Scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). The permeated flow of pure gases (N 2 and CO 2 ) was measured using conventional gas permeation cell at room temperature.

Effect of disinfectant solutions on the surface free energy and wettability of filling material.

INTRODUCTION Gutta-percha (GP) and Resilon (Res) cones are usually disinfected by the use of solutions such as sodium hypochlorite (NaOCl) and chlorhexidine (CHX). The aims of this study were to evaluate the surface free energy of GP and Res cones after disinfection procedures and to investigate the wettability of endodontic sealers in contact with these surfaces. METHODS GP and Res flat smooth surfaces were prepared. Thirty-six samples of each material were used. The samples were divided into 6 groups as follows: Control group GP, immersed in Milli-Q water (MQW); CHX group GP, immersed in 2% CHX solution and then washed with MQW; NaOCl group GP, immersed in 5.25% NaOCl and then washed with MQW; Control group Res, immersed in MQW; CHX group Res, immersed in 2% CHX solution and then washed with MQW; and NaOCl group Res, immersed in 5.25% NaOCl and then washed with MQW. Samples were analyzed first with a goniometer to measure the contact angle between the test surfaces and 3 solutions (water, ethylene glycol, and diiodomethane) to determine the surface free energy. Then the contact angle between surfaces and each one of the sealers tested, AH Plus and Real Seal SE, was measured. Data were statistically analyzed. RESULTS The results showed that when disinfectant solutions were used, the surface free energy was greater. When evaluating the interaction between materials and sealers, the use of CHX presented lower values of contact angle, followed by NaOCl. CONCLUSIONS It was concluded that the solutions used in decontamination increase the surface free energy, promoting high interaction between GP/Res and sealers.