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      Microstructural and Elemental Characterization of Root Canal Sealers Using FTIR, SEM, and EDS Analysis

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          Abstract

          Background: Root canal sealers and repair materials should have the desirable physical, chemical, and biological characteristics, and an antibacterial effect if possible. There is little information available on the biocompatibility of new sealers on the market. Fourier transform infrared spectroscopy (FTIR) can offer trustworthy data to examine chemical structures; another technique for revealing the elements in the constituents that may contribute to the cytotoxicity of these sealers is scanning electron microscopy (SEM), with the goal of elemental mapping utilizing energy-dispersive X-ray spectroscopy (EDX). Methodology: All the root canal sealers were mixed as per the manufacturers’ instructions and allowed to set in molds for 24 h. Then, the samples were placed into an incubator (Memmert GmbH + Co. KG, Schwabach, Germany for 72 h, in a moist environment to allow complete chemical setting of the sealers. The organic and inorganic components of the sample were identified using FTIR with the wavelength length in the infra-red region measuring 400–450 nm. The finely crushed samples were coated with gold metal; following that, the sealer samples were examined under a scanning electron microscope (SEM) at 5000×, 10,000×, and 20,000× magnification, followed by energy-dispersive X-ray spectroscopy. Results: The surfaces of BioRoot and DiaRoot sealers revealed a relatively uniform distribution of irregular micro-sized particles aggregated in clusters, with the particle size ranging from 1 to 65 µm and 0.4 to 55 µm, respectively. OneFill, iRoot, and CeraSeal demonstrated irregularly shaped particles with particle sizes of 0.5 to 105 µm, 0.5 to 195 µm, and 0.3 to 68 µm, respectively. The EDX microanalysis revealed that oxygen, calcium, and carbon were found in all the tested sealer materials. Silicone and zirconium were absent in DiaRoot, but DiaRoot contained fluoride and ytterbium. Moreover, aluminum was noted in DiaRoot, One Fill, and CeraSeal, and chloride was only observed in BioRoot. FTIR analysis revealed strong absorption bands at 666 cm−1 and 709 cm−1 in BioRoot. Bands at 739 cm−1, 804 cm−1, 863 cm−1, 898 cm−1, and 1455 cm−1 were observed in DiaRoot. Bands at 736 cm−1 and 873 cm−1 in OneFill suggested the presence of C-H bending. Similarly, bands were observed at 937 cm−1, 885 cm−1, 743 cm−1, and 1455 cm−1 in iRoot, representing C-H stretching. Conclusions: All root canal sealers had diverse surface morphologies that contained irregular, micro-sized particles that were uniformly distributed, and they lacked heavy metals. All the experimental sealers comprised mainly calcium, oxygen, and carbon.

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          Physical properties of 5 root canal sealers.

          The aim of this study was to evaluate the pH change, viscosity and other physical properties of 2 novel root canal sealers (MTA Fillapex and Endosequence BC) in comparison with 2 epoxy resin-based sealers (AH Plus and ThermaSeal), a silicone-based sealer (GuttaFlow), and a zinc oxide-eugenol-based sealer (Pulp Canal Sealer).
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            Evaluation of radiopacity, pH, release of calcium ions, and flow of a bioceramic root canal sealer.

            The aim of the present study was to evaluate the physicochemical properties of a bioceramic root canal sealer, Endosequence BC Sealer. Radiopacity, pH, release of calcium ions (Ca(2+)), and flow were analyzed, and the results were compared with AH Plus cement.
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              Apatite-forming ability (bioactivity) of ProRoot MTA.

              Apatite-forming ability, considered as an index of bioactivity (bond-to-bone ability), was tested on ProRoot MTA cement after immersion in phosphate-containing solution (DPBS). Disk samples were prepared and immersed in DPBS for 10 min, 5 h, 1 and 7 days. The cement surface was studied by attenuated total reflectance Fourier transform infrared (ATR-FTIR) spectroscopy, by micro-Raman spectroscopy and by environmental scanning electron microscope with energy dispersive X-ray (ESEM-EDX) analyses. The pH of the storage solution was also investigated. Spectroscopic analyses revealed calcium phosphate bands after 5-h immersion in DPBS. After 1 day, an even coating composed of apatite spherulites (0.1-0.8 micron diameter) was observed by ESEM/EDX. After 7 days, its thickness had increased. Apatite nucleation had already occurred after 5-h immersion. At this time, the presence of portlandite (i.e. Ca(OH)(2) , calcium hydroxide) on the cement surface was also observed; at longer times, this component was released into the medium, which underwent a remarkable pH increase. The study confirms the ability of ProRoot MTA to form a superficial layer of apatite within hours. The excellent bioactivity of ProRoot MTA might provide a significant clinical advantage over the traditional cements used for root-end or root-perforation repair. © 2010 International Endodontic Journal.
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                Journal
                ASPCC7
                Applied Sciences
                Applied Sciences
                MDPI AG
                2076-3417
                April 2023
                April 02 2023
                : 13
                : 7
                : 4517
                Article
                10.3390/app13074517
                18642cf9-9dbd-4c40-b8bf-07596b9617cf
                © 2023

                https://creativecommons.org/licenses/by/4.0/

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