Effect of calcium silicate and radiopacifier proportions on the physicochemical properties of endodontic calcium silicate-based sealers

Effect of calcium silicate and radiopacifier proportions on the physicochemical properties of endodontic calcium silicate-based sealers | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Research Article Effect of calcium silicate and radiopacifier proportions on the physicochemical properties of endodontic calcium silicate-based sealers Raimundo Sales Oliveira Neto, Guilherme Ferreira Silva, Tany Carvalho Moreira Veiga, and 5 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-6908130/v1 This work is licensed under a CC BY 4.0 License Status: Posted Version 1 posted You are reading this latest preprint version Abstract OBJECTIVES: This study investigated how varying calcium silicate (30-50%) and radiopacifier (45-65%) proportions affect the physicochemical properties in formulations P1–P3, compared to Bio-C Sealer, AH Plus Bioceramic and AH Plus Jet. MATERIAL AND METHODS: Flowability, solubility, and radiopacity were investigated according to ISO 6876/2012 standards. Setting times were measured based on ASTM C 266-2008 standards. Volumetric changes and pH were assessed using acrylic teeth (n=10) instrumented to #40.04 and filled with the sealers. pH was measured at 3, 24, 72, and 168 hours. The specimens were scanned using micro-CT immediately after filling and after 7 days. pH was measured at 3, 24, 72, and 168 hours. RESULTS: The P1 showed comparable initial setting time to AH Plus Bioceramic (p>0.05). All calcium silicate-based sealers demonstrated higher solubility than AH Plus Jet (p<0.05), with P3 being the only calcium silicate formulation that met ISO solubility standards. P1 and AH Plus Jet had superior radiopacity (p < 0.05). Bio-C Sealer and AH Plus Bioceramic showed higher volume alteration than P2 (p0.05). CONCLUSIONS: Variations in the proportions of tricalcium silicate and radiopacifiers significantly influenced the sealers' properties. P1 (30% calcium silicate/65% radiopacifier) demonstrated superior radiopacity and flowability, while P3 (50% calcium silicate/45% radiopacifier) was the only calcium silicate-based sealer complying with ISO solubility standards. CLINICAL RELEVANCE: Variations in the proportions of calcium silicate and radiopacifiers significantly influenced the sealers' properties. The calcium silicate-based endodontic sealer with 50% calcium silicate and 45% radiopacifier demonstrated ISO-compliant solubility while maintaining optimal physicochemical balance. calcium silicate dental materials physicochemical analysis root canal obturation Figures Figure 1 INTRODUCTION The complete filling of the root canal system remains a major challenge in endodontics. Although various materials and techniques have been proposed, none have achieved this goal [ 1 ]. In the field of endodontic filling materials, calcium silicate sealers have gained considerable prominence due to their positive influence on the repair of periapical tissues, being recognized as bioactive materials [ 2 , 3 ]. The bioactivity is primarily attributed to their ability to release ions, particularly calcium and hydroxyl ions [ 4 – 6 ]. Calcium silicate-based sealers or hydraulic sealers are well recognized for their ability to induce periapical repair [ 7 , 8 ]. These materials offer long-lasting marginal sealing, high radiopacity, low setting expansion, significant ion-releasing capacity, and adequate working time for endodontic procedures [ 9 – 11 ]. Their biological properties are due to the formation of calcium hydroxide during the setting reaction and its subsequent dissociation [ 12 ]. However, these endodontic sealers have certain limitations, particularly regarding their manipulation and insertion into the root canal system, which stem from their grainy texture [ 1 ]. To overcome these drawbacks, incorporating propylene glycol and barium sulfate can improve plasticity, thereby enhancing its performance as a sealing material. These modifications can occur in the liquid (originally distilled water) and the powder, which initially consisted solely of Portland cement and bismuth oxide [ 1 , 13 ]. Another disadvantage of early calcium silicate-based sealers was the discoloration of the tooth structure. Collagen in the dentin matrix reacts with bismuth oxide, resulting in a grayish discoloration [ 14 ]. To address this issue, alternative radiopacifiers, such as tantalum oxide and zirconium oxide, have been suggested for use in endodontic cement. Studies have reported favorable results regarding tooth color stability when these radiopacifiers are used [ 15 , 16 ]. The AH Plus Bioceramic (Dentsply De Trey, Konstanz, Germany) is a premixed tricalcium silicate cement-based sealer that demonstrates adequate properties to be considered a good sealer but still has high solubility [ 17 ]. To date, the volumetric change of AH Plus Bioceramic has not been evaluated. Manufactured by the same company, AH Plus Jet (Dentsply De Trey, Konstanz, Germany) is an epoxy resin-based endodontic sealer marketed in a dual-syringe auto-mix system. It is commonly used as a benchmark for evaluating new sealers due to its excellent physical properties (such as dimensional stability, sealing ability, and flow) and its favorable chemical and biological characteristics, making it the gold standard in clinical practice [ 18 ]. Bio-C Sealer (Angelus, Londrina, Brazil) is a premixed hydraulic sealer specifically developed for root canal obturation. This ready-to-use material, supplied in a single syringe, contains calcium silicates, calcium aluminate, calcium oxide, zirconium oxide, iron oxide, silicon dioxide, and dispersing agents. Recent studies have demonstrated its superior cytocompatibility compared to AH Plus, showing enhanced cell viability, migration, morphology, adhesion, and mineralization capacity [ 19 ]. While exhibiting favorable physicochemical properties, including a short setting time, alkalinizing ability, adequate flow, satisfactory radiopacity, and minimal volumetric change, the sealer shows higher solubility than permitted by ISO 6876 standards [ 20 ]. Variations in the type and proportion of radiopacifiers can affect the physical and chemical properties of sealers [ 21 ]. Also, changes in the calcium content can contribute to the formation of calcium carbonates, which are essential for the bioactivity and biocompatibility of these materials [ 1 , 19 , 22 ]. Therefore, determining the optimal ratio of components in hydraulic endodontic sealer is crucial. This study evaluated the physical and chemical properties of calcium silicate-based sealers with varying proportions of calcium silicate and radiopacifiers (P1-P3), including setting time, radiopacity, flowability, solubility, volumetric change, and pH. They were compared with two commercially available sealers: AH Plus Jet and AH Plus Bioceramic. The null hypothesis was that there are no significant differences in the physicochemical properties between the P1, P2, and P3, and the commercial sealers AH Plus Jet and AH Plus Bioceramic, and that the different proportions of calcium silicate and radiopacifiers do not significantly affect these physicochemical properties. MATERIAL AND METHODS The present study evaluated the physicochemical properties of calcium silicate-based sealers with varying proportions of calcium silicate and radiopacifiers (P1-P3). The composition of the tested sealers is detailed in Table 1 . They were mixed to a consistency of obturation endodontic sealer, with a powder-to-liquid ratio of 2:1. AH Plus Bioceramic and Bio-C Sealaer were handled according to the manufacturer’s instructions. In contrast, AH Plus Jet was manually mixed by blending equal lengths (1 cm) of pastes A and B with a metal spatula on a mixing pad for 30 seconds, until a homogeneous consistency was achieved [ 23 ]. Table 1 The manufacturer and composition of the tested sealers. Sealers and Manufactures Composition Proportion 1 (P1- Bauru School of Dentistry, University of São Paulo, Bauru, Brazil) Powder: 30% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 40% Tantalum oxide, 25% Zirconium oxide. Liquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate Proportion 2 (P2- Bauru School of Dentistry, University of São Paulo, Bauru, Brazil) Powder: 40% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 35% Tantalum oxide, 20% Zirconium oxide. Liquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate Proportion 3 (P3- Bauru School of Dentistry, University of São Paulo, Bauru, Brazil) Powder: 50% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 30% Tantalum oxide, 15% Zirconium oxide Liquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate AH Plus Bioceramic (Dentsply De Trey, Konstanz, Germany) Zirconium dioxide (50–75%), Tricalcium silicate (5–15%), Dimethyl sulfoxide (10–30%), Lithium carbonate (< 0.5%), Thickening agent (< 6%) AH Plus Jet (Dentsply De Trey, Konstanz, Germany) Paste A: Bisphenol-A epoxy resin, Bisphenol-F epoxy resin, Calcium tungstate, Zirconium oxide, Silica, Iron oxide pigments. Paste B: Dibenzyldiamine, Aminoadamantane, Tricyclodecane-diamine, Calcium tungstate, Zirconium oxide, Silica, Silicone oil. Bio-C Sealer (Angelus, Londrina, Brazil) Calcium silicate, calcium aluminate, calcium oxide, zirconium oxide, iron oxide, silicon dioxide and dispersing agent Setting Time Initial and final setting times were determined according to ASTM C 266–2008 [ 24 ]. The experiment was conducted under controlled conditions of temperature (37°C ± 1°C) and humidity (95% ± 5%). Fifteen type IV gypsum rings, with an inner diameter of 10 mm and a thickness of 2.0 mm, were used to prepare the specimens (n = 3). The cements were placed in the rings that had been pre-soaked in distilled water. After 180 ± 5 seconds of mixing, the specimens were tested for setting by applying vertical pressure using a Gilmore needle, first with a 113.5 g needle for the initial setting and then with a 456.5 g needle for the final setting. The time elapsed from insertion into the gypsum rings to when no indentation was visible from either needle on the specimen surface was recorded. Flowability The flowability test was performed according to ISO 6876/2012 [ 25 ]. After mixing, 0.05 ± 0.005 mL of each cement was dispensed onto a glass plate using a disposable syringe. After 180 ± 5 seconds, a second glass plate (20 mm) was placed on top of the cement drop, followed by a 100 g weight, totaling 120 ± 2 g. After 10 minutes, the weight was removed, and the largest and smallest diameters of the cement were measured using a digital caliper (0.001 mm). The difference between the largest and smallest diameters was not greater than 1.0 mm. All groups were tested in triplicate (n = 3). Radiopacity Radiopacity was assessed according to ISO 6876/2012 [ 25 ]. Fifteen specimens, 10.0 mm in diameter and 1.0 mm in height, were prepared using metal rings (n = 3). After preparation, the specimens were placed on occlusal radiographic films, each film receiving one specimen from each experimental group, along with a 1.0 mm control and an aluminum step wedge (scale 1–10 mm of Al). The films were X-ray sensitized using an X-ray machine operating at 70 kV, 10 mA, with exposure times of 0.3 seconds and a focus/film distance of 30 cm. Radiopacity quantification was performed through densitometric analysis using Adobe Photoshop CC 2017 software (Adobe Systems, USA), employing the formula proposed by Duarte et al. [ 26 ]: RD = [A × 2/B] + mm Al (immediately lower step), where 'A' is the difference between the radiographic density of the material (RDm) and that of the immediately lower aluminum step; 'B' is the difference between adjacent aluminum steps; and '2' is the standard increment between the steps of the penetrometer. The results were expressed in millimeters of aluminum (mm Al). Solubility Solubility was tested according to ISO 6876:2012 [ 25 ]. The solubility test was performed using metal rings for the AH Plus Jet and gypsum rings for the calcium silicate-based sealers (P1, P2, P3 and AH Plus Bioceramic) with an internal diameter of 20 mm and a thickness of 1.5 mm, placed on a glass plate covered with cellophane paper and filled with the endodontic cement. A waterproof nylon thread was inserted into the material, followed by the placement of another glass plate, also covered with cellophane paper. The assembly was manually pressed to ensure that the plates made uniform contact with the mold. The samples were kept in an oven at 37°C ± 1°C and 95% ± 5% relative humidity for a period equivalent to three times the setting time of the tested material. After removing residues and loose particles, the samples were weighed on a precision analytical balance. They were then suspended by the nylon thread and placed in plastic containers containing 7.5 mL of distilled and deionized water, ensuring they did not touch the container walls and remained fully submerged. The samples were maintained under these conditions in an oven at 37°C ± 1°C and 95% ± 5% relative humidity for 7 days. After this period, they were removed from the containers, rinsed with distilled and deionized water, and excess water was removed with absorbent paper. Subsequently, they were kept in a desiccator for 24 hours and weighed again. Solubility was determined by calculating the mass loss of each sample relative to its initial mass. Volumetric Change Analysis To analyze volumetric change, artificial teeth (IM do Brasil, São Paulo, Brazil) with 21 mm long circular canals were prepared using Genius Proflex rotary instruments (Medidenta, Las Vegas, NV, USA) up to a #40/.04 file with a working length 1.0 mm short of the foraminal opening. Before obturation, the apical patency was confirmed using K-type #20 instruments (Dentsply-Maillefer, Konstanz, Germany). After biomechanical preparation, the teeth were obturated using the single-cone technique with size 40.04 taper cones (Tanari, Tanariman, Manacapuru, AM, Brazil). Immediately following obturation, the specimens were scanned using micro-CT and then placed in acrylic pots containing 10 mL of phosphate-buffered saline (PBS), with only the root portion in contact with the liquid. The specimens were maintained in an incubator at 37°C and 95% humidity for 7 days. Pre- and post-scans were obtained using a micro-CT system (1174v2 SkyScan; Bruker-microCT, Kontich, Belgium) operating at 50 kV, 800 mA, with 360-degree rotation, and an isotropic resolution of 23.97 µm. The system includes a high-resolution camera (1304 × 1024 pixels). The images of each sample were reconstructed using specialized software (NRecon v.1.6.3; Bruker-microCT), generating transverse and axial slices of the samples’ structure. The surface segmentation and modeling were performed using the automatic CTAN v.1.12 software (Bruker-microCT) from the pre-scan images. For volumetric assessment of the material pre- and post-volume, the CTAN software (Bruker-microCT) was employed. The volume of material (mm³) was calculated for the apical 10 mm of each sample. Volumetric change was expressed as a percentage, calculated as the difference between the initial and final volumes. Negative values indicate volume expansion of the material [ 27 ]. pH The same acrylic teeth, prepared and obturated as described for the volumetric analysis, were used for pH determination. After obturation, the apices of the teeth were immediately immersed in acrylic pots containing 10 ml of phosphate-buffered saline and placed in an incubator at 37°C and 95% humidity for the experiment. All pots were pre-treated with nitric acid to prevent any interference with the results. pH measurements were conducted at 3, 24, 72, and 168 hours using a calibrated pH meter [ 2 ]. Statistical Analysis The data were subjected to normality analysis using the Kolmogorov-Smirnov test, which indicated a normal distribution. For global comparison, ANOVA was applied, and individual comparisons were performed using the Tukey test. The statistical software used was GraphPad Prism 9.0 (GraphPad Software Inc, San Diego, CA). A significance level of 5% was adopted. RESULTS Table 2 presents the mean and standard deviation for the initial and final setting times, flowability, radiopacity, solubility, and volumetric change. Statistically significant differences (p 0.05). The radiopacity results showed that P1 and AH Plus Jet demonstrated the highest radiopacity values, with no statistically significant difference between them (p > 0.05). Bio-C Sealer presented the lowest radiopacity value (p < 0.05). Significant differences were found between P1 and both P3 and AH Plus Bioceramic, between P2 and AH Plus Bioceramic, and between AH Plus Jet and P2, P3, and AH Plus Bioceramic (p < 0.05). The calcium silicate-based sealer (P1, P2, P3, Bio-C Sealer and AH Plus Bioceramic) exhibited higher solubility than AH Plus Jet (p 0.05). Regarding volumetric change, Bio-C Sealer and AH Plus Bioceramic showed significantly higher volume alteration than P2 (p 0.05) – Fig. 1 . Table 2 Mean and standard deviation of initial and final setting time (in minutes), flowability (mm), radiopacity (mmAl), solubility (%), and volumetric change (%) of the P1, P2, P3, AH Plus Jet, Bio-C Sealer, and AH Plus Bioceramic. Setting time (min) Sealers Initial Final Flowability (mm) Radiopacity (mm Al) Volumetric Change (%) Solubility (%) P1 124.0 ± 1.0 a 407 ± 1.0 a 20.69 ± 0.01 a 9.63 ± 1.39 ac 2.07 ± 2.14ª b 5.82+/-0.26 ab P2 155.0 ± 1.0 b 426 ± 1.0 b 19.70 ± 0.01 ab 9.22 ± 1.25 a 0.18 ± 3.10ª 4.68+/-2.49 ab P3 178.0 ± 1.0 c 625 ± 1.0 c 19.19 ± 0.01 b 6.93 ± 2.13 bd 3.35 ± 5.22ª b 2.68+/-1.57 a AH Plus Jet 847.3 ± 4.93 d 1725 ± 1.0 d 25.47 ± 0.01 c 11.73 ± 0.98 c 1.65 ± 1.47ª b 0.05+/-0.05 c Bio C Sealer 237.7 ± 6.42 e 446.7 ± 4.04 e 26.9 ± 0.99 d 6.30 ± 0.20 d 5.49 ± 4.24 b 8.10+/-2.15 b AH Plus Bioc 115.0+/-3.0 a 265+/1.0 f 30.38+/-0.01 e 6.58+/-0.59 b 4.54 ± 2.02 b 4.49+/-1.51 ab Different superscript lowercase letters represent statistically significance differences (p < 0.05) in the same column. Table 3 presents the mean and standard deviation of pH test results. In the intra-group evaluation, P1, P2, and P3 exhibited an increase in pH between 24 and 72 hours (p < 0.05). AH Plus Jet presented a significant pH increase between 3 and 24 hours (p 0.05). AH Plus Bioceramic showed significant pH increases between 3 and 168 hours, 24 and 72 hours, 72 and 168 hours (p < 0.05). At 3 hours, the pH of AH Plus Jet and Bioceramic was higher than that of P1, P2, and P3 (p 0.05). At 72 hours, the pH of P1, P2, P3, and AH Plus Bioceramic was higher than that of AH Plus Jet (p 0.05), while AH Plus Bioceramic showed the highest pH (p < 0.05). Bio-C Sealer presented the highest pH values, with statistically significant differences between experimental time points (p 0.05). Table 3 Mean and standard deviation of pH of the P1, P2, P3, AH Plus Jet, Bio-C Sealer, and AH Plus Bioceramic. pH Sealers 3h 24h 72h 168h ES1 6.86 ± 0.008 ABab 6.86 ± 0.007 Aa 6.88 ± 0.019 Bab 6.87 ± 0.015 ABa ES2 6.87 ± 0.011 ABabc 6.87 ± 0.003 ACac 6.88 ± 0.008 Bab 6.88 ± 0.010 ABac ES3 6.86 ± 0.005 Aa 6.86 ± 0.006 ACac 6.88 ± 0.015 Aa 6.88 ± 0.043 Aac AH Plus Jet 6.88 ± 0.005 Aac 6.87 ± 0.011 Aac 6.86 ± 0.007 Ab 6.87 ± 0.027 Aac Bio C Sealer 7.15 ± 0.012 Aa 7.00 ± 0.011 Bbd 7.25 ± 0.008 Cc 7.04 ± 0.050 Bb AH Plus Bioceramic 6,884+/-0,006 Ac 6,859+/-0,013 Ba 6,882+/-0,009 Aab 6,910+/-0,009 Cc Control 6.87 ± 0.013 Aac 6.87 ± 0.013 Ac 6.87 ± 0.013 Aab 6.87 ± 0.013 Aac Different superscript lower-case letters represent statistically significance differences (P < .05) between periods studied in the same group. Different superscript upper-case letters represent statistically significance differences (p < 0.05) in the same column. DISCUSSION Developing new endodontic sealers with optimized physicochemical and biological properties is crucial for endodontic treatment. Ready-to-use calcium silicate sealers have been introduced to the market, featuring variations in powder composition and vehicles. However, these materials often exhibit high solubility, with values frequently exceeding the limits of ISO standards [ 17 , 20 , 28 ]. Thus, the present study aimed to analyze three formulations with different calcium silicate/radiopacifiers proportions and compare them to the epoxy resin sealer AH Plus Jet and two ready-to-use commercial calcium silicate sealers, AH Plus Bioceramic and Bio-C Sealer. The results of our study indicate that the lower calcium silicate content led to a faster setting, as well as higher flowability and radiopacity. P1 exhibited an initial setting time similar to AH Plus Bioceramic, although its final setting time was slightly longer. This suggests that AH Plus Bioceramic may contain components that accelerate setting more effectively. Notably, lithium carbonate, present in small concentrations in its composition, can modulate the setting reaction. This compound is commonly used in cement mixtures for tiling to accelerate the setting time [ 29 , 30 ]. AH Plus Bioceramic exhibited shorter setting times than AH Plus Jet, consistent with findings from a previous study [ 17 ]. All sealers evaluated exhibited radiopacity greater than 3 mm of Al. AH Plus Jet, which contains zirconium oxide and calcium tungstate in its composition as radiopacifiers, showed the highest value. A recent study [ 31 ] reported that the use of tantalum and zirconium oxide as radiopacifiers appears to be systemically safe. These findings support the clinical safety of these radiopacifiers in endodontic sealers, so they were selected for the different proportions (P1, P2 e P3). The results of our study are consistent with those found by Kandemir Demirci et al. [ 32 ], who reported similar radiopacity values for AH Plus Jet. The formulations P1, P2, and P3, which combined zirconium oxide with tantalum oxide, demonstrated greater radiopacity than AH Plus Bioceramic, with P1 achieving values comparable to those of AH Plus Jet. This is in line with the fact that using 30% zirconium oxide can yield values near 3 mm Al, as reported by Duarte et al. [ 26 ]. Increased radiopacity enhances the material’s contrast with mineralized structures such as dentin, cementum, and bone, facilitating its visibility in radiographs. The lower proportions of calcium silicate and higher concentrations of radiopacifiers exhibited lower flowability. This could be due to the higher density of radiopacifiers, which might increase the viscosity of the material, making it less fluid. Additionally, the reduced proportion of calcium silicate may result in a thicker, less flowable mixture, potentially due to a decrease in the formation of hydrated compounds. These factors may collectively contribute to the observed reduction in flowability. The flowability of AH Plus Jet was similar to that observed in a previous study [ 28 ]. In our study, the AH Plus Bioceramic showed the highest flowability. While higher flowability may improve sealer penetration in complex anatomical areas and dentinal tubules, it could also lead to greater risk of extrusion, which can be associated with postoperative pain [ 34 ]. ISO standards set limits for the solubility of endodontic sealers to ensure their long-term effectiveness and safety. According to ISO 6876:2012, the maximum allowable solubility is 3% [ 25 ]. The results of the present study show solubility values within ISO standards only for the AH Plus Jet and P3. Interestingly, Bio-C Sealer, which exhibited the highest solubility and volumetric change among hydraulic sealers, also produced the highest pH values. This correlation may be explained by its greater ion release capacity, particularly calcium and hydroxyl ions, which is directly associated with the bioactivity of hydraulic cements [ 2 – 4 , 11 , 29 ]. While the solubility of calcium silicate-based sealers may be considered a disadvantage in terms of dimensional stability, it is precisely this characteristic that contributes to their reparative biological potential through enhanced bioactivity [ 1 , 12 ]. The solubility of tricalcium silicate sealers varies in the literature, possibly related to differences in protocols and methodologies used [ 1 , 11 , 29 ]. Ideally, endodontic sealers should exhibit minimal volumetric alteration after setting to prevent compromising the quality of the root canal filling [ 1 , 9 , 10 ]. The in vitro methods proposed by the ADA [ 34 ] and ISO [ 25 ] to assess solubility and dimensional stability do not fully replicate the clinical situation; therefore, our study employed a methodology previously reported in the literature, where only the radicular portion of the teeth remains in contact with the medium and is maintained in a controlled temperature and humidity environment [ 27 ]. Although natural teeth were not used in our study, a prior study demonstrated that artificial teeth can be considered a viable option for evaluating obturation quality using the single-cone technique with calcium silicate-based sealers [ 35 ]. To minimize the risk of bias, the single-cone technique was adopted, and all obturations were performed by a single experienced operator. Additionally, PBS solution was used as the storage medium, as previous research has shown that storage in PBS significantly reduces the volumetric change of calcium silicate-based sealers [ 28 ]. Our results indicate that the experimental sealers and AH Plus Jet exhibited lower volumetric changes compared to AH Plus Bioceramic and Bio-C Sealer. No studies have published data on the volumetric change of AH Plus Bioceramic; however, previous studies have reported similar volumetric changes for resin-based and calcium silicate-based sealers [ 20 , 33 ]. One of the main characteristics of calcium silicate-based sealers is the formation of calcium hydroxide during hydration, which leads to the alkalinization of the environment [ 4 ]. Although previous studies have shown that calcium silicate-based sealers can alkalinize the surrounding environment [ 2 , 4 , 27 ], our results revealed that none of the tested sealers could alkalinize the solution. This may be related to differences in the methodologies used to assess pH. The methodology employed in our study aimed to replicate clinical practice, where the sealers are placed within the root canal system, with no direct contact between the material and the extra-radicular environment. The null hypotheses were rejected, as significant differences (p < 0.05) were observed in several physicochemical properties, including setting times, flowability, radiopacity, solubility, and volumetric change, between the P1, P2, P3, and the commercial sealers (AH Plus Jet and AH Plus Bioceramic). The different proportions exhibited higher solubility and lower volumetric change compared to AH Plus Bioceramic, while radiopacity varied significantly among groups. Additionally, the different proportions of calcium silicate and radiopacifiers in the experimental sealers significantly influenced some properties, such as flowability and setting times, but not others, such as volumetric change among the experimental groups. The pH variations also showed significant differences at specific time points, further supporting the rejection of the null hypotheses. These findings indicate that the composition of sealers, particularly the proportions of calcium silicate and radiopacifiers, plays a critical role in determining their physicochemical properties. Physical and chemical studies are crucial and should be conducted before the biological testing of endodontic sealers, as they provide essential data on the material's properties. In our study, the P1 exhibited high radiopacity, high flow, low volumetric change, and a favorable setting time, while P3 was the only hydraulic sealer with solubility values within ISO [ 25 ] and ADA [ 34 ] limits. This suggests that the 50% calcium silicate/45% radiopacifier formulation may represent an optimal balance for clinical applications. The solubility of P1, P2, and AH Plus Bioceramic remained a drawback, indicating that compositional adjustments may be necessary for these formulations. Further biological and clinical studies are required to comprehensively evaluate these sealers, alongside additional tests such as bond strength (adhesion), push-out resistance, dentin-sealer interface analysis, and failure mode assessment. CONCLUSION Formulation P1 (30% calcium silicate / 65% radiopacifier) demonstrated high radiopacity, favorable flowability, and low volumetric change, comparable to AH Plus Jet. Notably, formulation P3 (50% calcium silicate / 45% radiopacifier) was the only hydraulic sealer with solubility values within ISO standards, whereas P1, P2, and the commercial calcium silicate-based sealers exhibited higher solubility than AH Plus Jet. Although compositional differences affected setting time and flowability, volumetric changes remained minimal for P1, P2, P3, and AH Plus Jet. Declarations Acknowledgements The authors deny any conflicts of interest related to this study. The first author would like to thank São Paulo Research Foundation (FAPESP- Process number: 2024/01063-0) for providing financial support. Author contributions: M.A.H.D., G.F.S., and R.S.O.N. contributed to the conceptualization. R.S.O.N., M.P.A., S.J.R. and M.A.H.D. contributed to the methodology. R.S.O.N., M.P.A., T.C.M.V., S.J.R., B.S.W. and M. A. H. D. contributed to the investigation. M.P.A., R. R. V., G.F.S., and M. A. H. D. contributed to the formal analysis. M.A.H.D., M.P.A., and R.S.O.N. contributed to data curation. R.S.O.N., G.F.S. and T.C.M.V. wrote and prepared the original draft. B.S.W., R.S.O.N. and M. A. H. D. contributed to the review and editing of the study report. M.A.H.D. contributed to supervision. M.P.A., R.R.V., G.F.S. and M.A.H.D. contributed to project administration. M.A.H.D. and R.S.O.N. contributed to funding acquisition. Conflict of Interest: The authors declare that they have no conflict of interest. Funding: Funding: This work was supported by São Paulo Research Foundation (FAPESP - Process number 2024/01063-0). Ethical approval: No ethical approval was required for this type of laboratory study Informed consent: No formal consent was required for this type of laboratory study. References Camilleri J, Atmeh A, Li X, Meschi N. Present status and future directions: Hydraulic materials for endodontic use. Int Endod J. 2022 May;55 Suppl 3(Suppl 3):710-777. doi: 10.1111/iej.13709. Epub 2022 Mar 17. Erratum in: Int Endod J. 2023 Mar;56(3):402. doi: 10.1111/iej.13881. Duarte MA, Demarchi AC, Yamashita JC, Kuga MC, Fraga Sde C. pH and calcium ion release of 2 root-end filling materials. Oral Surg Oral Med Oral Pathol Oral Radiol Endod. 2003 Mar;95(3):345-7. doi: 10.1067/moe.2003.12. Niu LN, Jiao K, Wang TD, Zhang W, Camilleri J, Bergeron BE, Feng HL, Mao J, Chen JH, Pashley DH, Tay FR. 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Clin Oral Investig. 2024 Jul 6;28(8):416. doi: 10.1007/s00784-024-05812-1. Torabinejad M, Pitt Ford TR, McKendry DJ, Abedi HR, Miller DA, Kariyawasam SP. Histologic assessment of mineral trioxide aggregate as a root-end filling in monkeys. J Endod. 1997 Apr;23(4):225-8. doi: 10.1016/S0099-2399(97)80051-9. Economides N, Pantelidou O, Kokkas A, Tziafas D. Short-term periradicular tissue response to mineral trioxide aggregate (MTA) as root-end filling material. Int Endod J. 2003 Jan;36(1):44-8. doi: 10.1046/j.0143-2885.2003.00611.x. Torabinejad M, Watson TF, Pitt Ford TR. Sealing ability of a mineral trioxide aggregate when used as a root end filling material. J Endod. 1993 Dec;19(12):591-5. doi: 10.1016/S0099-2399(06)80271-2. Camilleri J, Gandolfi MG, Siboni F, Prati C. Dynamic sealing ability of MTA root canal sealer. Int Endod J. 2011 Jan;44(1):9-20. doi: 10.1111/j.1365-2591.2010.01774.x. Khalil I, Naaman A, Camilleri J. Properties of Tricalcium Silicate Sealers. J Endod. 2016 Oct;42(10):1529-35. doi: 10.1016/j.joen.2016.06.002. Holland R, de Souza V, Nery MJ, Faraco Júnior IM, Bernabé PF, Otoboni Filho JA, Dezan Júnior E. Reaction of rat connective tissue to implanted dentin tube filled with mineral trioxide aggregate, Portland cement or calcium hydroxide. Braz Dent J. 2001;12(1):3-8. Torabinejad M, Hong CU, McDonald F, Pitt Ford TR. Physical and chemical properties of a new root-end filling material. J Endod. 1995 Jul;21(7):349-53. doi: 10.1016/S0099-2399(06)80967-2. Marciano MA, Costa RM, Camilleri J, Mondelli RF, Guimarães BM, Duarte MA. Assessment of color stability of white mineral trioxide aggregate angelus and bismuth oxide in contact with tooth structure. J Endod. 2014 Aug;40(8):1235-40. doi: 10.1016/j.joen.2014.01.044. Aguiar BA, Frota LMA, Taguatinga DT, Vivan RR, Camilleri J, Duarte MAH, de Vasconcelos BC. Influence of ultrasonic agitation on bond strength, marginal adaptation, and tooth discoloration provided by three coronary barrier endodontic materials. Clin Oral Investig. 2019 Nov;23(11):4113-4122. doi: 10.1007/s00784-019-02850-y. Lin HN, Wang LC, Chen MS, Chang PJ, Lin PY, Fang A, Chen CY, Lee PY, Lin CK. Discoloration Improvement by Mechanically-Milled Binary Oxides as Radiopacifier for Mineral Trioxide Aggregates. Materials (Basel). 2022 Nov 10;15(22):7934. doi: 10.3390/ma15227934. Souza LC, Neves GST, Kirkpatrick T, Letra A, Silva R. Physicochemical and Biological Properties of AH Plus Bioceramic. J Endod. 2023 Jan;49(1):69-76. doi: 10.1016/j.joen.2022.10.009. Silva EJNL, Ferreira CM, Pinto KP, Barbosa AFA, Colaço MV, Sassone LM. Influence of variations in the environmental pH on the solubility and water sorption of a calcium silicate-based root canal sealer. Int Endod J. 2021 Aug;54(8):1394-1402. doi: 10.1111/iej.13526. López-García S, Pecci-Lloret MR, Guerrero-Gironés J, Pecci-Lloret MP, Lozano A, Llena C, Rodríguez-Lozano FJ, Forner L. Comparative Cytocompatibility and Mineralization Potential of Bio-C Sealer and TotalFill BC Sealer. Materials (Basel). 2019 Sep 22;12(19):3087. doi: 10.3390/ma12193087. Zordan-Bronzel CL, Esteves Torres FF, Tanomaru-Filho M, Chávez-Andrade GM, Bosso-Martelo R, Guerreiro-Tanomaru JM. Evaluation of Physicochemical Properties of a New Calcium Silicate-based Sealer, Bio-C Sealer. J Endod. 2019 Oct;45(10):1248-1252. doi: 10.1016/j.joen.2019.07.006. Marciano MA, Duarte MA, Camilleri J. Calcium silicate-based sealers: Assessment of physicochemical properties, porosity and hydration. Dent Mater. 2016 Feb;32(2):e30-40. doi: 10.1016/j.dental.2015.11.008. Gandolfi MG, Taddei P, Modena E, Siboni F, Prati C. Biointeractivity-related versus chemi/physisorption-related apatite precursor-forming ability of current root end filling materials. J Biomed Mater Res B Appl Biomater. 2013 Oct;101(7):1107-23. doi: 10.1002/jbm.b.32920. Rosa SJ, Duarte MAH, Silva EJNL, Oliveira MCG, Titato PCG, Vasconcelos BC, Vivan RR, Alcalde MP. Does the Mixing Method of AH Plus Jet Affect its Physicochemical and Mechanical Properties? J Endod. 2024 Sep;50(9):1333-1339. doi: 10.1016/j.joen.2024.06.006. ASTM C266-08: Standard Test Method for Time of Setting of Hydraulic-Cement Paste by Gillmore Needles. West Conshohocken, PA: ASTM International, 2008. International Organization for Standardization. ISO 6876: Dental Root Canal Sealing Materials. Geneva, Switzerland: International Organization for Standardization; 2012. Húngaro Duarte MA, de Oliveira El Kadre GD, Vivan RR, Guerreiro Tanomaru JM, Tanomaru Filho M, de Moraes IG. Radiopacity of portland cement associated with different radiopacifying agents. J Endod. 2009 May;35(5):737-40. doi: 10.1016/j.joen.2009.02.006. Cavenago BC, Pereira TC, Duarte MA, Ordinola-Zapata R, Marciano MA, Bramante CM, Bernardineli N. Influence of powder-to-water ratio on radiopacity, setting time, pH, calcium ion release and a micro-CT volumetric solubility of white mineral trioxide aggregate. Int Endod J. 2014 Feb;47(2):120-6. doi: 10.1111/iej.12120. Torres FFE, Zordan-Bronzel CL, Guerreiro-Tanomaru JM, Chávez-Andrade GM, Pinto JC, Tanomaru-Filho M. Effect of immersion in distilled water or phosphate-buffered saline on the solubility, volumetric change and presence of voids within new calcium silicate-based root canal sealers. Int Endod J. 2020 Mar;53(3):385-391. doi: 10.1111/iej.13225. Cardinali F, Camilleri J. A critical review of the material properties guiding the clinician's choice of root canal sealers. Clin Oral Investig. 2023 Aug;27(8):4147-4155. doi: 10.1007/s00784-023-05140-w. Zhang Y, Wang Y, Li T, Xiong Z, Sun Y. Effects of lithium carbonate on performances of sulphoaluminate cement-based dual liquid high water material and its mechanisms. Construction and Building Materials. 2018;161:374-80. doi: 10.1016/j.conbuildmat.2017.11.130. Janini ACP, Moraes BF, Pelepenko LE, Dos Santos VAB, Barros-Costa M, Malosá GF, Batista FRS, Meira JAS, Matsumoto MA, Antunes TBM, Darin Filho G, Haiter Neto F, Gomes BPFA, Marciano MA. Physicochemical properties and biological interaction of calcium silicate-based sealers - in vivo model. Clin Oral Investig. 2025 Jan 25;29(1):86. doi: 10.1007/s00784-025-06150-6. Kandemir Demirci G, Çöven FO, Güneri P, Karavana SY, Nalbantsoy A, Köse T, Kaval ME. The solubility, pH value, chemical structure, radiopacity, and cytotoxicity of four different root canal sealers: an in vitro study. Clin Oral Investig. 2023 Sep;27(9):5413-5425. doi: 10.1007/s00784-023-05160-6. Drumond JPSC, Maeda W, Nascimento WM, Campos DL, Prado MC, de-Jesus-Soares A, Frozoni M. Comparison of Postobturation Pain Experience after Apical Extrusion of Calcium Silicate- and Resin-Based Root Canal Sealers. J Endod. 2021 Aug;47(8):1278-1284. doi: 10.1016/j.joen.2021.05.008. American National Standards/American Dental Association. Specification no. 57 for Endodontic Sealing Materials. Chicago, IL, USA: American National Standards/American Dental Association; 2000. Kooanantkul C, Shelton RM, Camilleri J. Comparison of obturation quality in natural and replica teeth root-filled using different sealers and techniques. Clin Oral Investig. 2023 May;27(5):2407-2417. doi: 10.1007/s00784-023-04884-9. Additional Declarations No competing interests reported. Cite Share Download PDF Status: Posted Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. 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Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-6908130","acceptedTermsAndConditions":true,"allowDirectSubmit":true,"archivedVersions":[],"articleType":"Research Article","associatedPublications":[],"authors":[{"id":473631053,"identity":"77287d39-e4f5-4e92-b937-e02eaedd0c26","order_by":0,"name":"Raimundo Sales Oliveira Neto","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA+0lEQVRIiWNgGAWjYFCCBDBiYDgA5tkkQAQLiNVygCEtgYENJGhAQAsDQsthiBYGPFr423MffniYcziP73jvwccfKs7n8ct3J354YMAgzy92AKsWiTPPjSUStx0uljxzLtngwJnbxZJtvJslgA4znDk7AasWA4k0BpCWxA03cswkDrbdTtxwjHcDSEuCwW2cWph/QLWY/zjYdg6kZfMPAlrY4LYwHGw7ANKyDa8tEmeesVkkbktPnHnmjLHEmTPJiTPbcrdZJBhI4PQLf3sa882f26wT+473GH6oqLBL7Gc+u/nmjwobeX5p7FpwAgnSlI+CUTAKRsEoQAEAzKNplUw3bMsAAAAASUVORK5CYII=","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":true,"prefix":"","firstName":"Raimundo","middleName":"Sales Oliveira","lastName":"Neto","suffix":""},{"id":473631054,"identity":"2397855d-e034-4748-9f51-cd45be06b6d6","order_by":1,"name":"Guilherme Ferreira Silva","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Guilherme","middleName":"Ferreira","lastName":"Silva","suffix":""},{"id":473631055,"identity":"89dbaecd-8823-4fdf-9d42-305b77a9d03b","order_by":2,"name":"Tany Carvalho Moreira Veiga","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Tany","middleName":"Carvalho Moreira","lastName":"Veiga","suffix":""},{"id":473631056,"identity":"18122b71-48b5-4c54-b5ed-2e6f42ad99c9","order_by":3,"name":"Stefani Jovedi Rosa","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Stefani","middleName":"Jovedi","lastName":"Rosa","suffix":""},{"id":473631057,"identity":"462e146e-79e1-4bae-ae5c-8927c5c5ef97","order_by":4,"name":"Brenda Stefhany Wilchenski","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Brenda","middleName":"Stefhany","lastName":"Wilchenski","suffix":""},{"id":473631058,"identity":"5426d800-b95e-4be5-8b98-b57321cda3b0","order_by":5,"name":"Rodrigo Ricci Vivan","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Rodrigo","middleName":"Ricci","lastName":"Vivan","suffix":""},{"id":473631059,"identity":"ff8bfe45-1b0e-4ba9-b9df-fa4da8953de4","order_by":6,"name":"Murilo Priori Alcalde","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Murilo","middleName":"Priori","lastName":"Alcalde","suffix":""},{"id":473631060,"identity":"45405bff-a9e7-47d4-950e-2769dc76efc5","order_by":7,"name":"Marco Antonio Hungaro Duarte","email":"","orcid":"","institution":"University of São Paulo – USP","correspondingAuthor":false,"prefix":"","firstName":"Marco","middleName":"Antonio Hungaro","lastName":"Duarte","suffix":""}],"badges":[],"createdAt":"2025-06-16 19:08:05","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-6908130/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-6908130/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":85301142,"identity":"1cc7bd70-2279-4501-8f9f-0211aa981683","added_by":"auto","created_at":"2025-06-24 12:01:26","extension":"png","order_by":1,"title":"Figure 1","display":"","copyAsset":false,"role":"figure","size":195554,"visible":true,"origin":"","legend":"\u003cp\u003eRepresentative micro-CT three-dimensional reconstructions of the evaluated root canal sealers: A – Proportion 1, B – Proportion 2, C – \u0026nbsp;Proportion 3, D – Bio-C Sealer, E – AH Plus Jet, F – AH Plus Bioceramic.\u003c/p\u003e","description":"","filename":"floatimage1.png","url":"https://assets-eu.researchsquare.com/files/rs-6908130/v1/f35fcadffccb5d973053a2e6.png"},{"id":86216108,"identity":"42849899-7a42-4278-a4de-9e588b77d99d","added_by":"auto","created_at":"2025-07-08 06:02:12","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":790243,"visible":true,"origin":"","legend":"","description":"","filename":"manuscript.pdf","url":"https://assets-eu.researchsquare.com/files/rs-6908130/v1/49283a0a-677d-4876-af8d-8fc8eb206c85.pdf"}],"financialInterests":"No competing interests reported.","formattedTitle":"Effect of calcium silicate and radiopacifier proportions on the physicochemical properties of endodontic calcium silicate-based sealers","fulltext":[{"header":"INTRODUCTION","content":"\u003cp\u003eThe complete filling of the root canal system remains a major challenge in endodontics. Although various materials and techniques have been proposed, none have achieved this goal [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. In the field of endodontic filling materials, calcium silicate sealers have gained considerable prominence due to their positive influence on the repair of periapical tissues, being recognized as bioactive materials [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR3\" class=\"CitationRef\"\u003e3\u003c/span\u003e]. The bioactivity is primarily attributed to their ability to release ions, particularly calcium and hydroxyl ions [\u003cspan additionalcitationids=\"CR5\" citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR6\" class=\"CitationRef\"\u003e6\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eCalcium silicate-based sealers or hydraulic sealers are well recognized for their ability to induce periapical repair [\u003cspan citationid=\"CR7\" class=\"CitationRef\"\u003e7\u003c/span\u003e, \u003cspan citationid=\"CR8\" class=\"CitationRef\"\u003e8\u003c/span\u003e]. These materials offer long-lasting marginal sealing, high radiopacity, low setting expansion, significant ion-releasing capacity, and adequate working time for endodontic procedures [\u003cspan additionalcitationids=\"CR10\" citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e]. Their biological properties are due to the formation of calcium hydroxide during the setting reaction and its subsequent dissociation [\u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. However, these endodontic sealers have certain limitations, particularly regarding their manipulation and insertion into the root canal system, which stem from their grainy texture [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e]. To overcome these drawbacks, incorporating propylene glycol and barium sulfate can improve plasticity, thereby enhancing its performance as a sealing material. These modifications can occur in the liquid (originally distilled water) and the powder, which initially consisted solely of Portland cement and bismuth oxide [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR13\" class=\"CitationRef\"\u003e13\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eAnother disadvantage of early calcium silicate-based sealers was the discoloration of the tooth structure. Collagen in the dentin matrix reacts with bismuth oxide, resulting in a grayish discoloration [\u003cspan citationid=\"CR14\" class=\"CitationRef\"\u003e14\u003c/span\u003e]. To address this issue, alternative radiopacifiers, such as tantalum oxide and zirconium oxide, have been suggested for use in endodontic cement. Studies have reported favorable results regarding tooth color stability when these radiopacifiers are used [\u003cspan citationid=\"CR15\" class=\"CitationRef\"\u003e15\u003c/span\u003e, \u003cspan citationid=\"CR16\" class=\"CitationRef\"\u003e16\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eThe AH Plus Bioceramic (Dentsply De Trey, Konstanz, Germany) is a premixed tricalcium silicate cement-based sealer that demonstrates adequate properties to be considered a good sealer but still has high solubility [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e]. To date, the volumetric change of AH Plus Bioceramic has not been evaluated. Manufactured by the same company, AH Plus Jet (Dentsply De Trey, Konstanz, Germany) is an epoxy resin-based endodontic sealer marketed in a dual-syringe auto-mix system. It is commonly used as a benchmark for evaluating new sealers due to its excellent physical properties (such as dimensional stability, sealing ability, and flow) and its favorable chemical and biological characteristics, making it the gold standard in clinical practice [\u003cspan citationid=\"CR18\" class=\"CitationRef\"\u003e18\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eBio-C Sealer (Angelus, Londrina, Brazil) is a premixed hydraulic sealer specifically developed for root canal obturation. This ready-to-use material, supplied in a single syringe, contains calcium silicates, calcium aluminate, calcium oxide, zirconium oxide, iron oxide, silicon dioxide, and dispersing agents. Recent studies have demonstrated its superior cytocompatibility compared to AH Plus, showing enhanced cell viability, migration, morphology, adhesion, and mineralization capacity [\u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e]. While exhibiting favorable physicochemical properties, including a short setting time, alkalinizing ability, adequate flow, satisfactory radiopacity, and minimal volumetric change, the sealer shows higher solubility than permitted by ISO 6876 standards [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eVariations in the type and proportion of radiopacifiers can affect the physical and chemical properties of sealers [\u003cspan citationid=\"CR21\" class=\"CitationRef\"\u003e21\u003c/span\u003e]. Also, changes in the calcium content can contribute to the formation of calcium carbonates, which are essential for the bioactivity and biocompatibility of these materials [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR19\" class=\"CitationRef\"\u003e19\u003c/span\u003e, \u003cspan citationid=\"CR22\" class=\"CitationRef\"\u003e22\u003c/span\u003e]. Therefore, determining the optimal ratio of components in hydraulic endodontic sealer is crucial. This study evaluated the physical and chemical properties of calcium silicate-based sealers with varying proportions of calcium silicate and radiopacifiers (P1-P3), including setting time, radiopacity, flowability, solubility, volumetric change, and pH. They were compared with two commercially available sealers: AH Plus Jet and AH Plus Bioceramic. The null hypothesis was that there are no significant differences in the physicochemical properties between the P1, P2, and P3, and the commercial sealers AH Plus Jet and AH Plus Bioceramic, and that the different proportions of calcium silicate and radiopacifiers do not significantly affect these physicochemical properties.\u003c/p\u003e"},{"header":"MATERIAL AND METHODS","content":"\u003cp\u003eThe present study evaluated the physicochemical properties of calcium silicate-based sealers with varying proportions of calcium silicate and radiopacifiers (P1-P3). The composition of the tested sealers is detailed in Table\u0026nbsp;\u003cspan refid=\"Tab1\" class=\"InternalRef\"\u003e1\u003c/span\u003e. They were mixed to a consistency of obturation endodontic sealer, with a powder-to-liquid ratio of 2:1. AH Plus Bioceramic and Bio-C Sealaer were handled according to the manufacturer\u0026rsquo;s instructions. In contrast, AH Plus Jet was manually mixed by blending equal lengths (1 cm) of pastes A and B with a metal spatula on a mixing pad for 30 seconds, until a homogeneous consistency was achieved [\u003cspan citationid=\"CR23\" class=\"CitationRef\"\u003e23\u003c/span\u003e].\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab1\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 1\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eThe manufacturer and composition of the tested sealers.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"2\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSealers and Manufactures\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c2\"\u003e \u003cp\u003eComposition\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eProportion 1 (P1- Bauru School of Dentistry, University of S\u0026atilde;o Paulo, Bauru, Brazil)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePowder: 30% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 40% Tantalum oxide, 25% Zirconium oxide.\u003c/p\u003e \u003cp\u003eLiquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eProportion 2 (P2- Bauru School of Dentistry, University of S\u0026atilde;o Paulo, Bauru, Brazil)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePowder: 40% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 35% Tantalum oxide, 20% Zirconium oxide.\u003c/p\u003e \u003cp\u003eLiquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eProportion 3 (P3- Bauru School of Dentistry, University of S\u0026atilde;o Paulo, Bauru, Brazil)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePowder: 50% Calcium silicate, 2% Calcium chloride, 3% Calcium oxide, 30% Tantalum oxide, 15% Zirconium oxide\u003c/p\u003e \u003cp\u003eLiquid: 90% Propylene glycol, 5% Dimethyl sulfoxide, 5% Polycarboxylate\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Bioceramic (Dentsply De Trey, Konstanz, Germany)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eZirconium dioxide (50\u0026ndash;75%), Tricalcium silicate (5\u0026ndash;15%), Dimethyl sulfoxide (10\u0026ndash;30%), Lithium carbonate (\u0026lt;\u0026thinsp;0.5%), Thickening agent (\u0026lt;\u0026thinsp;6%)\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Jet (Dentsply De Trey, Konstanz, Germany)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003ePaste A: Bisphenol-A epoxy resin, Bisphenol-F epoxy resin, Calcium tungstate, Zirconium oxide, Silica, Iron oxide pigments.\u003c/p\u003e \u003cp\u003ePaste B: Dibenzyldiamine, Aminoadamantane, Tricyclodecane-diamine, Calcium tungstate, Zirconium oxide, Silica, Silicone oil.\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eBio-C Sealer (Angelus, Londrina, Brazil)\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003eCalcium silicate, calcium aluminate, calcium oxide, zirconium oxide, iron oxide, silicon dioxide and dispersing agent\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cdiv id=\"Sec3\" class=\"Section2\"\u003e \u003ch2\u003eSetting Time\u003c/h2\u003e \u003cp\u003eInitial and final setting times were determined according to ASTM C 266\u0026ndash;2008 [\u003cspan citationid=\"CR24\" class=\"CitationRef\"\u003e24\u003c/span\u003e]. The experiment was conducted under controlled conditions of temperature (37\u0026deg;C\u0026thinsp;\u0026plusmn;\u0026thinsp;1\u0026deg;C) and humidity (95% \u0026plusmn; 5%). Fifteen type IV gypsum rings, with an inner diameter of 10 mm and a thickness of 2.0 mm, were used to prepare the specimens (n\u0026thinsp;=\u0026thinsp;3). The cements were placed in the rings that had been pre-soaked in distilled water. After 180\u0026thinsp;\u0026plusmn;\u0026thinsp;5 seconds of mixing, the specimens were tested for setting by applying vertical pressure using a Gilmore needle, first with a 113.5 g needle for the initial setting and then with a 456.5 g needle for the final setting. The time elapsed from insertion into the gypsum rings to when no indentation was visible from either needle on the specimen surface was recorded.\u003c/p\u003e \u003c/div\u003e\n\u003ch3\u003eFlowability\u003c/h3\u003e\n\u003cp\u003eThe flowability test was performed according to ISO 6876/2012 [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. After mixing, 0.05\u0026thinsp;\u0026plusmn;\u0026thinsp;0.005 mL of each cement was dispensed onto a glass plate using a disposable syringe. After 180\u0026thinsp;\u0026plusmn;\u0026thinsp;5 seconds, a second glass plate (20 mm) was placed on top of the cement drop, followed by a 100 g weight, totaling 120\u0026thinsp;\u0026plusmn;\u0026thinsp;2 g. After 10 minutes, the weight was removed, and the largest and smallest diameters of the cement were measured using a digital caliper (0.001 mm). The difference between the largest and smallest diameters was not greater than 1.0 mm. All groups were tested in triplicate (n\u0026thinsp;=\u0026thinsp;3).\u003c/p\u003e\n\u003ch3\u003eRadiopacity\u003c/h3\u003e\n\u003cp\u003eRadiopacity was assessed according to ISO 6876/2012 [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. Fifteen specimens, 10.0 mm in diameter and 1.0 mm in height, were prepared using metal rings (n\u0026thinsp;=\u0026thinsp;3). After preparation, the specimens were placed on occlusal radiographic films, each film receiving one specimen from each experimental group, along with a 1.0 mm control and an aluminum step wedge (scale 1\u0026ndash;10 mm of Al). The films were X-ray sensitized using an X-ray machine operating at 70 kV, 10 mA, with exposure times of 0.3 seconds and a focus/film distance of 30 cm. Radiopacity quantification was performed through densitometric analysis using Adobe Photoshop CC 2017 software (Adobe Systems, USA), employing the formula proposed by Duarte et al. [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]: RD = [A \u0026times; 2/B]\u0026thinsp;+\u0026thinsp;mm Al (immediately lower step), where 'A' is the difference between the radiographic density of the material (RDm) and that of the immediately lower aluminum step; 'B' is the difference between adjacent aluminum steps; and '2' is the standard increment between the steps of the penetrometer. The results were expressed in millimeters of aluminum (mm Al).\u003c/p\u003e\n\u003ch3\u003eSolubility\u003c/h3\u003e\n\u003cp\u003eSolubility was tested according to ISO 6876:2012 [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. The solubility test was performed using metal rings for the AH Plus Jet and gypsum rings for the calcium silicate-based sealers (P1, P2, P3 and AH Plus Bioceramic) with an internal diameter of 20 mm and a thickness of 1.5 mm, placed on a glass plate covered with cellophane paper and filled with the endodontic cement. A waterproof nylon thread was inserted into the material, followed by the placement of another glass plate, also covered with cellophane paper. The assembly was manually pressed to ensure that the plates made uniform contact with the mold. The samples were kept in an oven at 37\u0026deg;C\u0026thinsp;\u0026plusmn;\u0026thinsp;1\u0026deg;C and 95% \u0026plusmn; 5% relative humidity for a period equivalent to three times the setting time of the tested material. After removing residues and loose particles, the samples were weighed on a precision analytical balance. They were then suspended by the nylon thread and placed in plastic containers containing 7.5 mL of distilled and deionized water, ensuring they did not touch the container walls and remained fully submerged. The samples were maintained under these conditions in an oven at 37\u0026deg;C\u0026thinsp;\u0026plusmn;\u0026thinsp;1\u0026deg;C and 95% \u0026plusmn; 5% relative humidity for 7 days. After this period, they were removed from the containers, rinsed with distilled and deionized water, and excess water was removed with absorbent paper. Subsequently, they were kept in a desiccator for 24 hours and weighed again. Solubility was determined by calculating the mass loss of each sample relative to its initial mass.\u003c/p\u003e\n\u003ch3\u003eVolumetric Change Analysis\u003c/h3\u003e\n\u003cp\u003eTo analyze volumetric change, artificial teeth (IM do Brasil, S\u0026atilde;o Paulo, Brazil) with 21 mm long circular canals were prepared using Genius Proflex rotary instruments (Medidenta, Las Vegas, NV, USA) up to a #40/.04 file with a working length 1.0 mm short of the foraminal opening. Before obturation, the apical patency was confirmed using K-type #20 instruments (Dentsply-Maillefer, Konstanz, Germany). After biomechanical preparation, the teeth were obturated using the single-cone technique with size 40.04 taper cones (Tanari, Tanariman, Manacapuru, AM, Brazil). Immediately following obturation, the specimens were scanned using micro-CT and then placed in acrylic pots containing 10 mL of phosphate-buffered saline (PBS), with only the root portion in contact with the liquid. The specimens were maintained in an incubator at 37\u0026deg;C and 95% humidity for 7 days. Pre- and post-scans were obtained using a micro-CT system (1174v2 SkyScan; Bruker-microCT, Kontich, Belgium) operating at 50 kV, 800 mA, with 360-degree rotation, and an isotropic resolution of 23.97 \u0026micro;m. The system includes a high-resolution camera (1304 \u0026times; 1024 pixels). The images of each sample were reconstructed using specialized software (NRecon v.1.6.3; Bruker-microCT), generating transverse and axial slices of the samples\u0026rsquo; structure. The surface segmentation and modeling were performed using the automatic CTAN v.1.12 software (Bruker-microCT) from the pre-scan images. For volumetric assessment of the material pre- and post-volume, the CTAN software (Bruker-microCT) was employed. The volume of material (mm\u0026sup3;) was calculated for the apical 10 mm of each sample. Volumetric change was expressed as a percentage, calculated as the difference between the initial and final volumes. Negative values indicate volume expansion of the material [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e].\u003c/p\u003e \u003cdiv id=\"Sec8\" class=\"Section2\"\u003e \u003ch2\u003epH\u003c/h2\u003e \u003cp\u003eThe same acrylic teeth, prepared and obturated as described for the volumetric analysis, were used for pH determination. After obturation, the apices of the teeth were immediately immersed in acrylic pots containing 10 ml of phosphate-buffered saline and placed in an incubator at 37\u0026deg;C and 95% humidity for the experiment. All pots were pre-treated with nitric acid to prevent any interference with the results. pH measurements were conducted at 3, 24, 72, and 168 hours using a calibrated pH meter [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e].\u003c/p\u003e \u003c/div\u003e \u003cdiv id=\"Sec9\" class=\"Section2\"\u003e \u003ch2\u003eStatistical Analysis\u003c/h2\u003e \u003cp\u003eThe data were subjected to normality analysis using the Kolmogorov-Smirnov test, which indicated a normal distribution. For global comparison, ANOVA was applied, and individual comparisons were performed using the Tukey test. The statistical software used was GraphPad Prism 9.0 (GraphPad Software Inc, San Diego, CA). A significance level of 5% was adopted.\u003c/p\u003e \u003c/div\u003e"},{"header":"RESULTS","content":"\u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab2\" class=\"InternalRef\"\u003e2\u003c/span\u003e presents the mean and standard deviation for the initial and final setting times, flowability, radiopacity, solubility, and volumetric change. Statistically significant differences (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05) were observed in setting times among all groups, except for the initial setting time between P1 and AH Plus Bioceramic (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05). The radiopacity results showed that P1 and AH Plus Jet demonstrated the highest radiopacity values, with no statistically significant difference between them (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05). Bio-C Sealer presented the lowest radiopacity value (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). Significant differences were found between P1 and both P3 and AH Plus Bioceramic, between P2 and AH Plus Bioceramic, and between AH Plus Jet and P2, P3, and AH Plus Bioceramic (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). The calcium silicate-based sealer (P1, P2, P3, Bio-C Sealer and AH Plus Bioceramic) exhibited higher solubility than AH Plus Jet (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). No statistically significant differences were observed in solubility among the three P (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05). Regarding volumetric change, Bio-C Sealer and AH Plus Bioceramic showed significantly higher volume alteration than P2 (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). No significant differences were observed between P1, P3, AH Plus Jet, and the other materials (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05) \u0026ndash; Fig.\u0026nbsp;\u003cspan refid=\"Fig1\" class=\"InternalRef\"\u003e1\u003c/span\u003e.\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab2\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 2\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eMean and standard deviation of initial and final setting time (in minutes), flowability (mm), radiopacity (mmAl), solubility (%), and volumetric change (%) of the P1, P2, P3, AH Plus Jet, Bio-C Sealer, and AH Plus Bioceramic.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"7\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c6\" colnum=\"6\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c7\" colnum=\"7\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colname=\"c1\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colspan=\"2\" nameend=\"c3\" namest=\"c2\"\u003e \u003cp\u003eSetting time (min)\u003c/p\u003e \u003c/th\u003e \u003cth align=\"left\" colname=\"c4\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colname=\"c5\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colname=\"c6\"\u003e\u0026nbsp;\u003c/th\u003e \u003cth align=\"left\" colname=\"c7\"\u003e\u0026nbsp;\u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSealers\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cb\u003eInitial\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cb\u003eFinal\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cb\u003eFlowability (mm)\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cb\u003eRadiopacity (mm Al)\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e\u003cb\u003eVolumetric Change (%)\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e\u003cb\u003eSolubility (%)\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e124.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e407\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e20.69\u0026thinsp;\u0026plusmn;\u0026thinsp;0.01\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e9.63\u0026thinsp;\u0026plusmn;\u0026thinsp;1.39\u003csup\u003eac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e2.07\u0026thinsp;\u0026plusmn;\u0026thinsp;2.14\u0026ordf;\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e5.82+/-0.26\u003csup\u003eab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e155.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e426\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e19.70\u0026thinsp;\u0026plusmn;\u0026thinsp;0.01\u003csup\u003eab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e9.22\u0026thinsp;\u0026plusmn;\u0026thinsp;1.25\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e0.18\u0026thinsp;\u0026plusmn;\u0026thinsp;3.10\u0026ordf;\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e4.68+/-2.49\u003csup\u003eab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eP3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e178.0\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e625\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e19.19\u0026thinsp;\u0026plusmn;\u0026thinsp;0.01\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.93\u0026thinsp;\u0026plusmn;\u0026thinsp;2.13\u003csup\u003ebd\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e3.35\u0026thinsp;\u0026plusmn;\u0026thinsp;5.22\u0026ordf;\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e2.68+/-1.57\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Jet\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e847.3\u0026thinsp;\u0026plusmn;\u0026thinsp;4.93\u003csup\u003ed\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e1725\u0026thinsp;\u0026plusmn;\u0026thinsp;1.0\u003csup\u003ed\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e25.47\u0026thinsp;\u0026plusmn;\u0026thinsp;0.01\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e11.73\u0026thinsp;\u0026plusmn;\u0026thinsp;0.98\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e1.65\u0026thinsp;\u0026plusmn;\u0026thinsp;1.47\u0026ordf;\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e0.05+/-0.05\u003csup\u003ec\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eBio C Sealer\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e237.7\u0026thinsp;\u0026plusmn;\u0026thinsp;6.42\u003csup\u003ee\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e446.7\u0026thinsp;\u0026plusmn;\u0026thinsp;4.04\u003csup\u003ee\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e26.9\u0026thinsp;\u0026plusmn;\u0026thinsp;0.99\u003csup\u003ed\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.30\u0026thinsp;\u0026plusmn;\u0026thinsp;0.20\u003csup\u003ed\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e5.49\u0026thinsp;\u0026plusmn;\u0026thinsp;4.24\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e8.10+/-2.15\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Bioc\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e115.0+/-3.0\u003csup\u003ea\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e265+/1.0\u003csup\u003ef\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e30.38+/-0.01\u003csup\u003ee\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.58+/-0.59\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c6\"\u003e \u003cp\u003e4.54\u0026thinsp;\u0026plusmn;\u0026thinsp;2.02\u003csup\u003eb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c7\"\u003e \u003cp\u003e4.49+/-1.51\u003csup\u003eab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003ctfoot\u003e \u003ctr\u003e\u003ctd colspan=\"7\"\u003eDifferent superscript lowercase letters represent statistically significance differences (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05) in the same column.\u003c/td\u003e\u003c/tr\u003e \u003c/tfoot\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e \u003cp\u003e \u003c/p\u003e \u003cp\u003eTable\u0026nbsp;\u003cspan refid=\"Tab3\" class=\"InternalRef\"\u003e3\u003c/span\u003e presents the mean and standard deviation of pH test results. In the intra-group evaluation, P1, P2, and P3 exhibited an increase in pH between 24 and 72 hours (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). AH Plus Jet presented a significant pH increase between 3 and 24 hours (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05), with no further significant changes in subsequent periods (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05). AH Plus Bioceramic showed significant pH increases between 3 and 168 hours, 24 and 72 hours, 72 and 168 hours (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). At 3 hours, the pH of AH Plus Jet and Bioceramic was higher than that of P1, P2, and P3 (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). From 24 hours onwards, no significant differences were observed between groups (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05). At 72 hours, the pH of P1, P2, P3, and AH Plus Bioceramic was higher than that of AH Plus Jet (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). At 168 hours, no differences were found between P1, P2, P3, and AH Plus Jet (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05), while AH Plus Bioceramic showed the highest pH (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05). Bio-C Sealer presented the highest pH values, with statistically significant differences between experimental time points (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05), except between 24 and 168 hours (p\u0026thinsp;\u0026gt;\u0026thinsp;0.05).\u003c/p\u003e \u003cp\u003e \u003cdiv class=\"gridtable\"\u003e\u003ctable float=\"Yes\" id=\"Tab3\" border=\"1\"\u003e \u003ccaption language=\"En\"\u003e \u003cdiv class=\"CaptionNumber\"\u003eTable 3\u003c/div\u003e \u003cdiv class=\"CaptionContent\"\u003e \u003cp\u003eMean and standard deviation of pH of the P1, P2, P3, AH Plus Jet, Bio-C Sealer, and AH Plus Bioceramic.\u003c/p\u003e \u003c/div\u003e \u003c/caption\u003e \u003ccolgroup cols=\"5\"\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c1\" colnum=\"1\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c2\" colnum=\"2\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c3\" colnum=\"3\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c4\" colnum=\"4\"\u003e\u003c/div\u003e \u003cdiv align=\"left\" class=\"colspec\" colname=\"c5\" colnum=\"5\"\u003e\u003c/div\u003e \u003cthead\u003e \u003ctr\u003e \u003cth align=\"left\" colspan=\"5\" nameend=\"c5\" namest=\"c1\"\u003e \u003cp\u003epH\u003c/p\u003e \u003c/th\u003e \u003c/tr\u003e \u003c/thead\u003e \u003ctbody\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eSealers\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e\u003cb\u003e3h\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e\u003cb\u003e24h\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e\u003cb\u003e72h\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e\u003cb\u003e168h\u003c/b\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eES1\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.86\u0026thinsp;\u0026plusmn;\u0026thinsp;0.008\u003csup\u003eABab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6.86\u0026thinsp;\u0026plusmn;\u0026thinsp;0.007\u003csup\u003eAa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.019\u003csup\u003eBab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.015\u003csup\u003eABa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eES2\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.011\u003csup\u003eABabc\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.003\u003csup\u003eACac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.008\u003csup\u003eBab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.010\u003csup\u003eABac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eES3\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.86\u0026thinsp;\u0026plusmn;\u0026thinsp;0.005\u003csup\u003eAa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6.86\u0026thinsp;\u0026plusmn;\u0026thinsp;0.006\u003csup\u003eACac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.015\u003csup\u003eAa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.043\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Jet\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.88\u0026thinsp;\u0026plusmn;\u0026thinsp;0.005\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.011\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.86\u0026thinsp;\u0026plusmn;\u0026thinsp;0.007\u003csup\u003eAb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.027\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eBio C Sealer\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e7.15\u0026thinsp;\u0026plusmn;\u0026thinsp;0.012\u003csup\u003eAa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e7.00\u0026thinsp;\u0026plusmn;\u0026thinsp;0.011\u003csup\u003eBbd\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e7.25\u0026thinsp;\u0026plusmn;\u0026thinsp;0.008\u003csup\u003eCc\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e7.04\u0026thinsp;\u0026plusmn;\u0026thinsp;0.050\u003csup\u003eBb\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eAH Plus Bioceramic\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6,884+/-0,006\u003csup\u003eAc\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6,859+/-0,013\u003csup\u003eBa\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6,882+/-0,009\u003csup\u003eAab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6,910+/-0,009\u003csup\u003eCc\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003ctr\u003e \u003ctd align=\"left\" colname=\"c1\"\u003e \u003cp\u003eControl\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c2\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.013\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c3\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.013\u003csup\u003eAc\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c4\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.013\u003csup\u003eAab\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003ctd align=\"left\" colname=\"c5\"\u003e \u003cp\u003e6.87\u0026thinsp;\u0026plusmn;\u0026thinsp;0.013\u003csup\u003eAac\u003c/sup\u003e\u003c/p\u003e \u003c/td\u003e \u003c/tr\u003e \u003c/tbody\u003e \u003c/colgroup\u003e \u003ctfoot\u003e \u003ctr\u003e\u003ctd colspan=\"5\"\u003eDifferent superscript lower-case letters represent statistically significance differences (P\u0026thinsp;\u0026lt;\u0026thinsp;.05) between periods studied in the same group. Different superscript upper-case letters represent statistically significance differences (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05) in the same column.\u003c/td\u003e\u003c/tr\u003e \u003c/tfoot\u003e \u003c/table\u003e\u003c/div\u003e \u003c/p\u003e"},{"header":"DISCUSSION","content":"\u003cp\u003eDeveloping new endodontic sealers with optimized physicochemical and biological properties is crucial for endodontic treatment. Ready-to-use calcium silicate sealers have been introduced to the market, featuring variations in powder composition and vehicles. However, these materials often exhibit high solubility, with values frequently exceeding the limits of ISO standards [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e, \u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e, \u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Thus, the present study aimed to analyze three formulations with different calcium silicate/radiopacifiers proportions and compare them to the epoxy resin sealer AH Plus Jet and two ready-to-use commercial calcium silicate sealers, AH Plus Bioceramic and Bio-C Sealer.\u003c/p\u003e \u003cp\u003eThe results of our study indicate that the lower calcium silicate content led to a faster setting, as well as higher flowability and radiopacity. P1 exhibited an initial setting time similar to AH Plus Bioceramic, although its final setting time was slightly longer. This suggests that AH Plus Bioceramic may contain components that accelerate setting more effectively. Notably, lithium carbonate, present in small concentrations in its composition, can modulate the setting reaction. This compound is commonly used in cement mixtures for tiling to accelerate the setting time [\u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e, \u003cspan citationid=\"CR30\" class=\"CitationRef\"\u003e30\u003c/span\u003e]. AH Plus Bioceramic exhibited shorter setting times than AH Plus Jet, consistent with findings from a previous study [\u003cspan citationid=\"CR17\" class=\"CitationRef\"\u003e17\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eAll sealers evaluated exhibited radiopacity greater than 3 mm of Al. AH Plus Jet, which contains zirconium oxide and calcium tungstate in its composition as radiopacifiers, showed the highest value. A recent study [\u003cspan citationid=\"CR31\" class=\"CitationRef\"\u003e31\u003c/span\u003e] reported that the use of tantalum and zirconium oxide as radiopacifiers appears to be systemically safe. These findings support the clinical safety of these radiopacifiers in endodontic sealers, so they were selected for the different proportions (P1, P2 e P3). The results of our study are consistent with those found by Kandemir Demirci et al. [\u003cspan citationid=\"CR32\" class=\"CitationRef\"\u003e32\u003c/span\u003e], who reported similar radiopacity values for AH Plus Jet. The formulations P1, P2, and P3, which combined zirconium oxide with tantalum oxide, demonstrated greater radiopacity than AH Plus Bioceramic, with P1 achieving values comparable to those of AH Plus Jet. This is in line with the fact that using 30% zirconium oxide can yield values near 3 mm Al, as reported by Duarte et al. [\u003cspan citationid=\"CR26\" class=\"CitationRef\"\u003e26\u003c/span\u003e]. Increased radiopacity enhances the material\u0026rsquo;s contrast with mineralized structures such as dentin, cementum, and bone, facilitating its visibility in radiographs.\u003c/p\u003e \u003cp\u003eThe lower proportions of calcium silicate and higher concentrations of radiopacifiers exhibited lower flowability. This could be due to the higher density of radiopacifiers, which might increase the viscosity of the material, making it less fluid. Additionally, the reduced proportion of calcium silicate may result in a thicker, less flowable mixture, potentially due to a decrease in the formation of hydrated compounds. These factors may collectively contribute to the observed reduction in flowability. The flowability of AH Plus Jet was similar to that observed in a previous study [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. In our study, the AH Plus Bioceramic showed the highest flowability. While higher flowability may improve sealer penetration in complex anatomical areas and dentinal tubules, it could also lead to greater risk of extrusion, which can be associated with postoperative pain [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eISO standards set limits for the solubility of endodontic sealers to ensure their long-term effectiveness and safety. According to ISO 6876:2012, the maximum allowable solubility is 3% [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e]. The results of the present study show solubility values within ISO standards only for the AH Plus Jet and P3. Interestingly, Bio-C Sealer, which exhibited the highest solubility and volumetric change among hydraulic sealers, also produced the highest pH values. This correlation may be explained by its greater ion release capacity, particularly calcium and hydroxyl ions, which is directly associated with the bioactivity of hydraulic cements [\u003cspan additionalcitationids=\"CR3\" citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e\u0026ndash;\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e]. While the solubility of calcium silicate-based sealers may be considered a disadvantage in terms of dimensional stability, it is precisely this characteristic that contributes to their reparative biological potential through enhanced bioactivity [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR12\" class=\"CitationRef\"\u003e12\u003c/span\u003e]. The solubility of tricalcium silicate sealers varies in the literature, possibly related to differences in protocols and methodologies used [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR11\" class=\"CitationRef\"\u003e11\u003c/span\u003e, \u003cspan citationid=\"CR29\" class=\"CitationRef\"\u003e29\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eIdeally, endodontic sealers should exhibit minimal volumetric alteration after setting to prevent compromising the quality of the root canal filling [\u003cspan citationid=\"CR1\" class=\"CitationRef\"\u003e1\u003c/span\u003e, \u003cspan citationid=\"CR9\" class=\"CitationRef\"\u003e9\u003c/span\u003e, \u003cspan citationid=\"CR10\" class=\"CitationRef\"\u003e10\u003c/span\u003e]. The in vitro methods proposed by the ADA [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e] and ISO [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e] to assess solubility and dimensional stability do not fully replicate the clinical situation; therefore, our study employed a methodology previously reported in the literature, where only the radicular portion of the teeth remains in contact with the medium and is maintained in a controlled temperature and humidity environment [\u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e]. Although natural teeth were not used in our study, a prior study demonstrated that artificial teeth can be considered a viable option for evaluating obturation quality using the single-cone technique with calcium silicate-based sealers [\u003cspan citationid=\"CR35\" class=\"CitationRef\"\u003e35\u003c/span\u003e]. To minimize the risk of bias, the single-cone technique was adopted, and all obturations were performed by a single experienced operator. Additionally, PBS solution was used as the storage medium, as previous research has shown that storage in PBS significantly reduces the volumetric change of calcium silicate-based sealers [\u003cspan citationid=\"CR28\" class=\"CitationRef\"\u003e28\u003c/span\u003e]. Our results indicate that the experimental sealers and AH Plus Jet exhibited lower volumetric changes compared to AH Plus Bioceramic and Bio-C Sealer. No studies have published data on the volumetric change of AH Plus Bioceramic; however, previous studies have reported similar volumetric changes for resin-based and calcium silicate-based sealers [\u003cspan citationid=\"CR20\" class=\"CitationRef\"\u003e20\u003c/span\u003e, \u003cspan citationid=\"CR33\" class=\"CitationRef\"\u003e33\u003c/span\u003e].\u003c/p\u003e \u003cp\u003eOne of the main characteristics of calcium silicate-based sealers is the formation of calcium hydroxide during hydration, which leads to the alkalinization of the environment [\u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e]. Although previous studies have shown that calcium silicate-based sealers can alkalinize the surrounding environment [\u003cspan citationid=\"CR2\" class=\"CitationRef\"\u003e2\u003c/span\u003e, \u003cspan citationid=\"CR4\" class=\"CitationRef\"\u003e4\u003c/span\u003e, \u003cspan citationid=\"CR27\" class=\"CitationRef\"\u003e27\u003c/span\u003e], our results revealed that none of the tested sealers could alkalinize the solution. This may be related to differences in the methodologies used to assess pH. The methodology employed in our study aimed to replicate clinical practice, where the sealers are placed within the root canal system, with no direct contact between the material and the extra-radicular environment.\u003c/p\u003e \u003cp\u003eThe null hypotheses were rejected, as significant differences (p\u0026thinsp;\u0026lt;\u0026thinsp;0.05) were observed in several physicochemical properties, including setting times, flowability, radiopacity, solubility, and volumetric change, between the P1, P2, P3, and the commercial sealers (AH Plus Jet and AH Plus Bioceramic). The different proportions exhibited higher solubility and lower volumetric change compared to AH Plus Bioceramic, while radiopacity varied significantly among groups. Additionally, the different proportions of calcium silicate and radiopacifiers in the experimental sealers significantly influenced some properties, such as flowability and setting times, but not others, such as volumetric change among the experimental groups. The pH variations also showed significant differences at specific time points, further supporting the rejection of the null hypotheses. These findings indicate that the composition of sealers, particularly the proportions of calcium silicate and radiopacifiers, plays a critical role in determining their physicochemical properties.\u003c/p\u003e \u003cp\u003ePhysical and chemical studies are crucial and should be conducted before the biological testing of endodontic sealers, as they provide essential data on the material's properties. In our study, the P1 exhibited high radiopacity, high flow, low volumetric change, and a favorable setting time, while P3 was the only hydraulic sealer with solubility values within ISO [\u003cspan citationid=\"CR25\" class=\"CitationRef\"\u003e25\u003c/span\u003e] and ADA [\u003cspan citationid=\"CR34\" class=\"CitationRef\"\u003e34\u003c/span\u003e] limits. This suggests that the 50% calcium silicate/45% radiopacifier formulation may represent an optimal balance for clinical applications. The solubility of P1, P2, and AH Plus Bioceramic remained a drawback, indicating that compositional adjustments may be necessary for these formulations. Further biological and clinical studies are required to comprehensively evaluate these sealers, alongside additional tests such as bond strength (adhesion), push-out resistance, dentin-sealer interface analysis, and failure mode assessment.\u003c/p\u003e"},{"header":"CONCLUSION","content":"\u003cp\u003eFormulation P1 (30% calcium silicate / 65% radiopacifier) demonstrated high radiopacity, favorable flowability, and low volumetric change, comparable to AH Plus Jet. Notably, formulation P3 (50% calcium silicate / 45% radiopacifier) was the only hydraulic sealer with solubility values within ISO standards, whereas P1, P2, and the commercial calcium silicate-based sealers exhibited higher solubility than AH Plus Jet. Although compositional differences affected setting time and flowability, volumetric changes remained minimal for P1, P2, P3, and AH Plus Jet.\u003c/p\u003e "},{"header":"Declarations","content":"\u003cp\u003eAcknowledgements\u0026nbsp;\u003c/p\u003e\n\u003cp\u003eThe authors deny any conflicts of interest related to this study. The first author would like to thank S\u0026atilde;o Paulo Research Foundation (FAPESP- Process number: 2024/01063-0) for providing financial support.\u003c/p\u003e\n\u003cp\u003eAuthor contributions: M.A.H.D., G.F.S., and R.S.O.N. contributed to the conceptualization. R.S.O.N., M.P.A., S.J.R. and M.A.H.D. contributed to the methodology. R.S.O.N., M.P.A., T.C.M.V., S.J.R., B.S.W. and M. A. H. D. contributed to the investigation. M.P.A., R. R. V., G.F.S., and M. A. H. D. contributed to the formal analysis. M.A.H.D., M.P.A., and R.S.O.N. contributed to data curation. R.S.O.N., G.F.S. and T.C.M.V. wrote and prepared the original draft. B.S.W., R.S.O.N. and M. A. H. D. contributed to the review and editing of the study report. M.A.H.D. contributed to supervision. M.P.A., R.R.V., G.F.S. and M.A.H.D. \u0026nbsp;contributed to project administration. M.A.H.D. and R.S.O.N. contributed to funding acquisition.\u003c/p\u003e\n\u003cp\u003eConflict of Interest: The authors declare that they have no conflict of interest.\u003c/p\u003e\n\u003cp\u003eFunding: Funding: This work was supported by S\u0026atilde;o Paulo Research Foundation (FAPESP - Process number 2024/01063-0).\u003c/p\u003e\n\u003cp\u003eEthical approval: No ethical approval was required for this type of laboratory study\u003c/p\u003e\n\u003cp\u003eInformed consent: No formal consent was required for this type of laboratory study.\u003c/p\u003e"},{"header":"References","content":"\u003col\u003e\n\u003cli\u003eCamilleri J, Atmeh A, Li X, Meschi N. Present status and future directions: Hydraulic materials for endodontic use. Int Endod J. 2022 May;55 Suppl 3(Suppl 3):710-777. doi: 10.1111/iej.13709. Epub 2022 Mar 17. Erratum in: Int Endod J. 2023 Mar;56(3):402. doi: 10.1111/iej.13881. \u003c/li\u003e\n\u003cli\u003eDuarte MA, Demarchi AC, Yamashita JC, Kuga MC, Fraga Sde C. pH and calcium ion release of 2 root-end filling materials. Oral Surg Oral Med Oral Pathol Oral Radiol Endod. 2003 Mar;95(3):345-7. doi: 10.1067/moe.2003.12. \u003c/li\u003e\n\u003cli\u003eNiu LN, Jiao K, Wang TD, Zhang W, Camilleri J, Bergeron BE, Feng HL, Mao J, Chen JH, Pashley DH, Tay FR. A review of the bioactivity of hydraulic calcium silicate cements. J Dent. 2014 May;42(5):517-33. doi: 10.1016/j.jdent.2013.12.015. \u003c/li\u003e\n\u003cli\u003eCandeiro GT, Correia FC, Duarte MA, Ribeiro-Siqueira DC, Gavini G. Evaluation of radiopacity, pH, release of calcium ions, and flow of a bioceramic root canal sealer. J Endod. 2012 Jun;38(6):842-5. doi: 10.1016/j.joen.2012.02.029.\u003c/li\u003e\n\u003cli\u003eL\u0026oacute;pez-Garc\u0026iacute;a S, S\u0026aacute;nchez-Bautista S, Garc\u0026iacute;a-Bernal D, Lozano A, Forner L, Sanz JL, Murcia L, Rodr\u0026iacute;guez-Lozano FJ, O\u0026ntilde;ate-S\u0026aacute;nchez RE. Premixed calcium silicate-based ceramic sealers promote osteogenic/cementogenic differentiation of human periodontal ligament stem cells: A microscopy study. Microsc Res Tech. 2024 Jul;87(7):1584-1597. doi: 10.1002/jemt.24545. \u003c/li\u003e\n\u003cli\u003eMora A, Garc\u0026iacute;a-Bernal D, Rodr\u0026iacute;guez-Lozano FJ, Sanz JL, Forner L, Ghilotti J, Lozano A, L\u0026oacute;pez-Garc\u0026iacute;a S. Biocompatibility, bioactivity and immunomodulatory properties of three calcium silicate-based sealers: an in vitro study on hPDLSCs. 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Assessment of color stability of white mineral trioxide aggregate angelus and bismuth oxide in contact with tooth structure. J Endod. 2014 Aug;40(8):1235-40. doi: 10.1016/j.joen.2014.01.044.\u003c/li\u003e\n\u003cli\u003eAguiar BA, Frota LMA, Taguatinga DT, Vivan RR, Camilleri J, Duarte MAH, de Vasconcelos BC. Influence of ultrasonic agitation on bond strength, marginal adaptation, and tooth discoloration provided by three coronary barrier endodontic materials. Clin Oral Investig. 2019 Nov;23(11):4113-4122. doi: 10.1007/s00784-019-02850-y.\u003c/li\u003e\n\u003cli\u003eLin HN, Wang LC, Chen MS, Chang PJ, Lin PY, Fang A, Chen CY, Lee PY, Lin CK. Discoloration Improvement by Mechanically-Milled Binary Oxides as Radiopacifier for Mineral Trioxide Aggregates. Materials (Basel). 2022 Nov 10;15(22):7934. doi: 10.3390/ma15227934. \u003c/li\u003e\n\u003cli\u003eSouza LC, Neves GST, Kirkpatrick T, Letra A, Silva R. Physicochemical and Biological Properties of AH Plus Bioceramic. 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J Endod. 2019 Oct;45(10):1248-1252. doi: 10.1016/j.joen.2019.07.006.\u003c/li\u003e\n\u003cli\u003eMarciano MA, Duarte MA, Camilleri J. Calcium silicate-based sealers: Assessment of physicochemical properties, porosity and hydration. Dent Mater. 2016 Feb;32(2):e30-40. doi: 10.1016/j.dental.2015.11.008. \u003c/li\u003e\n\u003cli\u003eGandolfi MG, Taddei P, Modena E, Siboni F, Prati C. Biointeractivity-related versus chemi/physisorption-related apatite precursor-forming ability of current root end filling materials. J Biomed Mater Res B Appl Biomater. 2013 Oct;101(7):1107-23. doi: 10.1002/jbm.b.32920. \u003c/li\u003e\n\u003cli\u003eRosa SJ, Duarte MAH, Silva EJNL, Oliveira MCG, Titato PCG, Vasconcelos BC, Vivan RR, Alcalde MP. Does the Mixing Method of AH Plus Jet Affect its Physicochemical and Mechanical Properties? J Endod. 2024 Sep;50(9):1333-1339. doi: 10.1016/j.joen.2024.06.006.\u003c/li\u003e\n\u003cli\u003eASTM C266-08: Standard Test Method for Time of Setting of Hydraulic-Cement Paste by Gillmore Needles. West Conshohocken, PA: ASTM International, 2008.\u003c/li\u003e\n\u003cli\u003eInternational Organization for Standardization. ISO 6876: Dental Root Canal Sealing Materials. Geneva, Switzerland: International Organization for Standardization; 2012.\u003c/li\u003e\n\u003cli\u003eH\u0026uacute;ngaro Duarte MA, de Oliveira El Kadre GD, Vivan RR, Guerreiro Tanomaru JM, Tanomaru Filho M, de Moraes IG. Radiopacity of portland cement associated with different radiopacifying agents. J Endod. 2009 May;35(5):737-40. doi: 10.1016/j.joen.2009.02.006.\u003c/li\u003e\n\u003cli\u003eCavenago BC, Pereira TC, Duarte MA, Ordinola-Zapata R, Marciano MA, Bramante CM, Bernardineli N. Influence of powder-to-water ratio on radiopacity, setting time, pH, calcium ion release and a micro-CT volumetric solubility of white mineral trioxide aggregate. Int Endod J. 2014 Feb;47(2):120-6. doi: 10.1111/iej.12120. \u003c/li\u003e\n\u003cli\u003eTorres FFE, Zordan-Bronzel CL, Guerreiro-Tanomaru JM, Ch\u0026aacute;vez-Andrade GM, Pinto JC, Tanomaru-Filho M. Effect of immersion in distilled water or phosphate-buffered saline on the solubility, volumetric change and presence of voids within new calcium silicate-based root canal sealers. Int Endod J. 2020 Mar;53(3):385-391. doi: 10.1111/iej.13225. \u003c/li\u003e\n\u003cli\u003eCardinali F, Camilleri J. A critical review of the material properties guiding the clinician\u0026apos;s choice of root canal sealers. Clin Oral Investig. 2023 Aug;27(8):4147-4155. doi: 10.1007/s00784-023-05140-w. \u003c/li\u003e\n\u003cli\u003eZhang Y, Wang Y, Li T, Xiong Z, Sun Y. Effects of lithium carbonate on performances of sulphoaluminate cement-based dual liquid high water material and its mechanisms. Construction and Building Materials. 2018;161:374-80. doi: 10.1016/j.conbuildmat.2017.11.130.\u003c/li\u003e\n\u003cli\u003eJanini ACP, Moraes BF, Pelepenko LE, Dos Santos VAB, Barros-Costa M, Malos\u0026aacute; GF, Batista FRS, Meira JAS, Matsumoto MA, Antunes TBM, Darin Filho G, Haiter Neto F, Gomes BPFA, Marciano MA. Physicochemical properties and biological interaction of calcium silicate-based sealers - in vivo model. Clin Oral Investig. 2025 Jan 25;29(1):86. doi: 10.1007/s00784-025-06150-6. \u003c/li\u003e\n\u003cli\u003eKandemir Demirci G, \u0026Ccedil;\u0026ouml;ven FO, G\u0026uuml;neri P, Karavana SY, Nalbantsoy A, K\u0026ouml;se T, Kaval ME. The solubility, pH value, chemical structure, radiopacity, and cytotoxicity of four different root canal sealers: an in vitro study. Clin Oral Investig. 2023 Sep;27(9):5413-5425. doi: 10.1007/s00784-023-05160-6. \u003c/li\u003e\n\u003cli\u003eDrumond JPSC, Maeda W, Nascimento WM, Campos DL, Prado MC, de-Jesus-Soares A, Frozoni M. Comparison of Postobturation Pain Experience after Apical Extrusion of Calcium Silicate- and Resin-Based Root Canal Sealers. J Endod. 2021 Aug;47(8):1278-1284. doi: 10.1016/j.joen.2021.05.008. \u003c/li\u003e\n\u003cli\u003eAmerican National Standards/American Dental Association. Specification no. 57 for Endodontic Sealing Materials. Chicago, IL, USA: American National Standards/American Dental Association; 2000.\u003c/li\u003e\n\u003cli\u003eKooanantkul C, Shelton RM, Camilleri J. Comparison of obturation quality in natural and replica teeth root-filled using different sealers and techniques. Clin Oral Investig. 2023 May;27(5):2407-2417. doi: 10.1007/s00784-023-04884-9.\u003c/li\u003e\n\u003c/ol\u003e"}],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":true,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":true,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":false,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":false,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true},"keywords":"calcium silicate, dental materials, physicochemical analysis, root canal obturation","lastPublishedDoi":"10.21203/rs.3.rs-6908130/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-6908130/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"\u003cp\u003eOBJECTIVES: This study investigated how varying calcium silicate (30-50%) and radiopacifier (45-65%) proportions affect the physicochemical properties in formulations P1–P3, compared to Bio-C Sealer, AH Plus Bioceramic and AH Plus Jet.\u003c/p\u003e\n\u003cp\u003eMATERIAL AND METHODS: Flowability, solubility, and radiopacity were investigated according to ISO 6876/2012 standards. Setting times were measured based on ASTM C 266-2008 standards. Volumetric changes and pH were assessed using acrylic teeth (n=10) instrumented to #40.04 and filled with the sealers. pH was measured at 3, 24, 72, and 168 hours. The specimens were scanned using micro-CT immediately after filling and after 7 days. pH was measured at 3, 24, 72, and 168 hours.\u003c/p\u003e\n\u003cp\u003eRESULTS: The P1 showed comparable initial setting time to AH Plus Bioceramic (p\u0026gt;0.05). All calcium silicate-based sealers demonstrated higher solubility than AH Plus Jet (p\u0026lt;0.05), with P3 being the only calcium silicate formulation that met ISO solubility standards. P1 and AH Plus Jet had superior radiopacity (p \u0026lt; 0.05). Bio-C Sealer and AH Plus Bioceramic showed higher volume alteration than P2 (p\u0026lt;0.05). P1, P2, and P3 demonstrated stable volumetric changes and progressive alkalinization (pH peak at 72h). Bio-C Sealer significantly increased the pH over time, except between 24 and 168 hours (p\u0026gt;0.05).\u003c/p\u003e\n\u003cp\u003eCONCLUSIONS: Variations in the proportions of tricalcium silicate and radiopacifiers significantly influenced the sealers' properties. P1 (30% calcium silicate/65% radiopacifier) demonstrated superior radiopacity and flowability, while P3 (50% calcium silicate/45% radiopacifier) was the only calcium silicate-based sealer complying with ISO solubility standards.\u003c/p\u003e\n\u003cp\u003eCLINICAL RELEVANCE: Variations in the proportions of calcium silicate and radiopacifiers significantly influenced the sealers' properties. The calcium silicate-based endodontic sealer with 50% calcium silicate and 45% radiopacifier demonstrated ISO-compliant solubility while maintaining optimal physicochemical balance.\u003c/p\u003e","manuscriptTitle":"Effect of calcium silicate and radiopacifier proportions on the physicochemical properties of endodontic calcium silicate-based sealers","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-06-24 12:01:22","doi":"10.21203/rs.3.rs-6908130/v1","editorialEvents":[{"type":"communityComments","content":0}],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"researchsquare","isNatureJournal":false,"hasQc":true,"allowDirectSubmit":true,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"/submission","title":"Research Square","twitterHandle":"researchsquare","acdcEnabled":true,"dfaEnabled":false,"editorialSystem":"","reportingPortfolio":"","inReviewEnabled":false,"inReviewRevisionsEnabled":true}}],"origin":"","ownerIdentity":"8cb4e186-4767-406e-b483-e88d95b91e7d","owner":[],"postedDate":"June 24th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"posted","subjectAreas":[],"tags":[],"updatedAt":"2025-07-08T05:54:05+00:00","versionOfRecord":[],"versionCreatedAt":"2025-06-24 12:01:22","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-6908130","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-6908130","identity":"rs-6908130","version":["v1"]},"buildId":"XKTyCvWXoU3ODBz1xrDgd","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}