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Physical properties and hydration behavior of a fast-setting bioceramic endodontic material Guo, Ya-juan; Du, Tian-feng; Li, Hong-bo; Shen, Ya; Mobuchon, Christophe; Hieawy, Ahmed; Wang, Zhe-jun; Yang, Yan; Ma, Jingzhi; Haapasalo, Markus Feb 20, 2016

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RESEARCH ARTICLE Open AccessPhysical properties and hydration behaviorof a fast-setting bioceramic endodonticmaterialYa-juan Guo1†, Tian-feng Du2,3†, Hong-bo Li1, Ya Shen3,4*, Christophe Mobuchon4, Ahmed Hieawy3,Zhe-jun Wang3, Yan Yang5, Jingzhi Ma5 and Markus Haapasalo3AbstractBackground: To investigate the physical properties and the hydration behaviour of the fast-setting bioceramiciRoot FS Fast Set Root Repair Material (iRoot FS) and three other endodontic cements.Methods: iRoot FS, Endosequence Root Repair Material Putty (ERRM Putty), gray and white mineral trioxide aggregate(G-MTA & W-MTA), and intermediate restorative material (IRM) were evaluated. The setting time was measured usingANSI/ADA standards. Microhardness was evaluated using the Vickers indentation test. Compressive strength and porositywere investigated at 7 and 28 days. Differential scanning calorimetry (DSC) was employed for the hydration test.Results: iRoot FS had the shortest setting time of the four bioceramic cements (p < .001). The microhardness values ofiRoot FS, ERRM Putty and MTA increased at different rates over the 28 days period. At day one, ERRM Putty had thelowest microhardness of the bioceramic cements (p < .001), but reached the same level as MTA at 4, 7 and 28 days. Themicrohardness of iRoot FS was lower than that of W-MTA at 7 and 28 days (p < .05). The porosity of the materials did notchange after 7 days (p < .05). The compressive strength values at 28 days were significantly greater for all bioceramicgroups compared to those at 7 days (p < .01). ERRM Putty had the highest compressive strength and the lowest porosityof the evaluated bioceramic cements (p < .05), followed by iRoot FS, W-MTA, and G-MTA, respectively. DSC showed thatiRoot FS hydrated fastest, inducing an intense exothermic reaction. The ERRM Putty did not demonstrate a clearexothermic peak during the isothermal calorimetry test.Conclusions: iRoot FS had a faster setting time and hydrating process than the other bioceramic cements tested. Themechanical properties of iRoot FS, G-MTA and W-MTA were relatively similar.Keywords: Calcium phosphate silicate cement, Calcium silicate-based cement, Differential scanning calorimetry,Microhardness, Mineral trioxide aggregate, Physical properties, Setting reactionBackgroundThe first hydraulic calcium silicate-based cement(HCSC) patented for endodontic applications was min-eral trioxide aggregate (MTA; Dentsply Tulsa DentalSpecialties, Johnson City, TN, USA) [1]. It has attractedconsiderable attention [2–4] owing to its excellentsealing ability, biocompatibility, regenerative capabilities,and antibacterial properties [2, 3, 5–7]. The main hy-draulic components in HCSCs are tricalcium silicate(Ca3SiO5 or C3S) and dicalcium silicate (Ca2SiO4 orC2S). HCSCs have been widely used as both endodonticrepair materials and dentin substitutes [8]. An increasingnumber of publications report that these cements pro-duce an apatite-rich surface layer after they contact sim-ulated body fluids [4, 5, 9]. Several HCSC based rootrepair materials have been developed following theintroduction of MTA and are available clinically for den-tists. These include ProRoot (Dentsply Tulsa Dental Spe-cialties), MTA Plus (Prevest-Denpro, Jammu City, India),* Correspondence:†Equal contributors3Division of Endodontics, Department of Oral Biological & Medical Sciences,Faculty of Dentistry, The University of British Columbia, 2199 Wesbrook Mall,Vancouver, BC V6T 1Z3, Canada4Department of Materials Engineering, The University of British Columbia,Vancouver, CanadaFull list of author information is available at the end of the article© 2016 Guo et al. Open Access This article is distributed under the terms of the Creative Commons Attribution 4.0International License (, which permits unrestricted use, distribution, andreproduction in any medium, provided you give appropriate credit to the original author(s) and the source, provide a link tothe Creative Commons license, and indicate if changes were made. The Creative Commons Public Domain Dedication waiver( applies to the data made available in this article, unless otherwise stated.Guo et al. BMC Oral Health  (2016) 16:23 DOI 10.1186/s12903-016-0184-1and BioAggregate (Innovative Bioceramix, Vancouver,Canada). However, there are some drawbacks associatedwith the use of HCSCs including long setting times, dif-ficulty with manipulation, limited resistance to washoutbefore setting, and the possibility of staining the toothstructure [3, 4, 10]. Therefore, new root repair materialsare continually being developed to further improve theirproperties.Calcium phosphate silicate cement (CPSC) is a newgeneration biological cement first proposed in 2006 [11].It consists of phosphate salts in addition to hydraulic cal-cium silicates. The reason for its development was theexpectation that the hydration process would enhance thecement’s mechanical properties and biocompatibility [12].As examples of CPSCs [13], Endosequence Root RepairMaterial Putty (ERRM Putty; Brasseler USA, Savannah,GA, USA) and Endosequence Root Repair Material Paste(ERRM Paste; Brasseler, USA) have been developed asready-to-use, premixed bioceramic materials. Their majorinorganic components include C3S, C2S, and calciumphosphates. The introduction of premixed CPSCs elimi-nates the potential of heterogeneous consistency duringon-site mixing. Because the material is premixed withnonaqueous but water-miscible carriers, it will not setduring storage and hardens only on exposure to an aque-ous environment [14]. Both ERRM Putty and Paste havereasonably good handling properties; their working time ismore than 30 min and their setting time is 4 h [15].However, the long setting time is one of the potentialdrawbacks of HCSCs and CPSCs, consequently two ap-pointments are required with a related increase in chair-side time.Recently, a CPSC iRoot FS Fast Set Root Repair Mater-ial ([iRoot FS]; Innovative Bioceramix) has been intro-duced for use as a root canal repair material, as a fastsetting white hydraulic premixed bioceramic paste( iRoot FS isan insoluble, radiopaque and aluminum-free materialbased on calcium silicate, which requires the presence ofwater to set and harden. A quickly setting cement couldallow for a reduction in chair-side time and the numberof visits needed per treatment. However, the fundamen-tal properties of this improved performance material arestill unknown. Differential scanning calorimetry (DSC) isa thermal analysis technique well suited to the study ofchemical reactions and phase transformations in a widerange of materials. DSC can be used to study the settingof cements by measuring the temperature (i.e., the exo-thermic heat) during the early stages of setting, as wellas monitoring the reaction products that form via theirdecomposition upon heating [16, 17]. The study of thekinetics of the setting reaction could provide significantinformation on new materials. Therefore, the purpose ofthis study was 1) to evaluate the physical properties ofiRoot FS, including the setting time, microhardness,compressive strength and porosity, and compare thesewith ERRM Putty and gray and white ProRoot MTA(G-MTA & W-MTA; Dentsply Tulsa Dental Special-ties) as well as an intermediate restorative material(IRM; Dentsply Caulk, Milford, DE, USA); and 2) toinvestigate the hydration behavior of the cementsusing DSC analysis.MethodsTwo commercially available HCSC, G-MTA (batch12120401B) and W-MTA (batch 11004159) were used inthe present study as well as two CPSC-based cements,ERRM Putty (batch 1306 BPP) and iRoot FS (batch1201FSP-T). IRM was included as a control material(Dentsply Caulk; batch 091214).Setting timeThe MTA and IRM were mixed and manipulated in ac-cordance with the manufacturer’s instructions. Moldswith an inner diameter of 10 mm and a height of 2 mmwere used for the MTA and IRM. The molds wereplaced on a glass plate and the mixed materials werepacked into them. The whole assembly was then trans-ferred to an incubator (37 °C, > 95 % relative humidity).For the iRoot FS and ERRM Putty, which require con-tinuous exposure to moisture during setting [18], plasterof Paris molds with a cavity of 10 mm diameter and2 mm height were used. The molds were first stored at37 °C in a water bath for 24 h, and then the iRoot FSand ERRM Putty were poured into these molds. Thewhole assembly was then stored in a water bath at 37 °C.The initial and final setting times of all samples werein accordance with the American Society for Testingand Materials (ASTM) International Standard C266-03[19] and the American National Standards Institute/American Dental Association (ANSI/ADA) SpecificationNo. 57 [20]. The Gilmore needle for testing the initialsetting time had a weight of 100 g and an active tip of2.0 mm diameter (initial needle). The needle for the finalsetting time had a weight of 400 g and an active tip of1.0 mm diameter (second needle) [21]. The initial needlewas applied lightly on the surface of each sample. Thisprocedure was repeated every 5 min for all bioceramiccements and every 2 min for IRM until the needle didnot create a complete circular depression on the speci-men surface. For each sample, the time that elapsed be-tween the end of mixing and the unsuccessfulindentation was recorded in minutes and defined as “theinitial setting time”. “The final setting time” was deter-mined following the same procedures using the secondneedle, with the 400 g load. Five parallel sets of mea-surements were made for each material.Guo et al. BMC Oral Health  (2016) 16:23 Page 2 of 6Microhardness testingMicrohardness of the set of cements was evaluated usingthe Vickers indentation test (MICROMET 3, BuehlerLtd., Lake Bluff, IL, USA). Each specimen was tested at1, 4, 7 and 28 days, at three points with 3 mm intervalsand a load of 100 g for 10 s. According to the pilotstudy, this load created a clear and reliable indent in allmaterials. Five samples of each material in each groupwere prepared. The tests were performed on surfacespolished with 1200 grit sand paper using a diamondindenter; the indentation size (i.e. diagonal d) wasmeasured and converted to a hardness value as HV[kg/mm2] = 0.0018544 L/d [22].Compressive strengthThe sample sizes for compressive strength were 6 mm indiameter by 12 mm in height. The compressive strengthof specimens was determined according to the methodrecommended by ANSI/ADA No. 96 [23] using auniversal testing machine (Instron 3369, Instron Co.,Norwood, MA, USA). The crosshead speed was 1 mm/minalong the long axis. The compressive strength σc [MPa]was calculated using the following Eq. 1). The specimenswere kept in 37 °C distilled water for pre-set periods of 7and 28 days, respectively. At least five specimens were usedfor each determination.σc ¼ 4P=πD2 ð1Þwhere P is the maximum load, N; D is the mean diam-eter of the specimen, mm.PorosityThe specimens were kept in 37 °C distilled water forpre-set periods of 7 and 28 days. The porosity was deter-mined using the test method described in ASTM Stand-ard C830-00 [24]. Kerosene was chosen as the saturationliquid instead of water to avoid any reaction with thespecimen [24]. The air-dried specimens were dried in anoven at 105 °C to a constant weight and the dry weight,B, was determined (for all weight measurements, thegram was the unit used with an accuracy of 0.001 g).The test specimens were then placed in a beaker con-taining kerosene and located in a vacuum chamber withan absolute pressure of not more than 6.4 kPa for60 min. At least five measurements were taken for eachgroup. The suspended weight, S, was determined foreach test specimen suspended in kerosene. The satu-rated weight, W, was determined by removing all dropsof liquid from the surface using a wet smooth linen. Theexterior volume was calculated by Eq. 2), the volume ofopen pores was calculated by Eq. 3), and the apparentporosity of the specimen was calculated by Eq. 4).V1 ¼ W– Sð Þ = γ ð2ÞV2 ¼ W– Dð Þ = γ ð3ÞP ¼ V2=V1ð Þ  100% ð4Þwhere V1 is the exterior volume of the specimen, cm3;W is the saturated weight, g; S is the suspended weight,g; γ is the density of kerosene, 0.80 g/cm3; V2 is the vol-ume of open pores, cm3; P is the apparent porosity, %; Dis the dry weight, g.Differential scanning calorimetryThe kinetics of the setting reactions of the all sampleswas evaluated with an isothermal calorimeter (DSCQ2000, TA Instruments, New Castle, DE, USA) at a con-stant temperature of 37 °C [25]. The samples weremixed and manipulated in accordance with the manu-facturer’s instructions. The mixtures were transferred topre-weighed 40-mL aluminum crucibles and weighed inan analytical balance so the amount of mixture in eachcould be calculated. The ERRM Putty and iRoot FS weremixed with 10 % distilled water (v/v) because they needto absorb moisture to initiate the setting reaction. Thesample preparation process was completed in 1 min.The heat flux was automatically recorded every 2 s. Eachcrucible was fitted with a lid to prevent water evapor-ation and placed in the DSC for 6 h to analyze any exo-thermic peaks associated with the setting reactions. As areference, an empty 40-mL aluminum crucible was used.All resulting DSC thermograms were evaluated by theDSC manufacturer’s software (TA Instruments). Individ-ual specimens were only tested once. Each cement wastested twice.The results were analyzed using one-way ANOVA ortwo-way ANOVA with post hoc analysis using software(SPSS for Windows 11.0, SPSS, Chicago, IL, USA) whennecessary at a significance level of p < 0.05.ResultsIRM had the shortest initial and final setting time of alltested cements. In the four bioceramic groups, iRoot FShad the shortest initial and final setting time of theCPSCs and HCSCs (p < .001) (Table 1). The initial andfinal setting time of ERRM Putty was longer than W-MTA (p < .001). There was no significant difference inthe initial and final setting time between ERRM Puttyand G-MTA.The microhardness of all materials gradually increasedover the 28 days period (Fig. 1a). At one-day of setting,ERRM Putty had the lowest microhardness among thefour bioceramic cements (p < .001), but reached thesame level as MTA at 4, 7 and 28 days. There was nosignificant difference amongst G-MTA, W-MTA, ERRMPutty and iRoot FS at 7 and 28 days. The microhardnessGuo et al. BMC Oral Health  (2016) 16:23 Page 3 of 6of iRoot FS was lower than W-MTA at 7 and 28 days(p < .05). IRM had had the lowest microhardness ofall tested cements at 28 days.The compressive strength values at 28 days were sig-nificantly greater for all bioceramic groups compared tothose at 7 days (p < .01) (Table 2). IRM had the lowestcompressive strength of all tested materials at 7 and28 days. There was no significant difference in porosityof the experimental groups between 7 and 28 days.ERRM Putty had the highest compressive strength andlowest porosity (p < .05) of the CPSCs and HCSCs.The results of DSC isothermal calorimetry are illus-trated in Fig. 1b. W-MTA showed two exothermicpeaks, a small and narrow peak (0.017 W/g) between 2to 16 min, and a broad peak between 18–60 min. G-MTA had one strong exothermic peak (0.019 W/g) be-tween 4–50 min. iRoot FS showed two exothermicpeaks: a strong and narrow peak (0.031 W/g) between2–15 min and a broad large peak between 40–100 min.The ERRM Putty did not show a clear exothermic peakduring the isothermal calorimetry test. The rate of heat fluxof IRM presented a strong (0.036 W/g) and narrow exo-thermic peak starting at 2 min and ending at 16 min, indi-cating the time and duration of setting reactions of IRM.DiscussionAn important factor in non-surgical as well as surgical re-storative repair in endodontics is to achieve a fluid-tightseal between the tooth and the repair material [26, 27]. Inmost cases a bioceramic material is the restorative mater-ial of choice. The main disadvantage of currently availablebioceramic materials is a setting time of approximately 3to 4 h [2, 3, 28], which compromises the application, espe-cially in supracrestal areas. The possibility of the materialbeing washed out at cervical/furcal area during the longsetting time needs to be considered [27]. In addition, earlyocclusal pressure directed to the material, even in a deeperlocation, may compromise the integrity of the seal [27].Therefore, a bioceramic material that has optimal mech-anical behavior and sets fast, would be attractive to theclinician in specific clinical situations. G-MTA and W-MTA were chosen in the present study as gold standardmaterials because they are widely used for retrograde fill-ing, apexification and perforation repair in endodontictreatment. Although the details of the reaction mecha-nisms of the new CPSCs remain unknown, the results ofthe present study showed that iRoot FS had the shortestsetting time of the CPSCs and HCSCs. The shortest set-ting time of iRoot FS may benefit some clinical challengecases with time demanding. However, clinical study is stillrequired to evaluate its performance.Most of the hydration of these cements occurs duringthe first several days, although complete hydration mayeven take one or two years [4, 9]. The point of max-imum exothermic heat generation has been used as anindication of the setting time of various dental cements[16, 17]. Two exothermic peaks were found in the iRootFS and W-MTA. The first peak possibly correlated withthe initial water absorption on the calcium silicate parti-cles surface, followed by their dissolution and the startof hydration of the calcium silicates in the cements. Thesecond peak can be related to the start of calcium hy-droxide precipitation, mostly on the surface, which is aby-product of calcium silicate hydration [16]. An earlyTable 1 The initial and final setting time (min) of the five materials measuredG-MTAc,d W-MTAe ERRM Puttyd iRoot FSf IRMgInitial setting time (min)a 58.3 ± 2.2 42.2 ± 2.1 61.8 ± 2.5 18.3 ± 2.6 7.2 ± 1.1Final setting time (min)b 217.2 ± 17.3 139.6 ± 10.3 208.0 ± 10.0 57.0 ± 2.7 10.8 ± 1.1Different superscript letters indicate statistically significant differences between groups (p < .05)Fig 1 a Microhardness values [kg/mm2] of MTA, ERRM Putty, iRoot FS and IRM at 1, 4, 7 and 28 days after mixing. b Graphical representation ofthe heat flux generated with time for the different materialsGuo et al. BMC Oral Health  (2016) 16:23 Page 4 of 6strong peak of iRoot FS was in accordance with our set-ting time results: iRoot FS had the shortest setting timeamong the CPSCs and HCSCs. It showed that the iso-thermal DSC analysis can provide a more complete un-derstanding of the setting property of the cements.Interestingly, while G-MTA had one intense exothermicpeak, W-MTA had two peaks. The hydration mechan-ism of G-MTA is expected to be the same as W-MTA,but the chemical components and particle size distribu-tion could be different, thus affecting the hydration kin-etics. No clear exothermic peak was found on ERRMPutty. Therefore, a more advance technique may be re-quired to accurately evaluate the hydration process ofERRM Putty in-depth.The surface microhardness of a material providessome indication of the surface strength of the material[29]. In the present study, the microhardness values ofall cements gradually increased over the 28-day period,which was demonstrated by an early study with G-MTAand W-MTA [30]. Interestingly, the rate of hardening ofERRM Putty was very low during the first day. However,the microhardness of ERRM Putty increased thereafterand reached the same level as the other bioceramic ce-ments at day four. The results showed that all biocera-mic cements used in the present study need at least7 days for complete setting.Compressive strength is one of the indicators of thesetting and strength of a material. Failure in compres-sion is complex, because both the mode and plane offailure are variable. Failure can occur by plastic yielding,cone failure, or by axial splitting [31]. In principle, themode of failure depends on the size and geometry of thespecimen, as well as the precise nature of the materialbeing tested and the rate of loading [31]. This test mea-sures the material’s ability to withstand compression.Higher strength is more desirable, although no clinicallyrelevant minimum, e.g. in endodontics, has been univer-sally proposed. Walsh et al. [32] evaluated the compres-sive strength of ERRM Putty after exposure to saline andfetal bovine serum. The results showed that the com-pressive strength value was 40–45 MPa at 7 days, whichwas lower than the present study. The possible reasonsfor this variation between the two studies (the presentstudy and Walsh et al. [32]) may be different methodolo-gies in the incubation environment and different dimen-sions of prepared samples (5 × 4.17 mm vs 12 × 6 mmin the present study). In the present study, ERRM Puttyhad the highest compressive strength among the ce-ments. This may be attributed to the slow hydrationprocess and small size of porosity of ERRM Putty. Por-osity has a significant role in the relationship betweenmechanical properties of calcium silicate cements, suchas the compressive strength-modulus of elasticity rela-tionship [33]. Indeed, ERRM Putty had the lowest poros-ity among the CPSCs and HCSCs in the present study.Torabinejad et al. [34] reported that the compressivestrength of G-MTA after 24 h was 40 MPa, and it in-creased to 67 MPa after 21 days. Their findings lendsupport to our results: the compressive strength for allbioceramic cements increased with time. The present re-sults revealed that the compressive strength of iRoot FS,G-MTA and W-MTA were relatively similar and stablemechanical properties of bioceramic cements can be ob-tained after 1 month.ConclusionsIn conclusion, iRoot FS had a faster setting time and hy-drating process than the other bioceramic cementstested. The mechanical characteristics of iRoot FS, G-MTA and W-MTA showed no major differences; HCSCcements (MTAs) had a slightly higher final hardnessthan the CPCSc cements, while the opposite was trueregarding the compressive strength.Competing interestsThe authors declare that they have no competing interests.Authors’ contributionsYG and TD carried out the studies and drafted the manuscript. HL, CM andAH participated in the experiment. ZW and YY performed the statisticalanalysis. JM participated in the coordination. YS and MH conceived anddesigned the experiments. YS helped to draft the manuscript. MH finalizedmanuscript. All authors read and approved the final manuscript.AcknowledgmentsThis work was supported by start-up funds provided by the Faculty ofDentistry, University of British Columbia, Canada and by Canada Foundationfor Innovation (CFI fund; Project number 32623). The authors thank BrasselerUSA and Innovative Bioceramix for donating some materials used in thisstudy. The authors deny any conflicts of interest.Table 2 Compressive strength (MPa) and porosity (%) of G-MTA, W-MTA, ERRM Putty, iRoot FS and IRM after 7 & 28 daysCompressive strength (MPa) (((MPa) Porosity (%)7 daysa 28 daysb 7 days 28 daysG-MTA 47.8 ± 12.3c 73.6 ± 14.1d 28.9 ± 2.2h 27.1 ± 1.1hW-MTA 49.6 ± 12.4c,g 78.3 ± 16.0d 31.4 ± 2.3h 30.0 ± 1.6hERRM Putty 107.4 ± 31.1e 176.6 ± 22.0f 16.7 ± 2.8i 14.3 ± 1.1iiRoot FS 56.6 ± 5.9g 96.0 ± 24.3e 20.8 ± 2.7j 21.6 ± 2.2jIRM 40.6 ± 6.4c 49.1 ± 8.0c,g 12.9 ± 2.4i 12.0 ± 2.3iDifferent superscript letters indicate statistically significant differences between the materials in different groups (p < .05)Guo et al. BMC Oral Health  (2016) 16:23 Page 5 of 6Author details1Institute of Stomatology, Chinese PLA General Hospital, Beijing, China.2Department of Stomatology, the First Affiliated Hospital of ZhengzhouUniversity, Zhengzhou, China. 3Division of Endodontics, Department of OralBiological & Medical Sciences, Faculty of Dentistry, The University of BritishColumbia, 2199 Wesbrook Mall, Vancouver, BC V6T 1Z3, Canada.4Department of Materials Engineering, The University of British Columbia,Vancouver, Canada. 5Department of Stomatology, Tongji Hospital, TongjiMedical College, Huazhong University of Science and Technology, Wuhan,China.Received: 13 August 2015 Accepted: 12 February 2016References1. Torabinejad M, White DJ. US Patents 5,769,638 and 5,415,547; 1995.2. Parirokh M, Torabinejad M. Mineral trioxide aggregate: a comprehensiveliterature review—part I: chemical, physical, and antibacterial properties.J Endod. 2010;36:16–27.3. Parirokh M, Torabinejad M. 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