Immersion In Hank's Balanced Salt Solution Research Articles

Multifunctional poly(allylamine hydrochloride)/bioactive glass layer by layer surface coating on magnesium alloy for biomedical applications

The present study reports on a novel multilayer coating for biodegradable magnesium (Mg) alloy substrates. This coating contains soy protein hydrolysate (SPH), poly(allylamine hydrochloride) (PAH), and folic acid (FA) templated bioactive glass (BG) nano particles. The multilayer, designated as SPH/(PAH/BG)n, was coated onto an alkaline-treated Mg alloy surface (AMgS) through a dip-coating process with various numbers of cycles (n = 5and 7) using a layer-by-layer (LbL) assembly. The BG particles had an average diameter of 12.53 ± 2.22 nm and were embedded with therapeutic FA molecules. Scratch testing, wettability, and roughness tests showed excellent adherence of the SPH/(PAH/BG)7 coating on AMgS, making it suitable for cell attachment. Electrochemical measurements in Hanks balanced salt solution (HBSS) demonstrated that the SPH/(PAH/BG)7 coating improved the corrosion resistance of the Mg alloy. SPH/(PAH/BG)7 coated substrate showed a maximum protective efficacy of 98.4041 %, thanks to the bioactive nature of BG. High-resolution XPS and XRD analyses on SPH/(PAH/BG)7/AMgS confirmed the corrosion deposition of Mg(OH)2, MgHPO4.H2O, CaHPO4.H2O, SiO2, MgCO3 and CaCO3 on the substrate surface after immersion in HBSS for 10 d at 37 °C. The LbL coated Mg substrate also showed excellent cytocompatibility by hemolysis assay These results suggest that the SPH/(PAH/BG)7/AMgS material has multifunctional properties and can be a possible alternative for biomedical applications of Mg alloys.

Corrosion behavior and microstructure of the surface corrosion film of biodegradable WE43 and ZX21 Mg alloys in Hanks’ balanced salt solution

In this study, the corrosion behavior and microstructure of the surface corrosion film of WE43 (Mg-4 wt%Y-3 wt%RE) and ZX21 (Mg-2 wt%Zn-1 wt%Ca) Mg alloys immersed in Hanks’ balanced salt solution (HBSS) at 37 °C are investigated. Through cross-sectional transmission electron microscopy (TEM) analysis, the surface corrosion films formed on both alloys after immersion in HBSS for 24 h are mainly a mixture of magnesium hydroxide (Mg(OH)2) and dicalcium phosphate dihydrate (DCPD) (CaHPO4·2H2O). Nevertheless, the surface corrosion film on WE43 alloy is only 114 ± 17 nm with Ca and P enriched in the outer portion of the film, while the surface corrosion film on ZX21 alloy is thicker (406 ± 50 nm) with some scattered hollow corrosion products on top of the film. The difference in the surface corrosion film thickness and microstructure is because of the faster corrosion rate of the ZX21 alloy, which resulted from the occurrence of localized corrosion on the alloy surface.

Localized Corrosion Behavior and the Relationship to the Second Phases in Biodegradable ZX21 Mg Alloy in Hanks' Balanced Salt Solution

Mg alloys are considered promising biodegradable implant materials owing to their high activity, which makes Mg alloys degradable in the human body and can avoid second removal surgeries. Also, compared with other biodegradable implant materials, Mg alloy has a similar density and Young’s modulus to human bones, which minimizes the stress shielding effect. ZX series Mg alloys, which contain Zn and Ca, are designed to increase the alloy strength but maintain biocompatibility. However, even with all the advantages, the high degradation rate limits the clinical applications of ZX series Mg alloys. With fast degradation, not only the mechanical properties are affected, but also a large amount of hydrogen gas and hydroxide ions would accumulate around the implant in the patient. Therefore, it is essential to investigate the corrosion mechanism of the ZX series Mg alloys to mitigate the degradation rates.Localized corrosion is one of the noticeable features in the corrosion process of ZX series Mg alloys, which is the main reason for the low corrosion resistance and high degradation rate of the alloy. However, the origin and detailed mechanism of the initiation and propagation of localized corrosion on ZX series Mg alloys are still unclear. The second phases, which contain Zn and Ca, play complex roles in the corrosion process owing to the inhomogeneous elemental distribution and different electrochemical potentials with respect to the Mg alloy matrix. Thus, this study aims to investigate the microstructure of the localized corrosion sites and the galvanic effects around the second phases in a ZX series Mg alloy.In this study, an Mg-2 wt%Zn-1 wt%Ca (ZX21) alloy was prepared, and the localized corrosion behavior was investigated in a Hanks’ balanced salt solution (HBSS) at 37°C. By scanning electron microscope (SEM)/focused ion beam (FIB) cross-sectional observations, two kinds of second phases were identified in the ZX21 Mg alloy, one is enriched with Zn and the other is not. After immersion in HBSS, galvanic corrosion sites were found in the Mg alloy matrix next to the second phase enriched with Zn, while the Mg alloy matrix next to the second phase with lower Zn concentration was intact. Furthermore, the second phases in the ZX21 Mg alloy were found to hinder the propagation of localized corrosion. The complex roles of the second phases in the ZX21 Mg alloy on the localized corrosion behavior will be discussed based on electrochemical measurements and microstructure characterizations. Figure 1

Chemical-Physical Properties and Bioactivity of New Premixed Calcium Silicate-Bioceramic Root Canal Sealers.

The aim of the study was to analyze the chemical-physical properties and bioactivity (apatite-forming ability) of three recently introduced premixed bioceramic root canal sealers containing varied amounts of different calcium silicates (CaSi): a dicalcium and tricalcium silicate (1-10% and 20-30%)-containing sealer with zirconium dioxide and tricalcium aluminate (CERASEAL); a tricalcium silicate (5-15%)-containing sealer with zirconium dioxide, dimethyl sulfoxide and lithium carbonate (AH PLUS BIOCERAMIC) and a dicalcium and tricalcium silicate (10% and 25%)-containing sealer with calcium aluminate, tricalcium aluminate and tantalite (NEOSEALER FLO). An epoxy resin-based sealer (AH PLUS) was used as control. The initial and final setting times, radiopacity, flowability, film thickness, open pore volume, water absorption, solubility, calcium release and alkalizing activity were tested. The nucleation of calcium phosphates and/or apatite after 28 days aging in Hanks balanced salt solution (HBSS) was evaluated by ESEM-EDX, vibrational IR and micro-Raman spectroscopy. The analyses showed for NeoSealer Flo and AH Plus the longest final setting times (1344 ± 60 and 1300 ± 60 min, respectively), while shorter times for AH Plus Bioceramic and Ceraseal (660 ± 60 and 720 ± 60 min, respectively). Radiopacity, flowability and film thickness complied with ISO 6876/12 for all tested materials. A significantly higher open pore volume was observed for NeoSealer Flo, AH Plus Bioceramic and Ceraseal when compared to AH Plus (p < 0.05), significantly higher values were observed for NeoSealer Flo and AH Plus Bioceramic (p < 0.05). Ceraseal and AH Plus revealed the lowest solubility. All CaSi-containing sealers released calcium and alkalized the soaking water. After 28 days immersion in HBSS, ESEM-EDX analyses revealed the formation of a mineral layer that covered the surface of all bioceramic sealers, with a lower detection of radiopacifiers (Zirconium for Ceraseal and AH Plus Bioceramic, Tantalum for NeoSealer Flo) and an increase in calcium, phosphorous and carbon. The calcium phosphate (CaP) layer was more evident on NeoSealer Flo and AH Plus Bioceramic. IR and micro-Raman revealed the formation of calcium carbonate on the surface of all set materials. A thin layer of a CaP phase was detected only on AH Plus Bioceramic and NeoSealer Flo. Ceraseal did not show CaP deposit despite its highest calcium release among all the tested CaSi-containing sealers. In conclusion, CaSi-containing sealers met the required chemical and physical standards and released biologically relevant ions. Slight/limited apatite nucleation was observed in relation to the high carbonation processes.

71 - Biomimetic Approach to Evaluate Mineralization of BAG-Containing Resin Composite

This study aims at explores immersion solutions other than standard SBF that could evaluate mineralization of dental resin composites containing low percentage bioactive glass (BAG). Experimental UDMA/TEGDMA resin composites containing total 25 vol% glass fillers (with 0.0, 1.9, 3.8 or 7.7 vol% of 45S5 bioactive glass (BAG) fillers) were prepared. The specimens were immersed in three different solutions either with bicarbonate which are Hanks balanced salt solution (HBSS) and cell culture medium (MEM), or without bicarbonate which is a novel Simple HEPES-containing Artificial Remineralization Promotion (SHARP) solution, for 3, 7 and 14 days. These solutions were then analyzed by ICP-OES and pH, and the surfaces of the BAG composites were analyzed by SEM, XRD and FTIR. ICP-OES revealed Ca and P concentration continuously decrease, while Si concentration increases with time in all groups. Only SHARP solution is able to maintain a constant pH over the immersion time. SEM, together with XRD and FTIR, showed nano-sized octacalcium phosphate (OCP) nanospheres formation on 3.8 and 7.7 vol% BAG composites after 14 days immersion in HBSS (500-600 nm) and MEM (300-400 nm). SHARP solution enabled OCP formation after 3 days and then self-assembled into urchin-like carbonated hydroxyapatite (CHA) microspheres encompassed with nanorods of 100 nm width and 8 m length after 14 days of immersion for 7.7 vol% BAG composites. This study suggests the SHARP solution can evaluate mineralization biomimetically whereas CHA microspheres can be formed on BAG-containing resin composites.

A biomimetic approach to evaluate mineralization of bioactive glass-loaded resin composites.

This study explores novel solutions other than standard SBF for biomimetic evaluations of mineralization particularly for resin composites containing bioactive glass (BAG). Experimental UDMA/TEGDMA resin composites with 0.0, 1.9, 3.8 or 7.7 vol% of 45S5 BAG fillers were prepared. Besides simulated body fluid (SBF) as control, the specimens were immersed in three other solutions either with bicarbonate which are Hank's balanced salt solution (HBSS) and cell culture medium (MEM), or without bicarbonate which is a novel Simple HEPES-containing Artificial Remineralization Promotion (SHARP) solution, for 3, 7 and 14 days. These solutions were then analyzed by ICP-OES and pH meter, and the surfaces of the BAG composites were analyzed by SEM, XRD and FTIR. ICP-OES revealed Ca and P concentration continuously decrease, while Si concentration increases with time in the solutions other than SBF, which showed almost unchanged elemental concentration. Only SHARP solution is able to maintain a constant pH over the immersion time. SEM, together with XRD and FTIR, showed nano-sized octacalcium phosphate (OCP) nanospheres formation on 3.8 and 7.7 vol% BAG composites after 14 days immersion in HBSS (500-600 nm) and MEM (300-400 nm). SHARP solution enabled OCP formation after 3 days and then self-assembled into urchin-like carbonated hydroxyapatite (CHA) microspheres encompassed with nanorods of 100 nm width and 8 µm length after 14 days of immersion for 7.7 vol% BAG composites. This study suggests SHARP solution can evaluate mineralization biomimetically whereas CHA microspheres can be formed on BAG-containing resin composites.

Sacrificial protection of Mg-based resorbable implant alloy by magnetron sputtered Mg5Gd alloy coating: A short-term study

In this work metallic pins made of Mg5Gd alloy were coated with magnetron sputtered PVD Mg5Gd layers. Immersion tests in Hank’s balanced salt solution (HBSS) were performed. The PVD coating drastically reduced the corrosion rate of the Mg5Gd pin. The corrosion mechanism of the coating was studied in model electrochemical measurements by Scanning Vibrating Electrode Technique and galvanic current measurements. The tests revealed the preferential anodic dissolution of the Mg5Gd coating galvanically coupled with the bulk Mg5Gd pin. Local measurements of Volta potential difference revealed the VPD contrast between the pin and the coating surfaces only after immersion in HBSS.

Effect of Silver on the Apatite Formation of Bioactive Silicate Glass

Abstract Silver (Ag) has the antibacterial property and can be easily introduced in glasses and glass-ceramics. In this research, the effect of Ag addition on the apatite formation of sol-gel derived new composition bioactive glass (BG) (55%SiO2 - 4% P2O5 -22%Na2O - (19-x) %CaO -x% Ag2O) (x=0, 5 and 8%) were investigated. The synthesized Ag doped BG samples were treated in Hank's Balanced Salt Solution (HBSS) for 14 days to study the bioactivity. The achieved samples were evaluated by X-ray powder diffraction (XRD) and Scanning electron microscope (SEM). The XRD spectra clearly show diffraction peaks of bone-like hydroxyapatite (HAp) for all samples after immersion in HBSS. However, the more intense of HAp peak at 32° was detected in Ag(5%) and Ag(8%) BGs compared with undoped BG. All glass samples are bioactive but BG with 8 wt% of Ag2O exhibited more apatite than the samples containing 5 wt% of Ag2O, as seen in SEM images. After 14 days immersion, full coverage of apatite in cluster crystal form on the Ag(8) glass surface was observed.

Dependence of calcium phosphate formation on nanostructure of rutile TiO2(110) surfaces

To demonstrate the effect of the surface nanostructures on the osteoconductivity of titanium dioxide (TiO2), formation of calcium phosphate on the rutile TiO2(110) surfaces in Hanks’ balanced salt solution (HBSS) was examined using X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM) techniques. When the TiO2(110) surfaces annealed in air were immersed in HBSS, calcium phosphate particles were formed on the surface. The calcium phosphate formation was suppressed by further annealing of the surfaces in O2 before the immersion in HBSS. The suppression of calcium phosphate formation is attributed to the transformation of the topmost layer of the air-annealed TiO2(110) surface from amorphous to rutile. The arrangement of the phosphate ions adsorbed on the rutile (1 × 1) surface does not match the hydrogen phosphate ion lattice of the CaHPO4 sheet of brushite.

In Vitro Biodegradation and Mechanical Properties of Mg-Zn Alloy and Mg-Zn-Hydroxyapatite Composite Produced by Mechanical Alloying for Potential Application in Bone Repair

A biodegradable Mg-6.5 wt pct Zn (Mg-Zn) alloy and Mg-6.5 wt pct Zn reinforced with 10 wt pct hydroxyapatite (HA) composite were prepared by mechanical milling. In vitro biodegradation activity as a function of immersion time was performed in Hank’s balanced salt solution (HBSS). The dissolution of Mg ions (Mg2+) decreased from 75.74 µg/ml of pure Mg to 59.24 µg/ml and 46.88 µg/ml corresponding to the Mg-Zn alloy and Mg-Zn/HA composite, respectively. This finding indicates the progressive effect of HA followed by the Zn addition in decelerating the degradation rate of Mg. More positive corrosion potential of Mg-6.5 wt pct Zn alloy (− 1.5015 V) and Mg-Zn/10 wt pct HA composite (− 1.4647 V) than that of pure Mg (− 1.6972 V) suggested that the Mg-Zn/10 wt pct HA composite exhibited the highest corrosion resistance in the bioenvironment. The compressive strength values after 7 days of immersion in HBSS of the Mg-Zn alloy and Mg-Zn/HA composite are 230.64 and 278.46 MPa, respectively, and these are considerably higher compared to the compressive strength of the cortical bone (100 to 230 MPa).

Properties of NeoMTA Plus and MTA Plus cements for endodontics.

To test a novel calcium silicate cement mixed with a water-based gel (NeoMTA Plus) with regard to chemical-physical properties and apatite-forming ability. NeoMTA Plus (Avalon Biomed Inc. Bradenton, FL, USA; lot. 2014090301) and a commercial MTA-based material with similar properties (MTA Plus, Prevest Denpro Limited, Jammu, India; lot. 41001) were tested for ion-releasing ability, initial and final setting times, radiopacity, open and impervious porosity and apparent porosity, water sorption, weight loss, solubility, ability to nucleate calcium phosphates (CaP) after immersion in HBSS (Hank's Balanced Salt Solution) by ESEM-EDX and micro-Raman spectroscopy. The results were analysed statistically with the anova test (P < 0.05). NeoMTA Plus had a prolonged setting time (315min) and a satisfactory radiopacity (3.76mm Al). Calcium and hydroxyl ion release was significantly greater and more prolonged in comparison with MTA Plus (P<0.05). Both NeoMTA Plus and MTA Plus had high values of open porosity and solubility. ESEM-EDX and micro-Raman confirmed the ability to nucleate calcium phosphates on their surface after immersion in HBSS. NeoMTA Plus is a new calcium silicate-based cement for root filling with an adequate radiopacity and prolonged setting time. The ion release and CaP-forming ability could increase stability of the root filling and promote endodontic and periodontal tissue regeneration, enhancing the bioactivity and biocompatibility of the material.

In vitro biodegradable and mechanical performance of biphasic calcium phosphate porous scaffolds with unidirectional macro-pore structure

In this study, porous biphasic calcium phosphate (BCP) scaffolds were fabricated by a freeze–gel casting technique using a tertiary-butyl alcohol (TBA) based slurry. After sintering, unidirectional macropore channels of scaffolds aligned regularly along the TBA ice growth direction were tailored simultaneously with micropores formed in the outer wall of the pore channels. The synthesized porous BCP scaffolds (two different sintering temperatures) exhibit compressive strength of 46.8MPa for 43.0% porosity and 33.1MPa for 45.9% porosity, respectively. After immersion in Hank's balanced salt solution (HBSS) for 1, 2, 4, 8 weeks, a precipitation started to be formed with individual small granules on the scaffolds surface. In the case of BCP scaffolds sintered at 1200°C, β-TCP were slowly degraded with increasing the immersing time; on the other hand, α-TCP (from BCP scaffolds sintered at 1300°C) was extremely degraded within 1 week of immersing. This behavior could be due to a fast hydrolysis (dissolution–reprecipitation) as a phase transformation from α-TCP to brushite or apatite compared to the β-TCP. After immersion in HBSS, overall the compressive strength of the scaffolds reduced by the gradual degradation in biological environment solution. This behavior is consistent with the degradation behavior of scaffolds after immersion in HBSS.

Porosity and root dentine to material interface assessment of calcium silicate-based root-end filling materials

The aim of this study was to evaluate the porosity and assess the root dentine to material interface of four root-end filling materials based on tricalcium silicate cement using two microscopy techniques. The porosity of Bioaggregate, Biodentine, a prototype radiopacified tricalcium silicate cement (TCS-20-Zr) and intermediate restorative material (IRM) was evaluated after immersion for 28 days in Hank's balanced salt solution (HBSS) using mercury intrusion porosimetry. The root dentine to material interface of the cements when used as root-end filling materials in extracted human teeth was assessed after 28 days of dry storage and immersion in HBSS using a confocal microscope together with fluorescent tracers and also a field emission gun scanning electron microscope. Biodentine and IRM exhibited the lowest level or degree of porosity. The confocal microscopy used in conjunction to fluorescent tracers demonstrated that dry storage resulted in gaps at the root dentine to material interface and also cracks in the material with Biodentine being the most affected. Zinc was shown to be present in root dentine adjacent to the IRM restorations. Dry storage of Biodentine resulted in changes in the material microstructure and cracks at the root dentine to Biodentine interface. Furthermore, the gaps resulting from material shrinkage allowed the passage of the fluorescent microspheres thus indicating that these gaps are significant and can potentially allow the passage of micro-organisms.

Morphology andIn VitroBehavior of Electrospun Fibrous Poly(D,L-lactic acid) for Biomedical Applications

This work describes the fabrication, optimization, and characterization of electrospun fibrous poly(D,L-lactic acid) (PDLLA) for biomedical applications. The influences of the polymer concentration of the electrospinning solution (5, 10, or 15 wt%) and the solution flow rate (0.1, 0.5, 1.0, or 2.0 mL/h) on the morphology of the obtained fibrous PDLLA were evaluated. Thein vitrobiocompatibility of two types of PDLLA, ester terminated PDLLA (PDLLA-R) and carboxyl terminated PDLLA (PDLLA-COOH), was evaluated by monitoring apatite formation on samples immersed in Hanks’ balanced salt (HBS) solution. 15 wt% polymer solution was the most beneficial for preparing a fibrous PDLLA structure. Meanwhile, no differences in morphology were observed for PDLLA prepared at various flow rates. Apatite precipitate is formed on both types of PDLLA only 1 day after immersion in HBS solution. After 7 days of immersion, PDLLA-COOH showed greater apatite formation ability compared with that of PDLLA-R, as measured by thin-film X-ray diffraction. The results indicated that the carboxyl group is effective for apatite precipitation in the body environment.

The chemical properties of light- and chemical-curing composites with mineral trioxide aggregate filler

ObjectiveOne of the challenges encountered with composite restorations is their inability to prevent secondary caries. Alternative fillers that initiate remineralization have been proposed but poor mechanical strength limits their use to lining and support materials. Mineral trioxide aggregate (MTA) is a material with many dental applications including root-end filling and pulp capping. MTA is capable of encouraging remineralization by leaching calcium in solution, and has the ability to form apatite in physiological solution. The aim of this study was to characterize and investigate the chemical properties of MTA-filled composite resins. MethodsComposite resins composed of light-cured (Heliobond) and chemical-cured (Superbond) dental resins filled with MTA Plus (MTA-Light, MTA-Chem) respectively, and MTA Plus mixed with water (MTA-W), were investigated. Un-hydrated and set materials were characterized by scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, X-ray diffraction (XRD) analysis and Fourier transform infrared (FT-IR) spectroscopy after being stored dry or immersed in Hank's balanced salt solution (HBSS). The chemical properties of the set materials were then investigated. ResultsXRD and FT-IR analyses revealed that MTA powder remains unhydrated within the composite, even after 28 days of immersion in HBSS. Furthermore neither resin appeared to chemically react with the MTA. EDX revealed minimal diffusion of bismuth oxide through the polymer network. Apatite formation on the material surfaces was demonstrated by SEM. Significantly less apatite deposition was exhibited on the composites compared to MTA-W. All materials leached calcium and produced an alkaline pH in physiological solution. The pH at 28 days was: MTA-W 12.7, MTA-Light 11.4, and MTA-Chem 10.8. Calcium ion concentration followed the same trend, with MTA-W>MTA-Light>MTA-Chem. SignificanceThe novel composites exhibited calcium ion release, alkalinizing pH and formation of apatite, although in each case not as strongly as the control (MTA-W). MTA-Chem fared less favorably than MTA-Light in these aspects. Thus they are recommended for applications where bioactivity is desirable but not critical, and only they have a significant advantage over ordinary MTA in some other aspect.

3D micro‐CT analysis of the interface voids associated with Thermafil root fillings used with AH Plus or a flowable MTA sealer

To investigate nondestructively the percentage of 3D voids and marginal gaps in a pre-defined interface volume of interest (VOI) within root fillings produced by Thermafil Obturators with either a hydrophobic epoxy-resin-based sealer (AH Plus) or a hydrophilic flowable calcium-silicate sealer [mineral trioxide aggregate (MTA) Flow]. Sixteen single root canals from extracted premolar teeth were prepared with ProTaper rotary instruments, randomly allocated into two groups (n = 8) and filled with size 30 Thermafil Obturators in association with AH Plus or MTA Flow sealers. The filled roots were stored at 37 °C in 5 mL of Hank's balanced salt solution (HBSS) used to represent body fluids and scanned after 7 days and 6 months using a high-resolution micro-CT. From each root, images of 3000 sections were analysed in 3D and binarized using a high-resolution micro-CT (4-μ resolution). The 3D distribution of voids (porosity and marginal gaps) at the gutta-percha-sealer-dentine interface was detected through a threshold grey level and expressed as percentage of the 40-μ-thick pre-defined interface VOI (20 μ of interface dentine and 20 μ of gutta-percha/sealer). A method of analysis based on the root canal segmentation was used, and coronal, middle and apical thirds considered separately. The percentage of 3D void volume was compared statistically using one-way anova (significance for P < 0.05). Environmental Scanning Electron Microscope with Energy Dispersive X-ray (ESEM-EDX) analysis was performed on the surface of both sealers after soaking in HBSS. Micro-CT detected gaps at the dentine-sealer interface in both groups. Void volumes wider than 10.21 μm(3) with 1.35 μm diameter were detected. Cul-de-sac-type voids (blind pores) and through-and-through voids (continuous pores) were discriminated. The apical thirds had a significantly lower 3D void volume (P < 0.05) than the middle and coronal thirds. The 3D void volume reduced significantly (P < 0.05) over time. ESEM-EDX analysis revealed that MTA Flow sealer created a dense apatite layer after 7 days of immersion in HBSS, whilst only sparse calcium phosphate deposits were detected on AH Plus even after 28 days. Micro-CT proved to be a powerful nondestructive 3D analysis tool for visualizing the porous internal microstructure of dental/endodontic materials at the interface with dentine. The proportion of voids was least in the apical third of root canals. Voids reduced over time in the presence of simulated body fluid.

In situ synthesis of magnesium-substituted biphasic calcium phosphate and in vitro biodegradation

In situ preparation of magnesium (Mg) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added magnesium were varied with the calcium in order to obtain constant (Ca+Mg)/P ratios of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized magnesium substituted BCP powders. The results have shown that substitution of magnesium in the calcium deficient apatites revealed the formation of biphasic mixtures of different HAp/β-TCP ratios after heating at 1000°C. The ratios of the formation of phase mixtures were dependent on the content of magnesium. After immersing in Hanks’ balanced salt solution (HBSS) for 1 week, 1wt% magnesium substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. On the other hand, in the case of pure BCP powders, the formation of new precipitates was detected after immersion in HBSS for 2 weeks. On the basis of these results, magnesium substituted BCP could be able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. In addition, the retention time to produce the new apatite phase in implantation operation for the BCP powder could be controlled by the amount of magnesium substitution.

The microstructure and surface morphology of radiopaque tricalcium silicate cement exposed to different curing conditions

ObjectiveTricalcium silicate is the major constituent phase in mineral trioxide aggregate (MTA). It is thus postulated that pure tricalcium silicate can replace the Portland cement component of MTA. The aim of this research was to evaluate the microstructure and surface characteristics of radiopaque tricalcium silicate cement exposed to different curing conditions namely at 100% humidity or immersed in either water or a simulated body fluid at 37°C. MethodsThe materials under study included tricalcium silicate and Portland cements with and without the addition of bismuth oxide radiopacifier. Material characterization was performed on hydrated cements using a combination of scanning electron microscopy (SEM) with X-ray energy dispersive (EDX) analyses and X-ray diffraction (XRD) analyses. Surface morphology was further investigated using optical profilometry. Testing was performed on cements cured at 100% humidity or immersed in either water or Hank's balanced salt solution (HBSS) for 1 and 28 days at 37°C. In addition leachate analysis was performed by X-ray fluorescence of the storage solution. The pH of the storage solution was assessed. ResultsAll the cements produced calcium silicate hydrate and calcium hydroxide on hydration. Tricalcium silicate showed a higher reaction rate than Portland cement and addition of bismuth oxide seemed to also increase the rate of reaction with more calcium silicate hydrate and calcium hydroxide being produced as demonstrated by SEM and XRD analysis and also by surface deposits viewed by the optical profilometer. Cement immersion in HBSS resulted in the deposition of calcium phosphate during the early stages following immersion and extensive calcification after 28 days. The pH of all storage solutions was alkaline. The immersion in distilled water resulted in a higher pH of the solution than when the cements were immersed in HBSS. Leachate analysis demonstrated high calcium levels in all cements tested with higher levels in tricalcium silicate and bismuth replaced cements. SignificanceTricalcium silicate cement is more bioactive than Portland cement as demonstrated by various characterization techniques. The bioactivity was monitored by measuring the production of calcium hydroxide and the formation of calcium phosphate when in contact with simulated body fluids.

In situ synthesis of silicon-substituted biphasic calcium phosphate and their performance in vitro

In situ preparation of silicon (Si) substituted biphasic calcium phosphate (BCP) of hydroxyapatite (HAp)/ β-tricalcium phosphate (β-TCP) were carried out through aqueous co-precipitation method. The concentrations of added silicon were varied with the phosphor in order to obtain constant Ca/(P+Si) ratios of 1.602. X-ray diffraction (XRD) and Fourier transformed infrared (FTIR) spectroscopy were used to characterize the structure of synthesized silicon substituted BCP powders. The characterization revealed that the formation of biphasic mixtures of different HAp/ β-TCP ratios was dependent on the content of silicon. After immersing in Hanks' balanced salt solution (HBSS) for 1 week, 3 wt% silicon substituted BCP powders were degraded and precipitation started to be formed with small granules consisting of number of flake-like crystal onto the surface of synthesized powders. In the case of 1 wt% silicon substituted BCP powders, the degradation behavior was detected after immersion in HBSS for 3 weeks. On the other hand, silicon unsubtituted BCP powders were not degraded even after that duration. On the basis of these results, silicon substituted BCP is able to develop a new apatite phase on the surface in contact with physiological fluids faster than BCP does. This enhanced reactivity resulted in reduction for the stability of the β-TCP structure due to SiO 4 tetrahedral distortion and disorder at the hydroxyl site when silicon incorporates into BCP.

Characterization of the surface deposition on anodized-hydrothermally treated commercially pure titanium after immersion in simulated body fluid

The interface phenomena between anodized-hydrothermally treated commercially pure titanium (SA-treated c.p.Ti) endosseous implants and biological tissue are important in osseous wound healing. Therefore purpose of this study was to characterize the morphological, structural and chemical features of SA-treated c.p.Ti surfaces after immersion in Hanks' balanced salt solution (HBSS). Anodic oxide (AO) c.p.Ti and SA-treated c.p.Ti disks were immersed for 14 and 28 days in HBSS (37 degrees C, pH 7.4). These samples were analyzed by X-ray photoelectron spectroscopy, X-ray diffraction, scanning electron microscopy, electron probe microanalyzer, and ion chromatography. X-ray photoelectron spectroscopy and X-ray diffraction patterns were similar in each sample before and after HBSS immersion. Scanning electron microscopy performed after 28 days immersion in HBSS revealed deposits completely covering SA-treated c.p.Ti. However, deposits were not observed on AO c.p.Ti after 14 or 28 days immersion. Electron probe microanalyzer results revealed an even distribution of calcium and phosphorus on SA-treated c.p.Ti after 28 days immersion, however there was no change in AO c.p.Ti disks during all immersion periods. Ion chromatography showed increased levels of calcium and phosphorus on SA-treated c.p.Ti disks compared to AO c.p.Ti disks, after 28 days immersion. The results indicate that the deposits formed on SA-treated c.p.Ti surfaces contained calcium phosphate. These deposits may be formed as a consequence of the topography and physicochemical properties of SA-treated c.p.Ti surfaces and may play a key role in osteoconduction during osseous wound healing.