Influence of setting liquid composition and liquid-to-powder ratio on properties of a Mg-substituted calcium phosphate cement

The influence of four variables on various properties of a Mg-substituted calcium phosphate cement (CPC) was investigated. The variables were the heat treatment temperature of the precipitated powders, the composition of the setting liquid, the liquid-to-powder ratio (LPR), and the time over which hardened specimens were cured in air. The properties analysed were the phase composition of the starting powder, the initial setting time, the evolution of the storage shear modulus (G′) and the loss shear modulus (G″) with the cement paste curing time (t), and the compressive strength. The presence of α-TCP in CPC facilitated the setting and hardening properties due to its progressive dissolution and the formation of brushite crystals. As far as the liquid composition is concerned, in cases where citric acid was used, adding a rheology modifier (10 wt.% polyethylene glycol or 0.5 wt.% hydroxyl propylmethylcellulose) to the acid led to an increase in the initial setting time, while an increase in the acid concentration led to a decrease in the initial setting time. The initial setting time showed to be very sensitive towards the LPR. The evolution of G′ and G″ with curing time reflected the internal structural changes of cement pastes during the setting process. The compressive strength of the wet-hardened cement specimens with and without Mg increased with curing time increasing, being slightly higher in the case of Mg-substituted CPC. The results suggest that Mg-substituted CPC holds a promise for uses in orthopaedic and trauma surgery such as for filling bone defects.     

Measurement of Poisson's ratio of dental composite restorative materials

The aim of this study was to determine the Poisson ratio of resin-based dental composites using a static tensile test method. Materials used in this investigation were from the same manufacturer (3M ESPE) and included microfill (A110), minifill (Z100 and Filtek Z250), polyacid-modified (F2000), and flowable (Filtek Flowable [FF]) composites. The Poisson ratio of the materials were determined after 1 week conditioning in water at 37 degrees C. The tensile test was performed with using a uniaxial testing system at crosshead speed of 0.5 mm/min. Data was analysed using one-way ANOVA/post-hoc Scheffe's test and Pearson's correlation test at significance level of 0.05. Mean Poisson's ratio (n=8) ranged from 0.302 to 0.393. The Poisson ratio of FF was significantly higher than all other composites evaluated, and the Poisson ratio of A110 was higher than Z100, Z250 and F2000. The Poisson ratio is higher for materials with lower filler volume fraction.     

Synthesis of a proline-modified acrylic acid copolymer in supercritical CO2 for glass-ionomer dental cement applications

Supercritical (sc-) fluids (such as sc-CO₂) represent interesting media for the synthesis of polymers in dental and biomedical applications. Sc-CO₂ has several advantages for polymerization reactions in comparison to conventional organic solvents. It has several advantages in comparison to conventional polymerization solvents, such as enhanced kinetics, being less harmful to the environment and simplified solvent removal process. In our previous work, we synthesized poly(acrylic acid-co-itaconic acid-co-N-vinylpyrrolidone) (PAA-IA-NVP) terpolymers in a supercritical CO₂/methanol mixture for applications in glass-ionomer dental cements. In this study, proline-containing acrylic acid copolymers were synthesized, in a supercritical CO₂ mixture or in water. Subsequently, the synthesized polymers were used in commercially available glass-ionomer cement formulations (Fuji IX commercial GIC). Mechanical strength (compressive strength (CS), diametral tensile strength (DTS) and biaxial flexural strength (BFS)) and handling properties (working and setting time) of the resulting modified cements were evaluated. It was found that the polymerization reaction in an sc-CO₂/methanol mixture was significantly faster than the corresponding polymerization reaction in water and the purification procedures were simpler for the former. Furthermore, glass-ionomer cement samples made from the terpolymer prepared in sc-CO₂/methanol exhibited higher CS and DTS and comparable BFS compared to the same polymer synthesized in water. The working properties of glass-ionomer formulations made in sc-CO₂/methanol were comparable and better than the values of those for polymers synthesized in water.     

Influence of the modification of P/L ratio on a new formulation of acrylic bone cement

The use of smaller powder/liquid (P/L) ratio favours the handling and wetting of poly(methyl methacrylate) (PMMA) beads in bone cement formulations. In this paper a P/L ratio of 1.86 is tested to overcome adhesion problems found in hydroxypropyl methacrylate (HPMA) modified bone cements and the influence on bone cement characteristics was analysed. The reduction of the P/L ratio leads to higher temperature peaks and shorter setting times, whereas the residual monomer content increases slightly. Water uptake obeys the diffusion laws, and the introduction of a more hydrophilic monomer gives rise to an increase of this parameter, which does not present significant changes with modification of the P/L ratio. Polymerization shrinkage is slightly greater because of the introduction of higher proportions of monomer in the formulation. Mechanical properties are similar to those obtained with conventional P/L ratios. The analysis of scanning electron microscopy (SEM) reveals an improvement of the adhesion between phases with respect to P/L = 2 formulations.     

Biphenyl liquid crystalline epoxy resin as a low-shrinkage resin-based dental restorative nanocomposite

Low-shrinkage resin-based photocurable liquid crystalline epoxy nanocomposite has been investigated with regard to its application as a dental restoration material. The nanocomposite consists of an organic matrix and an inorganic reinforcing filler. The organic matrix is made of liquid crystalline biphenyl epoxy resin (BP), an epoxy resin consisting of cyclohexylmethyl-3,4-epoxycyclohexanecarboxylate (ECH), the photoinitiator 4-octylphenyl phenyliodonium hexafluoroantimonate and the photosensitizer champhorquinone. The inorganic filler is silica nanoparticles (～70–100 nm). The nanoparticles were modified by an epoxy silane of γ-glycidoxypropyltrimethoxysilane to be compatible with the organic matrix and to chemically bond with the organic matrix after photo curing. By incorporating the BP liquid crystalline (LC) epoxy resin into conventional ECH epoxy resin, the nanocomposite has improved hardness, flexural modulus, water absorption and coefficient of thermal expansion. Although the incorporation of silica filler may dilute the reinforcing effect of crystalline BP, a high silica filler content (～42 vol.%) was found to increase the physical and chemical properties of the nanocomposite due to the formation of unique microstructures. The microstructure of nanoparticle embedded layers was observed in the nanocomposite using scanning and transmission electron microscopy. This unique microstructure indicates that the crystalline BP and nanoparticles support each other and result in outstanding mechanical properties. The crystalline BP in the LC epoxy resin-based nanocomposite was partially melted during exothermic photopolymerization, and the resin expanded via an order-to-disorder transition. Thus, the post-gelation shrinkage of the LC epoxy resin-based nanocomposite is greatly reduced, ～50.6% less than in commercialized methacrylate resin-based composites. This LC epoxy nanocomposite demonstrates good physical and chemical properties and good biocompatibility, comparable to commercialized composites. The results indicate that this novel LC nanocomposite is worthy of development and has potential for further applications in clinical dentistry.     

Influence of mixing techniques on the physical properties of acrylic bone cement

Palacos R bone cement was prepared using three commercially available mixing techniques, first generation, second generation and third generation, to determine the mechanical properties and porosity contents of the bone cement. The compressive strengths, bending strengths and flexural moduli were expressed as a function of void content. The volume of pores within the cement structure was found to be a contributing factor to the physical properties of acrylic bone cement. The lower the volume of voids in the cement the better the compressive and flexural properties, hence stronger bone cement. It was found that the best results were obtained from cement that had been mixed using the Mitab Optivac or Summit HiVac Syringe systems at a reduced pressure level of between -72 and -86 kPa below atmospheric pressure, resulting in cement of porosity 1.44-3.17%; compressive strength 74-81 MPa; flexural modulus 2.54-2.60 GPa; and flexural strength 65-73 MPa.     

Influence of mixing technique on some properties of PMMA bone cement

PMMA bone cements (Refobacin-Palacos R, Sulfix 6, AKZ, and CMW bone cement, types I and II), from six different clinics, were investigated in three stages. In the first stage, studies of density, hardness, flexural strength, and compressive strength were made, as well as molecular weight measurements and microscopic investigations. These studies reflected the current state of techniques of application used in operating theaters. They revealed wide variations in the properties of the materials studied. Secondly, a comprehensive study of the process-technology in the laboratory was performed. The following variables were investigated or discussed: mixing vessel, order of the individual components, mixing time, rate of mixing, pressure application on the mixed bone cement, kneading, cement thickness, pouring into the syringe, contact force during polymerization, and preparation quantity. The third stage involved the development and clinical testing of an improved mixing technique. Using this improved mixing technique, all three selected clinics achieved far better results with reduced variability. A comparison between a centrifuging technique after mixing and our improved, but conventional, mixing technique, displays advantages for the latter. The question regarding a correlation between cement specimens of high porosity and early implant loosening could not be answered on the basis of the 43 PMMA bone cement explants investigated (implanted 6 months to 15 years). In some cases, the studies revealed that the bone cement manufacturers should be required to revise and quantify existing instructions for use. The users, on the other hand, should give more consideration to the mixing technique and its consequences.     

Dental polyelectrolyte cements: II: Effect of powder/liquid ratio on their rheology

The Theological behaviour during the setting of a range of zinc polycarboxylate and glass ionomer dental cements has been studied. The influence of the powder/liquid ratio was found to alter the rate of reaction without altering the basic form of the kinetics. Two models were advanced to explain the rheological and chemical differences between the two types of polyelectrolyte cement. The setting of the glass ionomer cements was consistent with the development of a homogeneous polymer network whereas the zinc polycarboxylate cements were viewed as setting by an inhomogeneous core-growth reaction.     

Glass ceramic approach to controlling the properties of a glass-ionomer bone cement

Glass-ionomer dental cements have potential as bone cements in joint replacement surgery. However, commercially available glasses used in dental cements suffer from the loss of fluorine during the melting procedure and from phase separation of the glass upon quenching, giving rise to inter- and intra-batch variation. A model glass was examined in which minimal loss of fluorine is observed. This results in a glass whose composition is reproducible between batches. This glass will crystallize both above and below the glass transition temperature following heat treatments. Cements can be produced whose properties vary with the degree of crystallinity of the glass-ceramic. A commercial glass was also examined and was found to crystallize to an apatite phase.     

The release of fluoride and other chemical species from a glass-ionomer cement

The elution of fluoride, sodium and silica from a glass-ionomer cement was studied for 598 days. It was found that these species were still being released when the experiments were concluded, however, the rate of release was much diminished. The release of fluoride, sodium and silica was incongruent. Only fluoride associated with sodium appeared to be available for release.     

The effect of oxalic acid incorporation on the setting time and strength of a glass-ionomer cement

Oxalic acid and its metal oxalate salts have been used extensively in dentistry in a range of applications: as desensitisers, in cavity preparation, and as bonding agents. This study investigated the influence of oxalic acid upon the working time, initial setting time, 24-h hardness and compressive strength of a glass-ionomer cement. Conventional glass-ionomer liquids were prepared from polyacrylic acid, tartaric acid, water, and oxalic acid at concentrations of 0-7% w/w. Liquids were dosed into capsules with a commercial glass-ionomer powder, activated and mixed. The resultant pastes were assessed for working time, initial setting time, 24-h hardness and 24-h compressive strength. Liquids containing 0.5-1% oxalic acid lengthened the working time and initial setting time. At concentrations greater than 2%, both working and initial setting times decreased with increasing oxalic acid. Surface hardness values using liquids with 3% and 7% oxalic acid were less hard than the control. Compressive strength was unchanged over the concentrations tested. Oxalic acid may be a useful reaction modifier in glass-ionomer systems. It accelerated the setting reaction without affecting strength, but was limited to low concentrations because of its relatively poor solubility in water.     

Demineralization and ion binding action of polycarboxylate cement liquid on human dental enamel

The demineralization and ion binding effects on dental tissues due to poly(acrylic) acid attack under different dilution conditions of the latter are studied by scanning electron microscope (SEM) and infrared (IR) spectroscopy. The results indicate that in addition to the general demineralization effects such as preferential prism core attack, prism periphery attack, and protruding prism rods, competing ion binding effects also occur. Using optimum dilution conditions, the microstructural effects of demineralization and ion binding are shown and the effects are related to IR spectral observations.     

Influence of the method of blending an antibiotic powder with an acrylic bone cement powder on physical, mechanical, and thermal properties of the cured cement

Two variants of antibiotic powder-loaded acrylic bone cements (APLBCs) are widely used in primary total joint replacements. In the United States, the antibiotic is manually blended with the powder of the cement at the start of the procedure, while, in Europe, pre-packaged commercially-available APLBCs (in which the blending is carried out using an industrial mixer) are used. Our objective was to investigate the influence of the method of blending gentamicin sulphate with the powder of the Cemex XL formulation on a wide collection of properties of the cured cement. The blending methods used were manual mixing (the MANUAL Set), use of a small-scale, easy-to-use, commercially-available mechanical powder mixer, OmoMix 1 (the MECHANICAL Set), and use of a large-scale industrial mixer (Cemex Genta) [the INDUSTRIAL Set]. In the MECHANICAL and MANUAL Sets, the blending time was 3 min. In preparing the test specimens for each set, the blended powder used contained 4.22 wt% of the gentamicin powder. The properties determined were the strength, modulus, and work-to-fracture (all obtained under four-point bending), plane-strain fracture toughness, Weibull mean fatigue life (fatigue conditions: +/-15 MPa; 2 Hz), activation energy and frequency factor for the cement polymerization process (both determined using differential scanning calorimetry, at heating rates of 5, 10, 15, and 20 Kmin(-1)), the diffusion coefficient for the absorption of phosphate buffered saline, PBS, at 37 degrees C, and the rate of elution of the gentamicin into PBS, at 37 degrees C (E). Also determined were the particle size, particle size distribution, and morphology of the blended powders and of the gentamicin. For each of the cured cement properties (except for E), there is no statistically significant difference between the means for the 3 cements, a finding that parallels the observation that there are no significant differences in either the mean particle size or the morphology of the blended cement powders. Notwithstanding these results, it is suggested that when the powder mixture is blended in the operating room, using the OmoMix 1 is more likely to produce a more consistent and reproducible mixture than when manual mixing is used.     

Transmittance of a bioceramic dental restorative material based on calcium aluminate

This article investigates the transmittance of a new ceramic filling material as a function of time, thickness, wavelength, and addition of pigments. In the hardened state the ceramic material is composed of hydrates, calcium aluminate, and glass fillers. The radiopacity of the investigated material is also measured. The results of the transmittance are compared to a commercial glass ionomer cement (Fuji II) and resin composite (Tetric Ceram). The transmittance increased with time from low values after 1 h to values close to the glass ionomer cements after 1 week. The resin composite had almost twice the transmittance as the calcium aluminate material and the glass ionomer cement. The amount of light passing through the material was dependent on both the sample thickness and the wavelength. Samples of 0.5-mm thickness transmitted almost twice as much as 1-mm-thick samples. Regarding the wavelength, blue light was scattered very effectively (low transmittance), whereas red light was not (high transmittance). Addition of pigments lowered the transmittance. The radiopacity was slightly higher than that of enamel.     

An evaluation of accelerated Portland cement as a restorative material

Biocompatibility of two variants of accelerated Portland cement (APC) were investigated in vitro by observing the cytomorphology of SaOS-2 osteosarcoma cells in the presence of test materials and the effect of these materials on the expression of markers of bone remodelling. Glass ionomer cement (GIC), mineral trioxide aggregate (MTA) and unmodified Portland cement (RC) were used for comparison. A direct contact assay was undertaken in four samples of each test material, collected at 12, 24, 48 and 72 h. Cell morphology was observed using scanning electron microscopy (SEM) and scored. Culture media were collected for cytokine quantification using enzyme-linked immunosorbent assay (ELISA). On SEM evaluation, healthy SaOS-2 cells were found adhering onto the surfaces of APC variant, RC and MTA. In contrast, rounded and dying cells were observed on GIC. Using ELISA, levels of interleukin (IL)-1beta, IL-6, IL-18 and OC were significantly higher in APC variants compared with controls and GIC (p<0.01), but these levels of cytokines were not statistically significant compared with MTA. The results of this study provide evidence that both APC variants are non-toxic and may have potential to promote bone healing. Further development of APC is indicated to produce a viable dental restorative material and possibly a material for orthopaedic     

Relative roles of cement molecular weight and mixing method on the fatigue performance of acrylic bone cement: Simplex P versus Osteopal

The weight-average molecular weight (MW(w)) of a cement and the method used to mix its powder and liquid monomer constituents have been identified in the literature as key variables that affect mechanical properties of the fully polymerized cement that are relevant to its performance as a grouting agent in cemented arthroplasties. The goal of the present work was to identify which of these two variables exerts the greater effect in the case of fully reversed tension-compression fatigue performance. A judicious choice of cement brands, Surgical Simplex P and Osteopal, and the use of hand versus vacuum mixing, permitted this identification to be achieved. Three key observations were made in this work. First, for a given cement, the fatigue performance of vacuum-mixed specimens is far superior to that of hand-mixed ones, which may be a consequence of the substantially lower percentage areal porosity of the former specimens. Second, regardless of the mixing method, the fatigue performance of Osteopal outstrips that of Simplex P, a result that is attributed to the much higher MW(w) of the former cement. Third, hand-mixed Osteopal outperforms vacuum-mixed Simplex P (especially at low alternating stress levels), indicating that MW(w) of a bone cement is more influential than mixing method on its fatigue performance.     

Effect of two variables on the fatigue performance of acrylic bone cement: mixing method and viscosity

The goal of the present work was to establish the relative influence of one exogenous variable versus one endogenous variable on the fully-reversed tension-compression fatigue performance of bone cement. The method used to mix the cement constituents was the exogenous variable, while the viscosity of the mixed cement dough was the endogenous variable. Two commercial cement formulations (Palacos R and Osteopal) and two cement mixing methods (hand mixing and vacuum mixing) were used. It was found that for a given mixing method, cement viscosity exerts a marginal influence on fatigue performance. On the other hand, for a given cement formulation, vacuum mixing led to a statistically significant improvement in fatigue performance. The present results demonstrate the superior influence of mixing method over cement viscosity.     

Metal-oxide nanoparticles for the reinforcement of dental restorative resins

Metal oxide nanoparticles were synthesized from tantalum ethoxide and zirconium isopropoxide and subsequently surface grafted with vinyl silane and silyl methacrylate coupling agents. The nanoparticles were then dispersed into a commercial dental resin, and the composite was photocured into rigid three-point bend and fracture toughness specimens. The optically transparent/translucent cured composites demonstrated strength, toughness, and elastic modulus inferior to the unfilled material. Therefore, modifications in surface functionalization are being made to improve coupling and reduce interparticle associations.     

Influence of Charnley hip neck-angle inclination on the stresses at stem/cement and bone/cement interfaces

The present work aims to elucidate the influence of neck-stem angle inclination on the principal normal and shear stress distributions and values along the interfaces of the stem/cement and bone/cement in a cemented Charnley curved back femoral component. The same stresses were also examined for the intact bone that was considered as a reference for the obtained results. The interface is considered the weakest link in the structure and its endurance limit to failure is much less than the limit of the adjacent materials. Interface loading is by far the influential aspect governing the induced interface stresses in femoral total hip replacement. Therefore, higher values and nonuniform distribution of stresses at the interface may lead to loosening and crack initiation and propagation that usually precede the stem fracture.     

Influence of muscle strength to weight ratio on functional task performance

Existing models of muscle deconditioning such as bed rest are expensive and time-consuming. We propose a new model utilizing a weighted suit to manipulate muscle strength, power, or endurance relative to body weight. The aims of the study were to determine as to which muscle measures best predict functional task performance and to determine muscle performance thresholds below which task performance is impaired. Twenty subjects performed seven occupational astronaut tasks (supine and upright seat egress and walk, rise from fall, hatch opening, ladder climb, object carry, and construction board activity), while wearing a suit weighted with 0–120 % of body weight. Models of the relationship between muscle function/body weight and task completion time were developed using fractional polynomial regression and verified with pre- and post-flight astronaut performance data. Spline regression was used to identify muscle function thresholds for each task. Upright seat egress and walk was the most difficult task according to the spline regression analysis thresholds. Thresholds normalized to body weight were 17.8 N/kg for leg press isometric force, 17.6 W/kg for leg press power, 78.8 J/kg for leg press work, 5.9 N/kg isometric knee extension and 1.9 Nm/kg isokinetic knee extension torque. Leg press maximal isometric force/body weight was the most reliable measure for modeling performance of ambulatory tasks. Laboratory-based manipulation of relative strength has promise as an analog for spaceflight-induced loss of muscle function. Muscle performance values normalized to body weight can be used to predict occupational task performance and to establish relevant strength thresholds.