Percorrer por autor "Young, Anne M."
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- Determination of dental adhesive composition throughout solvent drying and polymerization using ATR–FTIR spectroscopyPublication . Almusa, Arwa; Delgado, António H. S.; Ashley, Paul; Young, Anne M.The of this study aim was to develop a rapid method to determine the chemical composition, solvent evaporation rates, and polymerization kinetics of dental adhesives. Single-component, acetone-containing adhesives One-Step (OS; Bisco, Anaheim, CA, USA), Optibond Universal (OU; Kerr, Brea, CA, USA), and G-Bond (GB; GC, Tokyo, Japan) were studied. Filler levels were determined gravimetrically. Monomers and solvents were quantified by comparing their pure Attenuated Total Reflectance-Fourier Transform Infra-Red (ATR–FTIR) spectra, summed in different ratios, with those of the adhesives. Spectral changes at 37 °C, throughout passive evaporation for 5 min, then polymerisation initiated by 20 s, and blue light emitting diode (LED) (600 mW/cm2) exposure (n = 3) were determined. Evaporation and polymerisation extent versus time and final changes were calculated using acetone (1360 cm−1) and methacrylate (1320 cm−1) peaks. OS, OU, and GB filler contents were 0, 9.6, and 5.3%. FTIR suggested OS and OU were Bis-GMA based, GB was urethane dimethacrylate (UDMA) based, and that each had a different diluent and acidic monomers and possible UDMA/acetone interactions. Furthermore, initial acetone percentages were all 40–50%. After 5 min drying, they were 0% for OS and OU but 10% for GB. Whilst OS had no water, that in OU declined from 18 to 10% and in GB from 25 to 20% upon drying. Evaporation extents were 50% of final levels at 23, 25, and 113 s for OS, OU, and GB, respectively. Polymerisation extents were all 50 and 80% of final levels before 10 and at 20 s of light exposure, respectively. Final monomer polymerisation levels were 68, 69, and 88% for OS, OU, and GB, respectively. An appreciation of initial and final adhesive chemistry is important for understanding the properties. The rates of evaporation and polymerisation provide indications of relative required drying and light cure times. UDMA/acetone interactions might explain the considerably greater drying time of GB.
- Methacrylate peak determination and selection recommendations using ATR-FTIR to investigate polymerisation of dental methacrylate mixturesPublication . Delgado, António H. S.; Young, Anne M.Investigation of polymerisation kinetics using ATR-FTIR systems is common in many dental studies. However, peak selection methods to calculate monomer-polymer conversion can vary, consequently affecting final results. Thus, the aim of this study is to experimentally confirm which method is less prone to systematic errors. Three commercial restorative materials were tested–Vertise Flow (VF), Constic and Activa Bioactive Restorative Kids. Firstly, Attenuated Total Reflectance Fourier Transform Infra-Red (ATR-FTIR) (Spectrum One, Perkin-Elmer, UK) spectra of monomers were acquired—10-methacryloyloxy decyl dihydrogen phosphate (10-MDP), bisphenol-A glycidyl dimethacrylate (Bis-GMA), 2-hydroxyethyl methacrylate (HEMA), triethyelene glycol dimethacrylate (TEGDMA) and urethane dimethacrylate (UDMA) to investigate proportionality of methacrylate peak heights versus concentration. Spectral changes upon light exposure of 2 mm discs of the restorative materials (irradiated for 20 s, LED curing unit 1100–1330 mW/cm2) were assessed to study polymerisation kinetics (n = 3), with continuous acquisition of spectra, before, during and after light exposure. Peak differences and degrees of conversion (DC %) were calculated using 1320/1336, 1320/1350 and 1636/1648 cm-1 as reaction/reference peaks. Inferential statistics included a MANOVA and within-subjects repeated measures ANOVA design (5% significance level). Proportionality of methacrylate peak height to concentration was confirmed, with the 1320/1352 cm-1 peak combination showing the lowest coefficient of variation (8%). Difference spectra of the polymerisation reaction showed noise interference around the 1500–1800 cm-1 region. Across the different materials, DC % results are highly dependent upon peak selection (p<0.001), with higher variability associated to the 1636 cm-1. Significant differences in the materials were only detected when the 1320 cm-1 peak was used (p<0.05). Within the same materials, methods were significantly different for Constic and Activa (p<0.05). It is possible to conclude that the 1320 cm-1 peak is more adequate to assess polymerisation of methacrylates and is therefore recommended.
- Modelling ATR-FTIR spectra of dental bonding systems to investigate composition and polymerisation kineticsPublication . Delgado, António H. S.; Young, Anne M.Component ratios and kinetics are key to understanding and optimising novel formulations. This warrants investigation of valid methods. Attenuated Total Reflectance Fourier Transform Infra-Red (ATR)-FTIR spectra of separate primers/adhesives were modelled using summed spectra of solvents (water, ethanol), methacrylate monomers (HEMA (hydroxyethyl methacrylate), Bis-GMA (bisphenol A glycidyl methacrylate), and 10-MDP (10-methacryloyloxydecyl dihydrogen phosphate)), and fillers, multiplied by varying fractions. Filler loads were obtained following their separation from the adhesives, by analysing three repetitions (n = 3). Spectral changes during light exposure at 37 °C (20 s, LED 1100–1330 mW/cm2) were used to determine polymerisation kinetics (n = 3). Independent samples T-test was used for statistical analysis (significance level of 5%). FTIR modelling suggested a primer solvent percentage of OBFL (Optibond FL) (30%) was half that of CFSE (Clearfil SE 2) (60%). OBFL included ethanol and water, while CFSE included only water. Monomer peaks were largely those of HEMA with lower levels of phosphate monomers. OBFL/CFSE adhesive model spectra suggested that both contained equal volumes of Bis-GMA/HEMA, with CFSE having 10-MDP. Filler levels and spectra from OBFL (48 wt.%) and CFSE (5 wt.%) were different. Both systems reached a 50% conversion rate within seconds of light exposure. The final conversion for OBFL (74 ± 1%) was lower compared to CFSE (79 ± 2%) (p < 0.05). ATR-FTIR is a useful method to investigate relative levels of main components in bonding systems and their polymerisation kinetics. Such information is valuable to understanding such behaviour.
- Modifying dental composites to formulate novel methacrylate-based bone cements with improved polymerisation kinetics, and mechanical propertiesPublication . Khan, Muhammad Adnan; Delgado, António H. S.; Young, Anne M.Objectives: The aim was to develop bone composites with similar working times, faster polymerisation and higher final conversion in comparison to Cortoss™. Additionally, low shrinkage/heat generation and improved short and longer-term mechanical properties are desirable. Methods: Four urethane dimethacrylate based composites were prepared using tri-ethylene-glycol dimethacrylate (TEGDMA) or polypropylene dimethacrylate (PPGDMA) diluent and 0 or 20 wt% fibres in the glass filler particles. FTIR was used to determine reaction kinetics, final degrees of conversions, and polymerisation shrinkage/heat generation at 37 °C. Biaxial flexural strength, Young’s modulus and compressive strength were evaluated after 1 or 30 days in water. Results: Experimental materials all had similar inhibition times to Cortoss™ (140 s) but subsequent maximum polymerisation rate was more than doubled. Average experimental composite final conversion (76%) was higher than that of Cortoss™ (58%) but with less heat generation and shrinkage. Replacement of TEGDMA by PPGDMA gave higher polymerisation rates and conversions while reducing shrinkage. Early and aged flexural strengths of Cortoss™ were 93 and 45 MPa respectively. Corresponding compressive strengths were 164 and 99 MPa. Early and lagged experimental composite flexural strengths were 164–186 and 240–274 MPa whilst compressive strengths were 240–274 MPa and 226–261 MPa. Young’s modulus for Cortoss™ was 3.3 and 2.2 GPa at 1 day and 1 month. Experimental material values were 3.4–4.8 and 3.0–4.1 GPa, respectively. PPGDMA and fibres marginally reduced strength but caused greater reduction in modulus. Fibres also made the composites quasi-ductile instead of brittle.