Percorrer por autor "Almusa, Arwa"
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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.
- Interpretation of ATR-FTIR spectra of dental adhesives throughout simultaneous polymerization and solvent lossPublication . Almusa, Arwa; Delgado, António H. S.; Young, Anne MargaretThis study developed new Fourier transform infrared (FTIR) spectroscopy methods to assess effects of drying level on the composition and polymerization kinetics of One‐Step® (OS), OptibondTM Universal (OU) and G‐Bond (GB) dental adhesives. 5 μL of each adhesive were placed in turn on an FTIR, Attenuated Total Reflectance (ATR) accessory, operating at 37ºC. Spectra were generated before, during and after light-curing (20 s, 1000 mW/cm2, 450−470 nm) at 10 s after placement or following 300 s of passive drying (n = 3). Individual spectra of solvents, monomers and fillers, combined with spectral change upon polymerization, were used to generate model spectra and quantify component levels versus time up to 300 s after start of light exposure. Polymerization rates and maximum degree of conversion were derived using a combination of polymer and monomer peaks at 1480 and 1320 cm-1. Inferential analyses included Kruskal-Wallis/Mann-Whitney U using a significance level of 5%. Initial acetone levels were 65, 48 and 50% in OS, OU and GB, respectively, whilst curing at 10 versus 300 s gave final acetone levels of 35, 20 and 32% versus 0, 0 and 10%. With earlier light exposure, monomer reaction rate was reduced but continued for longer leading to final conversions of 88, 86 and 40% versus 61, 66 and 77% for OS, OU and GB, respectively. The FTIR techniques developed could monitor process kinetics and demonstrate the large, highly significant effects of drying method on final polymerized dental adhesive composition and polymerization level.
