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Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy

Almusa, A; Delgado, AHS; Ashley, P; Young, AM; (2021) Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy. Polymers , 13 (22) p. 3886. 10.3390/polym13223886. Green open access

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Abstract

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, USA), Optibond Universal (OU; Kerr, USA), and G-Bond (GB; GC, 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.

Type: Article
Title: Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
Open access status: An open access version is available from UCL Discovery
DOI: 10.3390/polym13223886
Publisher version: https://doi.org/10.3390/polym13223886
Language: English
Additional information: © 2021 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/license s/by/4.0/).
Keywords: ATR–FTIR; acetone; dental adhesive; dental polymers; degree of conversion; methacrylate polymerization; photopolymerization; polymerization kinetics
UCL classification: UCL
UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences
UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Medical Sciences
UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Medical Sciences > Eastman Dental Institute
UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Medical Sciences > Eastman Dental Institute > Biomaterials and Tissue Eng
UCL > Provost and Vice Provost Offices > School of Life and Medical Sciences > Faculty of Medical Sciences > Eastman Dental Institute > EDI Craniofacial and Development Sci
URI: https://discovery-pp.ucl.ac.uk/id/eprint/10138457
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