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

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),...

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Main Authors: Arwa Almusa, António H. S. Delgado, Paul Ashley, Anne M. Young
Format: Article
Language:English
Published: MDPI AG 2021-11-01
Series:Polymers
Subjects:
Online Access:https://www.mdpi.com/2073-4360/13/22/3886
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author Arwa Almusa
António H. S. Delgado
Paul Ashley
Anne M. Young
author_facet Arwa Almusa
António H. S. Delgado
Paul Ashley
Anne M. Young
author_sort Arwa Almusa
collection DOAJ
description 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/cm<sup>2</sup>) exposure (<i>n</i> = 3) were determined. Evaporation and polymerisation extent versus time and final changes were calculated using acetone (1360 cm<sup>−1</sup>) and methacrylate (1320 cm<sup>−1</sup>) 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.
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spelling doaj.art-50a8b3e2bd32472e813529b078e364472023-11-23T01:08:10ZengMDPI AGPolymers2073-43602021-11-011322388610.3390/polym13223886Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR SpectroscopyArwa Almusa0António H. S. Delgado1Paul Ashley2Anne M. Young3Division of Biomaterials and Tissue Engineering, UCL Eastman Dental Institute, London WC1X 8DA, UKDivision of Biomaterials and Tissue Engineering, UCL Eastman Dental Institute, London WC1X 8DA, UKDivision of Biomaterials and Tissue Engineering, UCL Eastman Dental Institute, London WC1X 8DA, UKDivision of Biomaterials and Tissue Engineering, UCL Eastman Dental Institute, London WC1X 8DA, UKThe 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/cm<sup>2</sup>) exposure (<i>n</i> = 3) were determined. Evaporation and polymerisation extent versus time and final changes were calculated using acetone (1360 cm<sup>−1</sup>) and methacrylate (1320 cm<sup>−1</sup>) 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.https://www.mdpi.com/2073-4360/13/22/3886ATR–FTIRacetonedental adhesivedental polymersdegree of conversionmethacrylate polymerization
spellingShingle Arwa Almusa
António H. S. Delgado
Paul Ashley
Anne M. Young
Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
Polymers
ATR–FTIR
acetone
dental adhesive
dental polymers
degree of conversion
methacrylate polymerization
title Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
title_full Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
title_fullStr Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
title_full_unstemmed Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
title_short Determination of Dental Adhesive Composition throughout Solvent Drying and Polymerization Using ATR–FTIR Spectroscopy
title_sort determination of dental adhesive composition throughout solvent drying and polymerization using atr ftir spectroscopy
topic ATR–FTIR
acetone
dental adhesive
dental polymers
degree of conversion
methacrylate polymerization
url https://www.mdpi.com/2073-4360/13/22/3886
work_keys_str_mv AT arwaalmusa determinationofdentaladhesivecompositionthroughoutsolventdryingandpolymerizationusingatrftirspectroscopy
AT antoniohsdelgado determinationofdentaladhesivecompositionthroughoutsolventdryingandpolymerizationusingatrftirspectroscopy
AT paulashley determinationofdentaladhesivecompositionthroughoutsolventdryingandpolymerizationusingatrftirspectroscopy
AT annemyoung determinationofdentaladhesivecompositionthroughoutsolventdryingandpolymerizationusingatrftirspectroscopy