title: Discrepancies in degree of conversion measurements by FTIR.
abstract: The purpose of this study was to evaluate the influence of the internal standard peak on the measured degree of conversion (DC) for methacrylate-based resins analyzed by Fourier-transform infrared spectroscopy (FTIR). The influence of different baseline measurement methods was also determined. Different blends were prepared, mixing BisGMA/BisEMA and BisGMA/TEGDMA at proportions of 0% to 100%, in weight. Camphoroquinone and ethyl-4-dimethylamino-benzoate were used to permit the light activation of blends. Degree of conversion was evaluated using FTIR equipped with an attenuated total reflectance (ATR) device. Samples were dispensed onto ATR crystal and light activated for 40 s. The DC was calculated by relating the height of the peak 1637 cm-1 to the intensity of different internal standard peaks (1715, 1608, or 1582 cm-1), measured using two different baseline methods, before and after polymerization. Data were compared by ANOVA at 5% significance. The relationship between DC and monomer ratio was obtained by regression analysis. Double-bond conversion ranged from 32.75% to 78.50% for BisGMA/BisEMA blends, and from 32.75% to 76.22% for BisGMA/TEGDMA blends. For the BisGMA/BisEMA blends, the DC showed a linear association with the composition of the comonomer blends, independent of the internal standard peak and baseline method used. In contrast, the trends in DC for BisGMA/TEGDMA blends were different for each method of measurement. The internal standard peaks and measurement baseline should be taken into account when using FTIR to calculate the DC of methacrylate-based resins, especially comonomer blends containing a high degree of monomers that lack aromatic rings.
authors.affiliation: Dental Materials Laboratory, School of Dentistry, Universidade Federal do Rio Grande do Sul, Porto AlegreRS, Brazil.
authors.forename: Fabrício Mezzomo
authors.initials: FM
authors.lastname: Collares
authors.affiliation: Dental Materials Laboratory, School of Dentistry, Universidade Federal do Rio Grande do Sul, Porto AlegreRS, Brazil.
authors.forename: Fernando Freitas
authors.initials: FF
authors.lastname: Portella
authors.affiliation: Dental Materials Laboratory, School of Dentistry, Universidade Federal do Rio Grande do Sul, Porto AlegreRS, Brazil.
authors.forename: Vicente Castelo Branco
authors.initials: VC
authors.lastname: Leitune
authors.affiliation: Dental Materials Laboratory, School of Dentistry, Universidade Federal do Rio Grande do Sul, Porto AlegreRS, Brazil.
authors.forename: Susana Maria Werner
authors.initials: SM
authors.lastname: Samuel
mesh_terms: D000704:Analysis of Variance; D017438:Bisphenol A-Glycidyl Methacrylate / Q000737:chemistry*; D055115:Light-Curing of Dental Adhesives / Q000379:methods*; D008422:Materials Testing; D008689:Methacrylates / Q000737:chemistry*; D055668:Photochemical Processes; D011092:Polyethylene Glycols / Q000737:chemistry*; D058105:Polymerization; D011109:Polymethacrylic Acids / Q000737:chemistry*; D012016:Reference Values; D012044:Regression Analysis; D017550:Spectroscopy, Fourier Transform Infrared; D013997:Time Factors
chemical_list: D008689:Methacrylates; D011109:Polymethacrylic Acids; C020946:triethylene glycol dimethacrylate; C041979:2,2-bis-(4-(2-methacryloxyethoxy)phenyl)propane; D011092:Polyethylene Glycols; D017438:Bisphenol A-Glycidyl Methacrylate