Investigation of infrared calibration methods for application to the study of methyl methacrylate polymerization

Abstract

Infrared spectroscopy has been used to monitor the polymerization of methyl methacrylate. Concentrations of methyl methacrylate in the reaction mixture were determined by use of three calibration methods. Classical quantitative analysis was used to measure the height of the stretching vibration bands of the vinyl group at 1639 cm(-1). A calibration procedure using the considerably higher intensity of the C = O stretching vibration band of the carbonyl ester group at 1725 cm(-1) seemed useful only for high concentrations of methyl methacrylate, i.e. at the beginning of reaction, because this band overlaps that of poly(methyl methacrylate). Use of second-derivative spectra and measuring their values at 1725 cm(-1) enabled estimation of ten times lower concentrations of methyl methacrylate the calibration using the band from the vinyl group.

Differences in infrared spectroscopic data of connective tissues in transflectance and transmittance modes

“…In addition, Bassan et al [21] reported that 2 nd derivative spectra may provide more accurate quantitative information for comparison among these data collection modes, and therefore second derivative spectra peak heights were measured, and positions used to accurately define the wavenumbers of the identified peaks. The areas of the carbonyl (1660–1800 cm −1 ), C-O-C stretching (1256–1340 cm −1 ) and CH 3 rocking (1092–1176 cm −1 ) absorbances of PMMA were identified and used to characterise differences in the transmission/transflectance spectral response[23]. For the non-polarized cartilage and tendon data, collagen and proteoglycan (PG) were evaluated in the 1594–1718 cm −1 (amide I absorbance) and 985–1140 cm −1 (sugar C-O-C ring absorbance) spectral regions, respectively.…”

Pseudo‐interpenetrating polymer networks based on tetrafunctional epoxy resins and poly(methyl methacrylate)

“…(2), was re‐expressed in terms of the time dependence of the cyclic ether absorbance at 906 cm −1 : where the temperature‐dependent characteristic chemical reaction time constant (λ) for n th‐order irreversible kinetics is defined by We used a similar strategy to analyze transient IR data for TGDDM and EDA in the presence of MMA. Ambient‐temperature spectroscopic evidence that the vinyl monomer polymerized to yield PMMA interspersed within the network produced by TGDDM and EDA was obtained from the carbonyl stretching vibration in the ester functional group, whose superficial absorption peak shifted from 1722 cm −1 in MMA to 1727 cm −1 in PMMA after 3 h under polymerization conditions 35. There was also a significant decrease in the carbon–carbon double‐bond stretching vibration at 1639 cm −1 as the vinyl monomer was converted to linear polymer 35.…”

“…Ambient‐temperature spectroscopic evidence that the vinyl monomer polymerized to yield PMMA interspersed within the network produced by TGDDM and EDA was obtained from the carbonyl stretching vibration in the ester functional group, whose superficial absorption peak shifted from 1722 cm −1 in MMA to 1727 cm −1 in PMMA after 3 h under polymerization conditions 35. There was also a significant decrease in the carbon–carbon double‐bond stretching vibration at 1639 cm −1 as the vinyl monomer was converted to linear polymer 35. Because MMA was not the major component in these p‐IPNs and the CC stretch at 1639 cm −1 was rather weak and not completely resolved, we evaluated the effect of MMA on the kinetics of network formation by focusing on the cyclic ether deformation at 906 cm −1 .…”

Final Report of the Cosmetic Ingredient Review Expert Panel Safety Assessment of Polymethyl Methacrylate (PMMA), Methyl Methacrylate Crosspolymer, and Methyl Methacrylate/Glycol Dimethacrylate Crosspolymer

“…21 During manufacture, infrared spectroscopy is used to monitor the polymerization of MMA to PMMA. 22 Table 2 shows the methods of physical and chemical analysis of PMMA used as bone cement.…”