Gas Chromatographic Method for the Determination of Residual Monomers, 2-(Acryloyloxy)ethyl Isocyanate and 2-(Methacryloyloxy)ethyl Isocyanate, as Curing Agents in an Ultraviolet Curable Adhesive

A gas chromatographic method is described for the determination of residual 2-(acryloyloxy)ethyl isocyanate (AOI) and 2-(methacryloyloxy)ethyl isocyanate (MOI) as curing agents in an ultraviolet curable adhesive. Pre-column derivatization was employed in the determination of AOI and MOI as a means of enhancing the response of the flame ionization detector. Urethane derivatives of AOI and MOI were derived using methanol for 30 min at room temperature. The accuracies (n 5 5, three concentration levels) were in the range of 113.4 to 126.7%, and precisions (n 5 5, three concentration levels) were in the range of 0.8 to 4.3% for AOI-OMe. Furthermore, the accuracies were in the range of 79.5 to 108.6% and the precisions were in the range of 1.0 to 2.4% for MOI-OMe. The correlation coefficients of six calibration standards were all greater than 0.9999 for AOI-OMe and greater than 0.9998 for MOI-OMe over the range from 10 to 100 mg/mL.