Pyrolysis gas chromatography coupled with FT-IR (Py-GC/FT-IR) has been applied to the study of silane treatment of E-glass fiber. The glass fiber treated with a silane coupling agent, γ-anilinopropyltrimethoxysilane (AnPS), is pyrolyzed at 750°C. The pyrolysates are fractionated by GC and analyzed by FT-IR. The main fraction is assigned to the organofunctional group of the coupling agent. Thus, Py-GC/FT-IR enables us to identify the treated coupling agent qualitatively. A mixture of two different coupling agents, AnPS and γ-methacryloxypropyltrimethoxysilane on glass fiber, is separated and characterized from the spectra of fractions resulting from each coupling agent. Py-GC/FT-IR also provides quantitative information regarding the coupling agents on glass fiber. The total amount of the treated coupling agent is estimated according to the calibration curves, which are proportional to the amount of the coupling agent. Moreover, Py-GC/FT-IR enables us to evaluate the fixing ratio of the coupling agent to the total amount through washing the samples with methanol. The fixing ratio falls significantly above treatment concentration. This tendency is consistent with the results from nondestructive sampling preparation techniques in infrared spectroscopy. The above results indicate the usefulness of Py-GC/FT-IR for the evaluation of silane treatment.
Etsuo Nishio, Nobuo Ikuta, Tsuneaki Hirashima, and Joichi Koga, "Pyrolysis-GC/FT-IR Analysis for Silane Coupling Treatment of Glass Fibers," Appl. Spectrosc. 43, 1159-1164 (1989)