采用裂解气相色谱/质谱法研究双酚A环氧树脂结构

采用裂解气相色谱/质谱联用方法对不同品种和牌号的双酚A环氧树脂进行分析研究。选择550℃裂解,其裂解产物通过SE～54高效毛细管柱分离和质谱鉴定,提供了有关环氧树脂的特征结构信息。通过对总离子流图中裂解碎片峰峰面积比值的计算,可初步鉴定7种不同牌号的环氧树脂。此方法,具有样品无需前处理,作量少,对应性强,灵敏度高等特点。

Structure determination of epoxy resin by pyrolysis-gas chromatograhpy/mass spectrometry

Seveal types of diphenylol propane epoxy resins have been identified by pyrolysis gas chromatography-mass spectrometry ( PyGG-MS). One vertical microfumace-type pyrolyzer was directly attached to a gas chromato graph-mass spectrometry. About 20μg of the epoxy resin sample was introduced into the heater center of the pyrolyzer at 550℃ under the flow of helium carrier gas. The inlet mode was split with an injection interval of 20s and the inlet pressure was 12 psi. The gas chromatograph was fitted with a fused-silica capillary column (SE-54 30m × 0.25mm× 0.25μm) . Temperature program settings were: initial temperature, 40℃; hold 5 min; increase at 5℃ min-1to 270℃; hold 5min . All pyrolysis products referred to were identified by mass spectrometry. The temperature of the ion source was 210℃ and the temperature of the transfer line was 250℃.The diphenylol propane epoxy resins could be identified as they had different molecular weight and ratio of the peak area in total ion chromatogram. This method is sensitive, accurate, convenient, and requires minimal sample manipulation.