紫外光引发剂907及其反应中间体的气相色谱测定

Determination of Photoinitiator 907and Its Reaction Intermediates by Gas Chromatography

建立了光引发剂907合成工艺控制中反应原料、中间体及产物的气相色谱分析方法。采用SE-54石英毛细管柱,程序升温进行分离,氢火焰离子化检测器(FID)进行检测。结果表明,原料苯甲硫醚,反应中间体807A、807B、907C和产物907线性范围分别为0.2～14.0μg/mL、0.4～20.0μg/mL、0.5～22.0μg/mL和0.6～19.0μg/mL,线性相关系数R均大于0.999,相对标准偏差小于2.5%,回收率为93.6%～106.8%。产物结构通过红外光谱进行表征。该方法线性关系、准确度和精密度良好,适用于光引发剂907合成工艺的快速监控及产品定量分析。

A method of gas chromatography（GC）was developed for the analysis of the raw material,intermediates and products in the synthesis process of photoinitiator 907.A silica capillary column SE-54 was used to separate the analytes by temperature programming.Flame ionization detector（FID）was used.The linear ranges for raw material thioanisole,intermediate 807Aand 807Band the final product 907were 0.2～14.0,0.4～20.0,0.5～22.0and 0.6～19.0μg/mL,respectively.The RSD of the method was less than 2.5%,and the recovery was between 93.6% and 106.8%.The structure of the final product 907was further illuminated by infrared spectrum（IR）.The result showed that the proposed method was good at linear relationship,accuracy and precision,it could be used in the rapid monitoring of the synthetic technology of photoinitiator 907.