液相色谱-核磁共振联用测定有机胺固化剂成分

Determination of main components and their contents of organic amine curing agent by HNMR-HPLC method

以核磁共振谱(NMR)和高压液相色谱(HPLC)方法对未知固化剂成分进行了解析和定量分析。首先用核磁共振方法定性了其主要成分为间苯二甲胺(m XDA)、苯甲醇(BA)、对叔丁基苯酚(PTBP),同时测定了三种主要成分的物质的量比为1.00∶1.09∶1.54。然后用液相色谱外标法建立PTBP浓度与峰面积关系曲线,线性关系式为Y=58.17+12.34X,线性回归系数为0.9999,测定了PTBP的质量分数为31.99%,加标回收率100.92%。最后由HNMR方法间接计算了mXDA和BA的质量分数分别为25.63%和18.71%。本研究工作为测定有机胺固化剂主要成分提供了一种新的思路。

The components of the unknown curing agent were analyzed and quantified by nuclear magnetic resonance spectroscopy(NMR)and high performance liquid chromatography(HPLC)methods.Firstly,the main components were determined to be m-xylylenediamine(mXDA),benzyl alcohol(BA),and p-tert-butylphenol(PTBP)by nuclear magnetic resonance method.At the same time,the molar ratio of the three main components was determined to be 1.00∶1.09∶1.54.Then the relationship curves between PTBP concentration and peak area was established by the external standard method of liquid chromatography.The linear relationship was Y=58.17+12.34 X and the linear regression coefficient was 0.9999.The content of PTBP was determined to be 31.99 wt%.The standard recovery rate was 100.92%.Finally,the contents of mXDA and BA were calculated indirectly by HNMR method to be 25.63 wt%and18.71 wt%,respectively.This research work provided a new idea for the determination of the main components of organic amine curing agents.