气相色谱-质谱联用法测定丁二烯中对叔丁基邻苯二酚含量

许琳　 张齐　 李海强　

摘　要：采用气相色谱-质谱联用(GC-MS)法测定丁二烯中阻聚剂对叔丁基邻苯二酚(TBC)含量,并与分光光度法和液相色谱法进行了比较.结果表明,用甲苯作为TBC的溶剂,其在被测组分的出峰区域不会形成干扰;采用选择离子模式检测可提高灵敏度.TBC质量分数为1×10~(-6)～50×10~(-6)时,外标法测定TBC含量的线性回归系数为0.999 5,加标回收率为98.60%～102.73%,相对偏差为2.42%～3.87%;GC-MS法与分光光度法、液相色谱法测得丁二烯中TBC含量相近,但GC-MS法更简便和快捷.
关键词：气相色谱-质谱联用法;丁二烯;阻聚荆;对叔丁基邻苯二酚
分类号：TQ314.24~+4　文献标识码：A
文章编号：1000-1255(2009)03-0193-03

Determination of p-tert-butylcatechol content in butadiene monomer by gas chromatography-mass spectrometry

Xu Lin（School of Chemistry and Chemical Engineering,South China University of Technology,Guangzhou 510640,China）　 Zhang Qi（Beijing Research Institute of Chemical Industry,SINOPEC,Beijing 100013,China）　 Li Haiqiang （Synthetic Rubber Plant of Qilu Company Ltd,SINOPEC,Zibo 255438,China）　

Abstract：The content of p-tert-butylcatechol (TBC) in butadiene monomer was determinated by gas chromatography-mass spectrometry (GC-MS),compared with those determinated by spectrophotom-etry and liquid chromatography (LC).The results showed that with toluene as solvent of TBC,it would not disturb TBC peak in the total ion chromatogram.The sensitivity of detection was improved by selected ion monitoring mode.There was a good linear relationship within the range of 1 × 10~(-6) to 50 × 10~(-6) (correlation coefficient 0.999 5) for external standard method,and the recovery was in the range of 98.60% - 102.73%.The TBC content in butadiene determined by GC-MC was similar to those detected by spectrophotometry and LC,and it was proved to be fast and easy.
Keywords：gas chromatography-mass spectrometry;butadiene;inhibitor;p-tert-butylcatechol