摘要
分别用丙酮、乙腈、二氯甲烷、甲醇、四氢呋喃、甲苯做溶剂配制同一个纯度已知(99%)的三苯基氯硅烷样品,然后用气质联用色谱仪(GCMS)对其进行检测,发现用这几种实验室常见的溶剂配制得到的检测结果不尽相同,有些甚至相差很大,通过对GCMS检测的总离子流(TIC)面积百分比以及定性结果分析发现:用丙酮做溶剂,92.31%为三苯基氯硅醇,三苯基氯硅烷只占3.49%;用乙腈做溶剂,三苯基氯硅烷占35.78%,三苯基氯硅醇占比56.35%;用二氯甲烷做溶剂,三苯基氯硅烷占94.93%,三苯基氯硅醇占比3.20%,对三联苯占比1.19%;用甲醇做溶剂,甲氧基三苯基氯硅烷占比高达97.63%;用四氢呋喃做溶剂时,三苯基氯硅烷占98.25%,对三联苯占比1.05%;用甲苯做溶剂,三苯基氯硅烷占98.56%。可见在色谱检测中,并不是所有的溶剂都能让三苯基氯硅烷保守原分子状态,合理选择样品溶剂对获得准确的检测结果非常重要。
Acetone,acetonitrile,dichloromethane,methanol,tetrahydrofuran and toluene are used as solvents to prepare the same triphenylchlorosilane sample(with known purity 99%)and detected by GCMS respectively.It is found that the test results of the samples prepared with these common solvents in the laboratory are different,some even differ greatly.Through the analysis of the total ion current(TIC)area percentage detected by GCMS and the qualitative results,it is found that using acetone as solvent,92.31%is triphenylchlorosilanol,and triphenylchlorosilane only accounts for 3.49%;Using acetonitrile as solvent,triphenylchlorosilane accounted for 35.78%,and triphenylchlorosilanol accounted for 56.35%;Using dichloromethane as solvent,triphenylchlorosilane accounts for 94.93%,triphenylchlorosilanol accounts for 3.20%,and p-terphenyl accounts for 1.19%;Using methanol as solvent,methoxy triphenylchlorosilane accounts for 97.63%;When tetrahydrofuran is used as solvent,triphenylchlorosilane accounts for 98.25%and p-terphenyl accounts for 1.05%;Using toluene as solvent,triphenylchlorosilane accounts for 98.56%.It can be seen that not all solvents can make triphenylchlorosilane conserve the original molecular state in chromatographic detection.Reasonable selection of sample solvents is very important to obtain accurate detection results.
作者
徐炫宗
潘统很
戴雷
冯才敏
白景芬
XU Xuanzong;PAN Tonghen;DAI Lei;FENG Caimin;BAI Jingfen(Guangdong Aglaia Optoelectronic Materials Co.,Ltd,Foshan Guangdong 528333,China;College of Light Chemical Industry and Materials Engineering,Shunde Polytechnic,Foshan Guangdong 528333,China)
出处
《顺德职业技术学院学报》
2023年第1期21-25,共5页
Journal of Shunde Polytechnic
基金
广东省自然科学基金项目(2021A1515012274)
顺德职业技术学院科研项目(ZX2022003001)
广东省攀登计划项目(pdjh2021b1009)。
