气相色谱-质谱联用法对三乙基硼合成反应副产物的研究  

Studies of By-products in Synthesis Reaction Triethylboron by Gas Chromatography-Mass Spectrometry

作　　者：符迈进[1] 朱京科[1] 王军娟[1] 

机构地区：[1]浙江大学材料与化工学院,杭州310027

出　　处：《分析化学》2007年第2期263-267,共5页Chinese Journal of Analytical Chemistry

摘　　要：利用气相色谱/质谱联用技术对三乙基硼合成反应的产物进行了定性研究。进样量为5μL,以HP-5毛细管柱(30.0 m×250μm,0.25μm)为气相色谱柱,在柱温90℃、气化室温度120℃、载气为氦气、流量为0.8 mL/min的条件下,三乙基硼合成产物得到了很好分离。通过对该反应产物进行人工质谱解析,并结合计算机谱库检索,鉴定出三乙基硼合成反应的5种副产物。其中二乙基环硼氧烷在其它文献中未见报道。通过对反应过程的研究,讨论了多种副产物产生的机理,佐证了副产物的结构,为三乙基硼及其类似物的研究奠定了基础。The products in synthesis of triethylboron were determined by gas chromatography-mass spectrometry. The helium gas flow rate was at 0.8 mL/min （constant flow）, and the oven temperature was held isothermally at 90℃. The injector temperature was 120℃ and the transfer line was maintained at 280℃. A 5μL of sample was introduced into GC by splitless injection and separated on a 30 m × 0.25 μm, 0.25 μm film thickness HP-5 MS capillary column. Five by-products were identified by manually mass spectrum analyzing and mass spectrum bank matching, in which one compound unreported （diethylboroxin） was found. The mechanisms of by-products＇ forming were proposed, which validated the by-products＇ structure. This method may be provided for the study of triethylboron and its analogs.

关 键 词：三乙基硼 二乙基环硼氧烷 气相色谱/质谱联用 质谱解析 反应机理 

分 类 号：O657.63[理学—分析化学]