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.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第2期263-267,共5页
Chinese Journal of Analytical Chemistry
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
Triethylboron, diethylboroxin, gas chromatography-mass spectrometry, mass spectrum analyzing, reaction mechanism
