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气相色谱-质谱法分析甲基苯基硅氧烷混合环体
引用本文:蒋可志,邬继荣,倪勇,来国桥.气相色谱-质谱法分析甲基苯基硅氧烷混合环体[J].分析化学,2008,36(8).
作者姓名:蒋可志  邬继荣  倪勇  来国桥
作者单位:杭州师范大学,有机硅化学及材料技术教育部重点实验室,杭州,310012
基金项目:浙江省高等学校青年教师资助计划,浙江省教育厅资助项目 
摘    要:用GC-MS对甲基苯基硅氧烷混合环体(Me2n-iPhiSinOn)样品进行分析,鉴定出了25个组分,其中包括甲基硅氧烷环体、含1个苯基的甲基硅氧烷环体以及含2个苯基的甲基硅氧烷环体。四甲基二苯基环三硅氧烷环体(Me4Ph2Si3O3)的2个异构体、六甲基二苯基环四硅氧烷环体(Me6Ph2Si4O4)的4个异构体都得到有效分离和归属,并且发现其各异构体的含量比例符合随机环化的理论值。同时对该混合环体的苯基/甲基比例以及苯基含量进行了计算,并得到氢谱的验证。

关 键 词:甲基苯基硅氧烷混合环体  气相色谱-质谱法  顺反异构体  苯基

Analysis of Mixture of Cyclic (Me2n-iPhiSinOn) by Gas Chromatography-Mass Spectrometry
JIANG Ke-Zhi,WU Ji-Rong,NI Yong,LAI Guo-Qiao.Analysis of Mixture of Cyclic (Me2n-iPhiSinOn) by Gas Chromatography-Mass Spectrometry[J].Chinese Journal of Analytical Chemistry,2008,36(8).
Authors:JIANG Ke-Zhi  WU Ji-Rong  NI Yong  LAI Guo-Qiao
Abstract:Cyclic(Me2n-iPhiSinOn),formed by the pyrolysis of HO-(MePhSiO)n-(Me2SiO)m-H,was analyzed by GC-MS on an HP-5ms capillary column,and 25 compounds were identified by library search and interpretation of the mass spectra,including cyclic(Me2SiO)n(n=3-7),cyclic(Me2n-1PhSinOn)and cyclic(Me2n-2Ph2SinOn).Two isomers of Me4Ph2Si3O3(D32Ph)and four isomers of Me6Ph2Si4O4(D42Ph)were separated respectively,and it was found that there was a statistical distribution of the isomers for every oligomethylphenylcyclosiloxanes(D32Ph,D42Ph and D52Ph).The phenyl content and the Phenyl/methyl ratio in the sample were also obtained,and validated with 1H NMR.
Keywords:Cyclic mixture of methylphenylcyclosiloxanes  gas chromatography-mass spectrometry  cis-and trans-isomers  content of phenyl group
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