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建立了苯乙烯与甲基二乙氧基硅烷硅氢化反应体系中各组分含量测定的气相色谱检测方法。在GC-14B气相色谱仪(HP-5毛细管柱、FID检测器)上,以氮气为载气,采用程序升温法对各组分进行定量分析。在本实验色谱条件下,常用作基准物的正庚烷和苯的谱峰重合;而采用N,N-二甲基苯胺作为基准物质,5种组分的谱峰分离效果较好,苯乙烯、甲基二乙氧基硅烷及两种加成产物的相对质量校正因子测定值分别为0.7006,1.998,1.530,1.530;而用有效碳数法计算的理论值分别为0.8431,2.1465,1.2706,1.2706。最后,用经校正的面积归一化法测定了硅氢化反应体系中各组分含量。方法可用于硅氢加成产物的定量分析及质量控制。
A gas chromatographic method for the determination of the components in the hydrosilylation reaction of styrene and methyldiethoxysilane was established. Quantitative analysis of each component was performed on a GC-14B gas chromatograph (HP-5 capillary column, FID detector) using nitrogen as the carrier gas and temperature programmed method. Under the experimental conditions, the peaks of n-heptane and benzene, which are commonly used as reference materials, are coincident with each other. However, N, N-dimethylaniline is used as the reference material, , Methyldiethoxysilane and two addition products of the relative mass correction factor measured values ?? were 0.7006,1.998,1.530,1.530; and calculated by the effective carbon number of the theoretical values were 0.8431,2.1465,1.2706,1.2706 . Finally, the content of each component in the hydrosilylation reaction system was determined by a calibrated area normalization method. The method can be used for the quantitative analysis and quality control of hydrosilylation product.