茚满合成产物馏分的气相色谱分析

Analysis of the Primary Components of Synthetic Indene by GC

为了了解茚满合成过程中主反应和副反应进行的程度 ,利用气相色谱分析方法对其反应产物进行了分析。选择了色谱分析条件 ,以非极性的阿皮松L为固定相 ,硅砖C2 2 为载体的2mm× 3m的不锈钢填充柱为分析柱 ,用FID检测器进行检测。以H2 为载气 ,N2 为辅助气。经实验最后选定的条件为 :汽化室温度 12 5℃ ;检测室温度 12 5℃ ;柱温 6 0℃ ;载气H2 流量 34mL/min ;辅助气N2 0 .0 3MPa;助燃气空气 0 .0 6MPa;检测器 (FID)灵敏度 :8× 10 -11A/mV ;进样量 :0 .6 μL。利用本方法可将茚满合成产物中的轻组分顺利分开 ,所有组分的分离度均大于 1.5 ,相对标准偏差 (RSD)小于 6 %。发现轻组分中 ,含量最大的为异戊烷 ,为茚满合成条件的确定提供了可靠的依据。

In order to find out the degree of primary reaction and by-reaction. The GC was used to analyze the production of reaction. The analytical conditions was selected. A stainless steel column 3 m×2 mm(ID)filled with C 22 coated 10% Apiezon grease L was used as reactor,FID was used as detector and hydrogen was used as carry gas and nitrogen was used as assistant gas. The finally chosen chromatographic conditions are as follows: the oven operation temperature is 60 ℃; the gasifying temperature is 125 ℃; the temperature of FID detector is 125 ℃; the flow amount of carrier hydrogen is 34 mL/min; the pressure of assistant nitrogen is 0.03 MPa; the pressure of combustion-supporting air is 0.06 MPa; the detector sensitivity is 8×10 -11 A/mV; injector volume is 0.6 μL. Using this analytical method the primary components of indene synthetic reaction are completely separated. The resolution of all components is more than 1.5, RSD was less than 6%. The content of isopentane is the greatest in the found primary components. The analytical results can provide reliable foundation for determine indene synthetic conditions.