气相色谱法测定环戊二烯三聚体的4种同分异构体的含量

Determination of 4 Isomers of Trimeric Cyclopentadiene by Gas Chromatography Spectrometry

样品(0.400 0g)用甲苯溶解并定容至5.0mL作为样品溶液,用于气相色谱法测定。选用TC-WAX毛细管柱为色谱分离柱,柱温条件为从50℃开始以6℃·min-1速率升温至230℃,保持10min,分流比为3∶1。在此条件下可达到环戊二烯三聚体4种同分异构体的有效分离。用氢火焰离子化检测器检测,以外标法定量。上述4种同分异构体的质量浓度均在5.00～100g·L-1范围内与其对应的峰面积之间呈线性关系,检出限(3S/N)在2.0～2.5mg·L-1之间。用标准加入法进行回收试验,测得回收率在94.8%～106%之间,测定值的相对标准偏差(n=10)均不大于2%。

The sample(0.4000 g)of trimeric cyclopentadiene(TCPD)was dissolved in and made its volume to 5.0 mL with toluene which was used as sample solution for GC determination of its 4 isomers.TC-WAX capillary column was selected for GC separation,and the 4 isomers were effectively separated under the following conditions:①column temperature was elevated from the initial value of 50℃to 230℃ at a rate of 6℃·min^-1 and kept for10 min at this temperature;and②separation-flowing ratio of 3 to 1 was taken.Hydrogen flame ionization detector was used in the detection.External standard method was adopted for quantification.Linear relationships between values of peak areas and mass concentrations of the 4 isomers were found in the same range of 5.00-100 g·L^-1,with detection limits(3 S/N)in the range of 2.0-2.5 mg·L^-1.Recovery was tested by standard addition method,giving values of recovery ranged from 94.8%to 106%,and RSDs(n=10)of the measured value were all less than2%.