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

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%。

Determination of 4 Isomers of Trimeric Cyclopentadiene by Gas Chromatography Spectrometry

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%.