毛细管气相色谱法研究对环芳烷二氯化产物的组成

Study on Components of Reaction Products of [2,2]-Paracyclophane Dichlorization by Capillary Gas Chromatography

在选定毛细管柱温、载气流量、分流比、注入口和 FID的温度等色谱条件下 ,分析了对环芳烷 (PCP)二氯化产物的组成。定性分析结果表明 ,PCP二氯化产物除主要组分是二氯对环芳烷 (DCPCP)外 ,还含少量的一氯对环芳烷(MCPCP)和三氯对环芳烷 (TCPCP) ;DCPCP的色谱图上出现了 3个明显的色谱峰 ,证明 3种异构体相对含量较高。用丙酮 -石油醚混合溶剂分离去除副产物 ,得到了纯度为 99.1 %的 DCPCP。以邻苯二甲酸二丁酯为内标物 ,测定了DCPCP对内标物的相对质量校正因子。按内标法定量分析了 PCP二氯化产物各组分的含量。对 DCPCP分析的相对标准偏差小于 3%。

The components of reaction products of [2,2] paracyclophane(PCP) dichlorization were analyzed by capillary gas chromatography under the optimized conditions. The result showed that dichloro [2,2] paracyclophane(DCPCP) is the main component of the products and monochloro [2,2] paracyclophane(MCPCP) and trichloro [2,2] paracyclophane (TCPCP) are byproducts.DCPCP showed three chromatographic peaks, indicating that the relative amounts of the three isomers are higher. The purity of DCPCP could reach 99.1% after the byproducts were removed with mixed solvent of acetone and petroleum ether. The dibutyl o phthalate was used as internal standard and the relative mass correction factor of DCPCP was determined. The contents of the reaction products were analyzed quantitatively by internal standard method. The relative standard deviation is less than 3%.