毛细管气相色谱法研究对环芳烷二氯化产物的组成

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 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％。

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

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%.