对二甲苯氧化产物的色谱分析

Analysis of p-xylene oxidation products by GC and HPLC

提出用气相色谱快速定量溶剂醋酸,用液相色谱法快速分析对二甲苯氧化反应体系的所有含苯环的组分的方法。应用Agilent1100高效液相色谱仪,采用D iamonsilC18(D5μm×4.6 mm×150 mm)色谱柱,用甲醇-乙腈-水为流动相,用外标法采用三元梯度洗脱程序分析固相产物中的对羧基苯甲醛和对苯二甲酸含量。以异丙苯为内标物,应用Agilent1100高效液相色谱仪,用甲醇-乙腈-水为流动相,采用三元梯度洗脱程序分析液相产物中的含苯环组分对甲基苯甲醛、对甲基苯甲酸、对羧基苯甲醛、对苯二甲酸、苯甲酸、对二甲苯和内标物异丙苯,应用Sh imazu6A气相色谱仪分析液相中的溶剂醋酸和内标物异丙苯,气相和液相结果通过内标物异丙苯关联。该法准确简捷、且分析周期短。

A method that use gas chromatography（GC） to rapid quantify the solvent acetic acid and use high performance liquid chromatography（HPLC） to rapid analyse all components contain benzene in PX oxidation system was provid- ed. By using Agilent 1100 HPLC and Diamonsilc 18 （（D5 μm×4.6mm×150mm）chromatography column,using methanol-acetonitrile-water as mobile phase, using external standard method three-component grade elution program,the 4-CBA and TA content in solid state product was analysed. By using isopropyl benzene as the internal standard material, using Agilent 1100 HPLC ,using methanol-acetonitrile-water as mobile phase ,using three-component grade elution program,the components that contain benzene such as TALD,PT,4-CBA,TA,BA,PX and internal standard material isopropyl benzene in liquid phase product was analysed. Shimazu6A GC was used to analyse the solvent acetic acid and internal standard material isopropyl benzne in liquid phase. The gas phase and liquid phase results are interrelated through internal standard material isopropyl benzne. The method is simple and rapid. The analysis period is short.