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建立了离子对反相液相色谱法同时检测PX氧化残渣中7种芳香羧酸的方法。本方法以Waters Atlantis dC18反相色谱柱为分离柱,四丁基氢氧化铵为离子对试剂,在优化色谱条件下,紫外检测波长为240nm,流速为0.35mL·min~(-1),色谱柱温度为35℃,7种芳香羧酸达到基线分离。方法线性范围10-200mg/kg,平均加标回收率为98-102%,相对标准偏差为<1%。将本方法用于氧化残渣回收的生产分析,结果满意。
A method for the simultaneous determination of seven kinds of aromatic carboxylic acids in PX oxidation residue by ion-pair reversed-phase liquid chromatography was established. In this method, a Waters Atlantis dC18 reversed-phase column was used as the separation column, and tetrabutylammonium hydroxide was used as the ion pair reagent. Under optimized chromatographic conditions, the UV detection wavelength was 240 nm, the flow rate was 0.35 mL · min -1, For 35 ℃, seven kinds of aromatic carboxylic acid to baseline separation. The linear range of the method was 10-200mg / kg, the average recovery was 98-102% and the relative standard deviation was <1%. The method is applied to the analysis of the production of oxidation residue recovery with satisfactory results.