工业用乙酸乙烯酯纯度及其有机杂质的气相色谱检测方法研究

Determination of purity and organic impurities in vinyl acetate for industrial use by gas chromatography method

研究了乙酸乙烯酯中14种有机杂质在HP-1和CP-SIL 5CB两种非极性色谱柱上的分离,采用校正面积归一化法定量,建立了测定工业用乙酸乙烯酯纯度及其有机杂质含量的气相色谱分析法。该方法可用于检测乙炔法和乙烯法两种不同工艺路线制备的乙酸乙烯酯产品纯度及有机杂质的含量。实验结果表明,方法重复性好且准确性高,5次重复测定相对标准偏差小于3.3%,组分回收率在93.3%~119.9%之间;方法检测灵敏度高,含氧有机杂质的检测限可达0.5~4.7 mg/kg,苯系物检测限可达0.2~0.7 mg/kg。为修订现行标准SH/T 1628.2—1996提供了基础,对乙酸乙烯酯的生产控制、产品检测和下游应用都具有重要意义。

HP-1 and CP-SIL 5CB columns were used for the separation of 14 impurities in vinyl acetate.The GC method was established for the determination of purity and organic impurities in vinyl acetate.The method determined all the required impurities in vinyl acetate produced by both ethylene method and the acetylene method.The results indicated that the method showed good repeatability and accuracy.The relative standard deviations of the 5 repeated measurements are less than 3.3%,and the recoveries of the impurities were in the range of 93.3%-119.9%.The method also showed high detection sensitivity,and the detection limits of oxygenated organic impurities and benzene series reached 0.5-4.7 mg/kg and 0.2-0.7 mg/kg,respectively.This study provides support for the revision of SH/T 1628.2—1996,and can be applied in production control,product testing and market trade of vinyl acetate.