气相色谱-质谱法测定橡胶材料中的五氯硫酚含量

Determination of Pentachlorothiophenol Content in Rubber Materials by Gas Chromatography-Mass Spectrometry

建立采用气相色谱-质谱法测定橡胶材料中五氯硫酚含量的分析方法。试样经甲醇超声萃取,在碳酸钾溶液中加入乙酸酐进行乙酰化后,用正己烷提取。采用气相色谱-质谱仪选择离子测定,外标法定量。试验结果表明,该方法具有准确、稳定、灵敏度高的特点,其检出限<0.5 mg·kg^(-1),加标回收率达到84%~92%,可以作为常规检测方法应用于实际产品检测中。

An analytical method using gas chromatography-mass spectrometry(GC-MS)to determine the content of pentachlorothiophenol in rubber materials was established.The sample was ultrasonically extracted with methanol,acetylated with acetic anhydride in a potassium carbonate solution,and then extracted with n-hexane.The gas chromatography-mass spectrometer was used with ion determination and the external standard method for quantification.The test results showed that the method was accurate,stable and sensitive with the detection limit of less than 0.5 mg·kg^(-1),and the recovery rate of standard addition was 84%~92%,which could be used as a routine analytical method in actual product detection.