采用反吹技术和GC-MS测定变压器油中的抗氧剂

Determination of the Antioxidant in Transformer Oil byBackflushing Technique and GC-MS

本文描述了使用带反吹装置的气相色谱质谱联用仪器测试变压器油中的抗氧剂2,6-二叔丁基苯酚(DBP)和2,6-二叔丁基甲酚(DBPC),通过反吹出重组分的方式来有效降低样品基质影响,提高了分析精度,并对它们的检出限、定量限、准确度以及精密度进行了研究,结果显示DBP的方法检出限是0.05 mg/kg,方法定量限是0.18 mg/kg,加标回收率在86.9%~109.3%之间,相对标准偏差在1.3%~2.4%之间,DBPC的方法检出限是0.1 mg/kg,方法定量限是0.33 mg/kg,加标回收率在89.8%~108.4%之间,相对标准偏差在1.1%~3.4%之间,完全满足痕量测试的要求,因此,本方法为变压器油中抗氧剂的测试提供了一个可靠的参考。

This article presents the utilization of a gas chromatography-mass spectrometry(GC-MS)instrument equipped with a backflush device for the testing of antioxidants 2,6-di-tert-butylphenol(DBP)and 2,6-di-tert-butyl-p-cresol(DBPC)in transformer oil.By effectively eliminating the influence of the sample matrix through the backflushing of heavy components,the analytical accuracy was significantly improved.The study also investigated the detection limits,quantitation limits,accuracy,and precision of the method.The results revealed that the detection limit for DBP was 0.05 mg/kg,with a quantitation limit of 0.18 mg/kg.The spiked recovery rates range from 86.9%to 109.3%,and the relative standard deviations fall between 1.3%and 2.4%.Similarly,for DBPC,the detection limit was 0.1 mg/kg,with a quantitation limit of 0.33 mg/kg.The spiked recovery rates were between 89.8%and 108.4%,and the relative standard deviations were within 1.1%to 3.4%.These results fully meetted the requirements for trace testing.Therefore,this method provides a reliable reference for the testing of antioxidants in transformer oil.