摘要
建立了分散液液微萃取(DLLME)样品制备方法,并用于工业润滑油中酚类抗氧剂的净化提取,结合气相色谱-氢火焰离子化检测技术(GC-FID),实现了变压器油全生命周期中酚类抗氧剂含量的测定。采用该方法测定了不同工业润滑油样品中酚类抗氧剂的含量,并监测了变压器油全生命周期中酚类抗氧剂含量的变化。结果表明:对于工业润滑油中两种抗氧剂2,6-二叔丁基对甲酚和2,6-二叔丁基酚的含量测定,所建DLLME-GC-FID方法的检测下限(质量浓度)均为0.03μg mL,方法中两种酚类抗氧剂的加标回收率介于84.7%~94.2%之间,其日内、日间精密度均介于1.2%~4.1%之间,且测定结果拟合曲线的线性相关系数均为0.9999,表明该方法具有较好的准确性和再现性;同时,该分析方法简单便捷、通用性强、灵敏度高、绿色环保。
A method for the preparation of dispersed liquid-liquid micro-extraction(DLLME)samples was developed and applied to the extraction and purification of phenolic antioxidants from industrial lubricating oil.Combined with gas chromatography and flame ionization detector(GC-FID),the measurement of phenolic antioxidants in the full life cycle of transformer oil was realized.This method was used to determine the content of phenolic antioxidants in different industrial lube oil samples and to monitor the change of phenolic antioxidants in transformer oil during its full life cycle.The results showed that the detection limit of the established method for 2,6-di-tert-butylphenol and 2,6-di-tert-butyl-methylphenol could be low to 0.03μg mL,respectively,the recoveries of the two phenolic antioxidants were between 84.7%-94.2%,the intra-day and inter-day precision were between 1.2%-4.1%,and linear correlation coefficients of the fitting curves were both 0.9999.This method is simple,convenient,universal,high sensitive and environmental friendly.
作者
王楠
曾颖峰
刘琼
Wang Nan;Zeng Yingfeng;Liu Qiong(SINOPEC Research Institute of Petroleum Processing Co.,Ltd.,Beijing 100083)
出处
《石油炼制与化工》
CAS
CSCD
北大核心
2023年第8期119-126,共8页
Petroleum Processing and Petrochemicals
关键词
变压器油
全生命周期
抗氧剂
分散液液微萃取法
色谱法
transformer oil
full life circle
antioxidant
dispersive liquid-liquid micro-extraction
chromatography