摘要
建立了涡旋液液微萃取(VA-LLME)联合高效液相色谱(HPLC)测定变压器绝缘油中主要腐蚀性硫化物二苄基二硫醚(DBDS)含量的方法。以乙腈为萃取剂,在最佳条件下,同时采用外标法和内标法进行分析。实验结果表明,变压器油中DBDS含量在0.1~600.0 mg/kg范围内线性关系良好,相关系数(r)大于0.999,检出限为6.9~7.1μg/kg。将该方法用于商品变压器油及老化变压器油中目标分析物的测定,其加标回收率为95.0%~112%,RSD不大于2.3%。该方法具有高效、灵敏和环境友好的特点,与现行美国IEC 62697的GC-ECD方法和我国GB/T 32508的GC-MS方法无显著性差异。相关研究可为我国变压器油中腐蚀性硫化物DBDS定量检测方法的标准修订提供参考。
An analytical method was established for the determination of the main corrosive sulfide,dibenzyl disulfide(DBDS)in transformer insulating oil by high performance liquid chromatography(HPLC)with vortex-assisted liquid-liquid microextraction(VA-LLME).Under the optimized conditions,the DBDS was quantified by external standard method and internal standard method with acetonitrile as extractant.Results showed that there were good linear relationship for DBDS in the concentration range of 0.1-600.0 mg/kg with correlation coefficients(r)more than 0.999.The limits of detection(LOD,S/N=3)were in the range of 6.9-7.1μg/kg.The method was applied in the determination of target analytes in commercial transformer oil samples and aging oil samples.The recoveries were in the range of 95.0%-112%with relative standard deviations(RSD)not more than 2.3%.The method has the characteristics of high efficiency,high sensitivity and environmental friendliness,and has no significant difference with the GC-ECD method of IEC 62697 in USA and GC-MS method of GB/T 32508 in China.It also provides references for the standards revision of quantitative detection of corrosive sulfide DBDS in transformer oils in China.
作者
李海燕
李吟霜
杨珍
付宇超
LI Hai-yan;LI Yin-shuang;YANG Zhen;FU Yu-chao(College of Chemistry and Materials Science,SouthCentral University for Nationalities,Wuhan 430074,China;Key Laboratory of Analytical Chemistry for Environment and Biological Resources in EthnicDistricts,SouthCentral University for Nationalities,Wuhan 430074,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2020年第4期526-531,共6页
Journal of Instrumental Analysis
基金
中国电力科学研究院科研项目(151000637)。
关键词
二苄基二硫醚(DBDS)
液液微萃取
高效液相色谱
变压器油
硫腐蚀
dibenzyl disulfide(DBDS)
liquid-liquid microextraction
high performance liquid chromatography(HPLC)
transformer oil
corrosive sulfide
