液液微萃取联合高效液相色谱法测定变压器绝缘油中腐蚀性硫化物二苄基二硫醚

李海燕; 李吟霜; 杨珍; 付宇超

doi:doi：10.3969/j.issn.1004-4957.2020.04.015

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液液微萃取联合高效液相色谱法测定变压器绝缘油中腐蚀性硫化物二苄基二硫醚

更新时间：2023-04-18

- 液液微萃取联合高效液相色谱法测定变压器绝缘油中腐蚀性硫化物二苄基二硫醚
- Determination of Corrosive Sulfide Dibenzyl Disulfide in Transformer Oil by High Performance Liquid Chromatography with Liquid-Liquid Microextraction
- 分析测试学报 2020年39卷第4期页码：526-531
- 作者机构：
  
  1. 中南民族大学化学与材料科学学院
  2. 中南民族大学民族地区环境与生物资源分析重点实验室
- 作者简介：
- 基金信息：
  
  中国电力科学研究院科研项目(151000637)
- DOI：doi：10.3969/j.issn.1004-4957.2020.04.015
  中图分类号：
- 纸质出版：2020
- 稿件说明：
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李海燕, 李吟霜, 杨珍, 付宇超. 液液微萃取联合高效液相色谱法测定变压器绝缘油中腐蚀性硫化物二苄基二硫醚[J]. 分析测试学报, 2020,39(4):526-531.

李海燕, 李吟霜, 杨珍, 付宇超. Determination of Corrosive Sulfide Dibenzyl Disulfide in Transformer Oil by High Performance Liquid Chromatography with Liquid-Liquid Microextraction[J]. 2020, 39(4): 526-531.
李海燕, 李吟霜, 杨珍, 付宇超. 液液微萃取联合高效液相色谱法测定变压器绝缘油中腐蚀性硫化物二苄基二硫醚[J]. 分析测试学报, 2020,39(4):526-531. DOI： doi：10.3969/j.issn.1004-4957.2020.04.015.

李海燕, 李吟霜, 杨珍, 付宇超. Determination of Corrosive Sulfide Dibenzyl Disulfide in Transformer Oil by High Performance Liquid Chromatography with Liquid-Liquid Microextraction[J]. 2020, 39(4): 526-531. DOI： doi：10.3969/j.issn.1004-4957.2020.04.015.

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6.9~7.1 μg/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。

Abstract

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 6.9-7.1 μg/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.

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