色谱 ›› 2020, Vol. 38 ›› Issue (6): 702-707.DOI: 10.3724/SP.J.1123.2019.11012

• 研究论文 • 上一篇    下一篇

六氟化硫中痕量一氧化碳和二氧化碳的气相色谱检测及其在断路器故障分析中的应用

杨韧1,*(), 汪金星2, 张悦3, 王青3, 岳宣峰3,*()   

  1. 1 国网陕西省电力公司电力科学研究院, 陕西 西安 710048
    2 国网陕西省电力公司, 陕西 西安 710048
    3 陕西省生命分析化学重点实验室, 陕西师范大学化学化工学院, 陕西 西安 710062
  • 收稿日期:2019-11-22 出版日期:2020-06-08 发布日期:2020-12-10
  • 通讯作者: 杨韧,岳宣峰
  • 作者简介:岳宣峰.Tel:(029)85310726, E-mail:xfyue@snnu.edu.cn
    杨韧.Tel:(029)89698077, E-mail:yangren1970@263.net;
  • 基金资助:
    中央高校科技成果转化培育项目(GK201806003);陕西省重点研发计划(2020GY-250);研究生教育教学改革研究项目(GERP-19-60);陕西师范大学2017-度实验技术研究项目

Gas chromatographic determination of trace carbon monoxide and carbon dioxide in sulfur hexafluoride and its application to probing potential breakdown of high-voltage circuit breaker

YANG Ren1,*(), WANG Jinxing2, ZHANG Yue3, WANG Qing3, YUE Xuanfeng3,*()   

  1. 1 Electric Power Research Institute of State Grid Shaanxi Electric Power Company, Xi'an 710048, China
    2 State Grid Shaanxi Electric Power Company, Xi'an 710048, China
    3 Key Laboratory of Analytical Chemistry for Life Science of Shaanxi Province, School of Chemistry and Chemical Engineering of Shaanxi Normal University, Xi'an 710062, China
  • Received:2019-11-22 Online:2020-06-08 Published:2020-12-10
  • Contact: YANG Ren,YUE Xuanfeng
  • Supported by:
    Fund for the Transformation of Scientific and Technological Achievements of Central Universities(GK201806003);Shaanxi Key Reserch and Development Project(2020GY-250);Project of Postgraduate Education and Teaching Reform(GERP-19-60);2017 Shaanxi Normal University Experimental Techniques Research Project

摘要:

为了准确分析高浓度SF6中痕量的CO及CO2,发展了可靠的气相色谱-火焰离子化检测器(GC-FID)方法。通过双Porapak Q色谱柱结合阀切换将SF6从待测样品中分离并排出检测系统,从而避免SF6可能造成的在线转化柱中毒现象,同时实现CO和CO2的完全分离;通过在线镍催化将CO和CO2的检测转化为对CH4的检测,极大地提高检测灵敏度。结果显示,该方法对CO和CO2的检测互不干扰,两者都可在2~500 μL/L范围内呈现良好的线性相应,测定重复性好(RSD小于2%),准确度高。建立的GC-FID方法可直接用于SF6高压断路器中痕量CO及CO2的检测,为SF6相关电气设备潜伏性故障诊断提供了研究手段。

关键词: 气相色谱, 一氧化碳, 二氧化碳, 六氟化硫, 断路器故障

Abstract:

A reliable gas chromatography-flame ionization detector (GC-FID) method was developed for the accurate determination of trace CO and CO2 in high concentration of SF6. Using a combination of dual Porapak Q chromatographic columns with valve switching, SF6 was separated from the tested samples and blown out of the detection system, with the aim of ruling out the possibility of conversion column poisoning. Meanwhile, CO and CO2 were on-line separated and subsequently converted to CH4 in the presence of a nickel catalyst to increase the sensitivity for the determination of carbon-borne gases. The results showed that neither gas interfered with the determination of the other. Satisfactory linearities were achieved in the range 2-500 μL/L for both CO and CO2, with highly accurate and reproducible determination (RSD < 2%). The developed GC-FID method is applicable to the determination of gases lodged in high-voltage circuit breakers toward the analysis of trace CO and CO2, thus providing a tool for probing the potential breakdown of SF6-insulated equipment.

Key words: gas chromatography (GC), carbon monoxide, carbon dioxide, sulfur hexafluoride, breakdown of circuit breaker