色谱 ›› 2020, Vol. 38 ›› Issue (5): 606-610.DOI: 10.3724/SP.J.1123.2019.10014

• 研究论文 • 上一篇    下一篇

基于自制气体循环系统测定全氟异丁腈中杂质成分

刘静, 黄青丹(), 王勇, 曾炼, 张亚茹   

  1. 广州供电局有限公司电力试验研究院, 广东 广州 510410
  • 收稿日期:2019-10-15 出版日期:2020-05-08 发布日期:2020-12-10
  • 通讯作者: 黄青丹
  • 作者简介:黄青丹.Tel:02087125511, E-mail:greengasguangzhou@163.com
  • 基金资助:
    南方电网公司重点科技项目(GZJKJXM20170330)

Determination of impurity components in the perfluoroisobutyrile based on home-made gas-circulating system

LIU Jing, HUANG Qingdan(), WANG Yong, ZENG Lian, ZHANG Yaru   

  1. Electric Power Test and Research Institute, Guangzhou Power Supply Co. Ltd., Guangzhou 510410, China
  • Received:2019-10-15 Online:2020-05-08 Published:2020-12-10
  • Contact: HUANG Qingdan
  • Supported by:
    Key Technology Project of China Southern Power Grid(GZJKJXM20170330)

摘要:

建立了基于自制全密闭进样系统的气相色谱-质谱测定全氟异丁腈(C4F7N)商品气中杂质的方法。待测气体在自制的密封系统内稀释并混合均匀,使用在线自动六通阀进样,采用Agilent GS-GASPRO色谱柱(30 m×0.32 mm×5 μm)分离,测定了国内某公司(DC公司)和国外某公司(AC公司)的全氟异丁腈绝缘气体的杂质成分。结果表明,全氟异丁腈商品气中含有微量的N2、O2、C3HF7和痕量的C3F6,其中AC公司的C4F7N商品气体中的杂质总含量为0.13%,C4F7N纯度为99.87%;DC公司的C4F7N商品气体中的杂质总含量为0.83%,C4F7N纯度为99.17%,两家公司的C4F7N含量均符合≥ 99%的标称含量。该法通过对C4F7N绝缘气体组成的测定,为其在电气绝缘输电设备中的应用提供基础成分数据。

关键词: 气相色谱-质谱, 杂质测定, 全氟异丁腈, 新型绝缘气体

Abstract:

A method for the determination of impurity components in perfluoroisobutyrile (C4F7N) gas was established by setting up a sealed pipe gas composition test system comprising an automatic six-way valve and gas chromatography-tandem mass spectrometry (GC-MS) apparatus. C4F7N commercial gases were purchased from an abroad company (AC company) and a domestic Chinese company (DC company). These gases were subjected to qualitative and quantitative analyses by our test system and separated on an Agilent GS-GASPRO column (30 m×0.32 mm×5 μm). The results showed that the C4F7N commercial gas contained N2, O2, C3HF7 and a trace amount of C3F6. In the C4F7N commercial gas from the AC company, the total amount of impurities was 0.13%, and the C4F7N content was 99.87%. In the C4F7N gas from DC Company, the total amount of impurities was 0.83%, and the C4F7N content was 99.17%. The C4F7N contents of the gases from both the companies were consistent with the claimed value (≥ 99%). The determination of the impurities C4F7N can be beneficial for the subsequent study of its insulation performance and thermal stability.

Key words: gas chromatography-tandem mass spectrometry(GC-MS), impurity determination, perfluoroisobutyrile (C4F7N), newly insulating gas