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

doi:10.3724/SP.J.1123.2019.11012

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

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 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 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/Abstract

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

杨韧, 汪金星, 张悦, 王青, 岳宣峰. 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[J]. 色谱, 2020, 38(6): 702-707.

YANG Ren, WANG Jinxing, ZHANG Yue, WANG Qing, YUE Xuanfeng. 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[J]. Chinese Journal of Chromatography, 2020, 38(6): 702-707.

图/表 9

图1 具有SF6切割功能的阀柱组合GC分析系统

Fig. 1 Column-valve GC analytical system with SF6 exclusion a. sampling step; b. injecting step. Column A: short chromatographic column (Porapak Q, 183 cm×3.8 cm (6 ft×1/8″)); column B: long chromatographic column (Porapak Q, 488 cm×3.8 cm (16 ft×1/8″)).

图2 以TCD为检测器时混合气体分离的色谱图

Fig. 2 Chromatogram of mixed gas on thermal conductivity detector (TCD) The upper and lower insets show an enlarged view of the chromatographic peaks for CO2 and CO, respectively. All the insets elsewhere in this article follow the same protocol for representation.

图3 CO2含量为500 μL/L时不同含量CO的色谱图

Fig. 3 Chromatograms of CO at various contents with CO2 at 500 μL/L

图4 CO含量为500 μL/L时不同含量CO2的色谱图

Fig. 4 Chromatograms of CO2 at various contents with CO at 500 μL/L

表1 不同共存CO2含量下CO气相色谱检测的方法特性

Table 1 Characteristics of GC method for determination of CO in the presence of varying contents of CO2

CO₂ content/(μL/L)	CO calibration equation	Correlation coefficient(r)	Linear range/(μL/L)	Total calibration equation
y: peak area of CO; x: CO content, μL/L.
20	y=7.324x-6.103	0.9999	2-500	y=7.261x-4.508
100	y=7.116x-7.253	0.9968	2-500
500	y=7.343x-1.694	0.9999	2-500

表2 不同共存CO含量下CO2气相色谱检测的方法特性

Table 2 Characteristics of GC method for determination of CO2 in the presence of varying contents of CO

CO content/(μL/L)	CO₂ calibration equation	r	Linear range/(μL/L)	Total calibration equation
y: peak area of CO₂; x: CO₂ content, μL/L.
20	y=3.104x+0.111	0.9999	2-500	y=2.994x+1.671
100	y=2.880x+1.328	0.9999	2-500
500	y=2.999x+3.574	0.9998	2-500

图5 436 μL/L CO重复测定的色谱图

Fig. 5 Chromatograms for duplicate determination of 436 μL/L CO

表3 控制样的标准值和测定值

Table 3 Standard values and measured values for control samples

Control sample	Analyte	Standard value/(μL/L)	Measured value/(μL/L)^*
* n=6, .
Sample 1	CO	15.0	14.9±0.6
	CO₂	465.0	463.7±22.3
Sample 2	CO	40.0	39.4±1.6
	CO₂	60.0	59.2±2.6

图6 断路器中实际气体样品的色谱图

Fig. 6 Chromatograms of actual samples in circuit breakers Sample 1 and sample 2: samples from two suspicious circuit breakers; sample 3: a sample from a new circuit breaker.

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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

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

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