CN111679025A - Gas chromatography detection system and method for determination of perfluoroisobutyronitrile gas composition - Google Patents
Gas chromatography detection system and method for determination of perfluoroisobutyronitrile gas composition Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 38
- AASDJASZOZGYMM-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanenitrile Chemical compound FC(F)(F)C(F)(C#N)C(F)(F)F AASDJASZOZGYMM-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 22
- 239000000203 mixture Substances 0.000 title claims description 14
- 238000004458 analytical method Methods 0.000 claims abstract description 46
- 238000013022 venting Methods 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 94
- 239000012159 carrier gas Substances 0.000 claims description 41
- 239000012535 impurity Substances 0.000 claims description 32
- 239000000126 substance Substances 0.000 claims description 13
- 238000000926 separation method Methods 0.000 claims description 11
- 238000002347 injection Methods 0.000 claims description 10
- 239000007924 injection Substances 0.000 claims description 10
- 238000010926 purge Methods 0.000 claims description 6
- 238000005070 sampling Methods 0.000 claims description 6
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 5
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 238000000354 decomposition reaction Methods 0.000 abstract description 10
- 230000009286 beneficial effect Effects 0.000 abstract description 6
- 238000004587 chromatography analysis Methods 0.000 description 8
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 4
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 description 4
- 229960004065 perflutren Drugs 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 238000013461 design Methods 0.000 description 3
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- 102100039236 Histone H3.3 Human genes 0.000 description 1
- 101001035966 Homo sapiens Histone H3.3 Proteins 0.000 description 1
- 229910018503 SF6 Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 241000894007 species Species 0.000 description 1
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 1
- 229960000909 sulfur hexafluoride Drugs 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8872—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample impurities
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Abstract
本发明提供了一种用于测定全氟异丁腈气体成分的气相色谱检测系统及方法,包括:第一分析单元和第二分析单元;第一分析单元包括依次连接的第一切换阀、第三色谱柱、第三切换阀和第一检测器;第一切换阀上的第一接口与待测气体样品源连接;第三切换阀上设有第二放空阀。第二分析单元包括依次连接的第二切换阀、第一色谱柱、第二色谱柱、第四切换阀和第二检测器;第二切换阀上的第一接口与待测气体样品源连接;第二切换阀上设有第三放空阀;第四切换阀上设有第四放空阀。本发明提供的气相色谱系统,只需一台仪器即可实现对C4F7N‑CO2混合气体分解产物的全部组分的精确分析,有利于据此准确判断电气设备的运行状况;同时,缩短了分析所用的时间。
The invention provides a gas chromatography detection system and method for measuring perfluoroisobutyronitrile gas components, comprising: a first analysis unit and a second analysis unit; the first analysis unit includes a first switching valve, a second There are three chromatographic columns, a third switching valve and a first detector; the first interface on the first switching valve is connected with the gas sample source to be tested; the third switching valve is provided with a second vent valve. The second analysis unit includes a second switching valve, a first chromatographic column, a second chromatographic column, a fourth switching valve and a second detector connected in sequence; the first interface on the second switching valve is connected to the gas sample source to be measured; The second switching valve is provided with a third venting valve; the fourth switching valve is provided with a fourth venting valve. The gas chromatography system provided by the invention can realize the accurate analysis of all the components of the C 4 F 7 N-CO 2 mixed gas decomposition products with only one instrument, which is beneficial to accurately judge the operation status of the electrical equipment; , reducing the analysis time.
Description
技术领域technical field
本发明涉及分析化学技术领域,具体而言,涉及一种用于测定全氟异丁腈气体成分的气相色谱检测系统及方法。The invention relates to the technical field of analytical chemistry, in particular to a gas chromatography detection system and method for measuring perfluoroisobutyronitrile gas components.
背景技术Background technique
气体绝缘的电气设备通常使用六氟化硫(SF6)气体作为绝缘介质,但由于SF6具有较强的温室效应,其GWP值约为CO2的23900倍,这阻碍了我国乃至全球电网的绿色发展。因此寻找到电气性能与之相当且环境友好的SF6替代气体成为近年来国内外研究的热点。2014年,法国阿尔斯通(ALSTOM)从美国3M公司制冷剂目录中筛选出了一种名为 Novec™4710 的气体全氟异丁腈(C4F7N)。C4F7N的绝缘性能是同等条件下SF6的2.2倍以上,同时GWP(全球变暖潜能值)又远低于 SF6气体。但同样受困于液化温度较高的问题,ALSTOM 不得不将 Novec™ 4710 与 CO2 混合使用。可因为液化温度较高一般与CO2混合使用,混合后气体的绝缘性强度仍能达到同等条件下SF6的87%~96%。因其具备优异的性能成为良好的替代气体,美国通用公司已将其应用到145kV的GIS中。Gas-insulated electrical equipment usually uses sulfur hexafluoride (SF 6 ) gas as the insulating medium, but due to the strong greenhouse effect of SF 6 , its GWP value is about 23,900 times that of CO 2 , which hinders the power grid in China and even the world. ECO development. Therefore, it has become a hot research topic at home and abroad in recent years to find SF 6 substitute gas with comparable electrical properties and environmental friendliness. In 2014, French Alstom (ALSTOM) screened a gas perfluoroisobutyronitrile (C 4 F 7 N) named Novec™ 4710 from the refrigerant catalog of 3M Company in the United States. The insulation performance of C 4 F 7 N is more than 2.2 times that of SF 6 under the same conditions, and the GWP (Global Warming Potential) is much lower than that of SF 6 gas. But also suffering from higher liquefaction temperatures, ALSTOM had to mix Novec™ 4710 with CO 2 . But because the liquefaction temperature is higher, it is usually mixed with CO 2 , and the insulating strength of the mixed gas can still reach 87%~96% of SF 6 under the same conditions. Because of its excellent performance, it has become a good substitute gas, and American General Company has applied it to 145kV GIS.
在电气设备运行过程中,若设备发生故障,可能会发生局部放电等现象。在放电条件下C4F7N-CO2混合气体会发生分解,可能产生大量的CF3自由基、CN自由基、CF自由基,这些自由基结合会发生复杂的化学反应,生成如CF3CN等分解产物,通过检测这些杂质含量可以推断设备运行状况。目前市面上没有C4F7N-CO2混合气体的系统的检测方法,一般利用多台仪器进行检测,如TCD(热导检测器)、FTIR等,而所检测的杂质不能包括其分解产物的特征杂质,且检出限也无法令人满意,有效快捷测检测C4F7N-CO2混合气体是一个技术难题。During the operation of electrical equipment, if the equipment fails, partial discharge and other phenomena may occur. Under discharge conditions, the C 4 F 7 N-CO 2 mixed gas will decompose and may generate a large number of CF 3 radicals, CN radicals, and CF radicals. The combination of these radicals will cause complex chemical reactions, such as CF 3 . CN and other decomposition products, by detecting the content of these impurities, the operation status of the equipment can be inferred. At present, there is no systematic detection method for C 4 F 7 N-CO 2 mixed gas on the market. Generally, multiple instruments are used for detection, such as TCD (thermal conductivity detector), FTIR, etc., and the detected impurities cannot include its decomposition products. The characteristic impurities are not satisfactory, and the detection limit is unsatisfactory, so it is a technical problem to effectively and quickly detect the C 4 F 7 N-CO 2 mixed gas.
对于检测C4F7N的分解产物等杂质,目前报道的检测方法有傅里叶红外光谱(FTIR)、GC-MS等,且都是简单的检测,杂质种类也比较少,单独采用色谱对C4F7N的分解产物进行检测的系统和方法尚未见有报道。For the detection of impurities such as the decomposition products of C 4 F 7 N, the currently reported detection methods include Fourier transform infrared spectroscopy (FTIR), GC-MS, etc., and they are all simple detections with relatively few types of impurities. The system and method for detecting the decomposition products of C 4 F 7 N have not yet been reported.
发明内容SUMMARY OF THE INVENTION
鉴于此,本发明提出了一种用于测定全氟异丁腈气体成分的气相色谱检测系统及方法,旨在解决现有技术中对于C4F7N-CO2混合气体中杂质组分进行检测时检测效率较低的问题。In view of this, the present invention proposes a gas chromatographic detection system and method for measuring perfluoroisobutyronitrile gas components, aiming to solve the problem in the prior art for the detection of impurity components in C 4 F 7 N-CO 2 mixed gas. The problem of low detection efficiency during detection.
一个方面,本发明提出了一种用于测定全氟异丁腈气体成分的气相色谱检测系统,包括:第一分析单元和第二分析单元;所述第一分析单元包括依次连接的第一切换阀、第三色谱柱、第三切换阀和第一检测器;所述第一切换阀上的第一接口与待测气体样品源连接;所述第三切换阀上设有第二放空阀;所述第二分析单元包括依次连接的第二切换阀、第一色谱柱、第二色谱柱、第四切换阀和第二检测器;所述第二切换阀上的第一接口与待测气体样品源连接;所述第二切换阀上设有第三放空阀;所述第四切换阀上设有第四放空阀。In one aspect, the present invention provides a gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, comprising: a first analysis unit and a second analysis unit; the first analysis unit includes a first switch connected in sequence a valve, a third chromatographic column, a third switching valve and a first detector; the first interface on the first switching valve is connected to the gas sample source to be measured; the third switching valve is provided with a second vent valve; The second analysis unit includes a second switching valve, a first chromatographic column, a second chromatographic column, a fourth switching valve and a second detector connected in sequence; the first interface on the second switching valve is connected to the gas to be measured The sample source is connected; the second switching valve is provided with a third venting valve; the fourth switching valve is provided with a fourth venting valve.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,第一载气与所述第一切换阀的第五接口连接;待测气体样品进口与所述第一切换阀的第一接口连接;所述第一切换阀的第二接口和所述第二切换阀的第一接口连接;所述第一切换阀的第三接口与所述第一切换阀的第六接口连接的管路上设有第一定量管;所述第一切换阀的第四接口和所述第三色谱柱的第一端连接。Further, in the above-mentioned gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, the first carrier gas is connected to the fifth interface of the first switching valve; the gas sample inlet to be tested is connected to the first switching valve. The first interface of the first switching valve is connected to the first interface of the second switching valve; the third interface of the first switching valve is connected to the sixth interface of the first switching valve The connected pipeline is provided with a first quantitative pipe; the fourth interface of the first switching valve is connected with the first end of the third chromatographic column.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,第四载气与所述第二切换阀的第四接口连接,第三载气与所述第二切换阀的第七接口连接;所述第三放空阀与所述第二切换阀的第八接口连接,待测气体样品出口与所述第二切换阀的第二接口连接;所述第二切换阀的第三接口与所述第二切换阀的第十接口连接的管路上设有第二定量管;所述第二切换阀的第五接口与所述第二切换阀的第九接口连接的管路上设有所述第一色谱柱;所述第二切换阀的第六接口与所述第四切换阀的第六接口连接的管路上设有所述第二色谱柱。Further, in the above-mentioned gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, the fourth carrier gas is connected to the fourth interface of the second switching valve, and the third carrier gas is connected to the second switching valve. The seventh port is connected; the third vent valve is connected with the eighth port of the second switching valve, the gas sample outlet to be tested is connected with the second port of the second switching valve; the third port of the second switching valve is connected A second quantitative pipe is provided on the pipeline connecting the three ports with the tenth port of the second switching valve; the pipeline connecting the fifth port of the second switching valve and the ninth port of the second switching valve is provided with The first chromatographic column is provided; the second chromatographic column is provided on the pipeline connecting the sixth interface of the second switching valve and the sixth interface of the fourth switching valve.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,第二载气与所述第三切换阀的第三接口连接,所述第二放空阀与所述第三切换阀的第一接口连接,所述第一检测器与所述第三切换阀的第五接口连接;所述第三色谱柱的另一端与所述第三切换阀的第六接口连接;所述第三切换阀的第二接口与所述第三切换阀的第四接口连接。Further, in the above-mentioned gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, the second carrier gas is connected to the third interface of the third switching valve, and the second vent valve is connected to the third switching valve. the first port of the valve is connected, the first detector is connected with the fifth port of the third switching valve; the other end of the third chromatographic column is connected with the sixth port of the third switching valve; the The second port of the third switching valve is connected to the fourth port of the third switching valve.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,所述第五载气与所述第四切换阀的第三接口连接,所述第四放空阀与所述第四切换阀的第一接口连接,所述第二检测器与所述第四切换阀的第五接口连接;所述第四切换阀的第二接口与所述第四切换阀的第四接口连接。Further, in the above-mentioned gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, the fifth carrier gas is connected to the third interface of the fourth switching valve, and the fourth vent valve is connected to the third port of the fourth switching valve. The first interface of the four switching valve is connected, the second detector is connected with the fifth interface of the fourth switching valve; the second interface of the fourth switching valve is connected with the fourth interface of the fourth switching valve .
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,所述第一检测器和所述第二检测器均为脉冲氦离子化检测器。Further, in the above gas chromatography detection system for measuring perfluoroisobutyronitrile gas components, the first detector and the second detector are both pulsed helium ionization detectors.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,所述第一切换阀、所述第三切换阀和所述第四切换阀为六通吹扫气动切换阀,所述第二切换阀为十通吹扫气动切换阀。Further, in the above-mentioned gas chromatography detection system for measuring perfluoroisobutyronitrile gas composition, the first switching valve, the third switching valve and the fourth switching valve are six-way purge pneumatic switching valves, The second switching valve is a ten-way purge pneumatic switching valve.
进一步地,上述用于测定全氟异丁腈气体成分的气相色谱检测系统中,所述第一色谱柱为C4F7N专用分析预柱;所述第二色谱柱为C4F7N专用分析柱,所述第三色谱柱为氟碳化合物分析毛细柱。Further, in the above-mentioned gas chromatographic detection system for measuring perfluoroisobutyronitrile gas components, the first chromatographic column is a C4F7N special analysis pre-column; the second chromatographic column is a C4F7N special analysis column, and the third The chromatographic column is a capillary column for fluorocarbon analysis.
本发明中,只需一台仪器即可实现对C4F7N-CO2混合气体分解产物的全部组分的精确分析,有利于据此准确判断电气设备的运行状况;同时,节省了劳动力和测试时间、也减少了仪器投资费用,使得使用成本大幅度降低,相应的也减少了仪器维护成本;此外,采用一台仪器分析可以减少采样量,减少样品气的使用量和样品使用后的处理量,更加安全环保。In the present invention, only one instrument can realize the accurate analysis of all components of the decomposition products of the C 4 F 7 N-CO 2 mixed gas, which is beneficial to accurately determine the operation status of the electrical equipment; meanwhile, labor is saved It also reduces the investment cost of the instrument, which greatly reduces the cost of use, and correspondingly reduces the maintenance cost of the instrument; in addition, using one instrument for analysis can reduce the amount of sampling, the amount of sample gas used, and the amount of sample gas after use. Processing capacity, more safety and environmental protection.
另一方面,本发明还提出了一种用于测定全氟异丁腈气体成分的气相色谱分析方法,包括以下步骤:步骤(1),第一切换阀采用阀进样的方式进样,经过第一定量管的C4F7N-CO2混合气体中的大部分氟碳类化合物经过第三色谱柱分离后,切换第三切换阀将分离的所述氟碳化合物切换到第一检测器中响应出峰;步骤(2),第二切换阀采用反吹进样的方式进行,经过第二定量管的C4F7N-CO2混合气体,先通过第一色谱柱实现待测气体样品的预分离,使得Air、CO、CF4、CO2和C2F6先进入第二色谱柱,然后切换第二切换阀反吹预分离得到的其他杂质组分;切换第四切换阀将所述第二色谱柱分离的杂质组分Air、CO、CF4、CO2和C2F6分别切换到第二检测器中响应出峰。On the other hand, the present invention also proposes a gas chromatographic analysis method for measuring perfluoroisobutyronitrile gas components, comprising the following steps: step (1), the first switching valve is injected by means of valve injection, and after After most of the fluorocarbons in the C 4 F 7 N-CO 2 mixed gas in the first quantitative tube are separated by the third chromatographic column, the third switching valve is switched to switch the separated fluorocarbons to the first detection In step (2), the second switching valve adopts the method of backflushing and sampling, and the C 4 F 7 N-CO 2 mixed gas passing through the second quantitative tube first passes through the first chromatographic column to realize the test to be detected. Pre-separation of gas samples, so that Air, CO, CF 4 , CO 2 and C 2 F 6 first enter the second chromatographic column, and then switch the second switching valve to backflush other impurity components obtained by pre-separation; switch the fourth switching valve The impurity components Air, CO, CF 4 , CO 2 and C 2 F 6 separated by the second chromatographic column are respectively switched to the second detector to respond to peaks.
进一步地,上述分析全氟异丁腈气体成分的方法中,所述进样步骤如下:Further, in the above-mentioned method for analyzing perfluoroisobutyronitrile gas components, the sample introduction step is as follows:
切换所述第一切换阀,第一载气携带所述第一定量管中的待测气体样品进入所述第三色谱柱,同时通过三通和第一放空阀进行分流,将所述第三色谱柱中出峰在C3F8之前的物质通过第二放空阀放空;切换所述第三切换阀,使得C3F8及其之后的杂质组分分别进入第一检测器出峰;待C2F5CN出峰完成后,切换所述第三切换阀回到初始状态,对C4F7N进行放空;The first switching valve is switched, and the first carrier gas carries the gas sample to be measured in the first quantitative tube into the third chromatographic column, and at the same time, the flow is split through the three-way and the first vent valve, and the third chromatographic column is separated. In the three chromatographic columns, the substances with peaks before C 3 F 8 are vented through the second vent valve; the third switching valve is switched, so that C 3 F 8 and the impurity components after it enter the first detector respectively to emit peaks; After the C 2 F 5 CN peak is completed, the third switching valve is switched back to the initial state, and the C 4 F 7 N is vented;
切换所述第二切换阀和所述第四切换阀,第四载气携带所述第二定量管中的待测气体样品进入所述第一色谱柱,当所述第一色谱柱中C2F6和出峰在C2F6之前的物质进入所述第二色谱柱后切换所述第二切换阀,使得出峰在C2F6之后的物质通过第三放空阀反吹放空;同时第三载气携带从所述第二色谱柱中分离的杂质进入第二检测器中完成出峰,待CF4出峰完成后,切换所述第四切换阀使得通过第四放空阀放空,当CO2完全放空后,切换所述第四切换阀回到初始状态,使得C2F6出峰。The second switching valve and the fourth switching valve are switched, and the fourth carrier gas carries the gas sample to be measured in the second quantitative tube into the first chromatographic column. When C 2 in the first chromatographic column The second switching valve is switched after F 6 and the substance whose peak is before C 2 F 6 enters the second chromatographic column, so that the substance whose peak is after C 2 F 6 is backflushed and vented through the third vent valve; The third carrier gas carries the impurities separated from the second chromatographic column into the second detector to complete the peak output. After the CF4 peak is completed, the fourth switching valve is switched so that the fourth vent valve is vented. When After the CO 2 is completely vented, the fourth switching valve is switched back to the initial state, so that the C 2 F 6 peaks.
本发明提供的分析全氟异丁腈气体成分的方法,通过一次进样就可以完成C4F7N-CO2混合气体中各种杂质的分析,避免多次进样引入的仪器和人为误差,提高了分析的准确性且分析时间短,有利于相关电气设备使用人员根据分析结果及时准确的判断出电气设备的运行状况进而及时采取相应的安全措施。The method for analyzing perfluoroisobutyronitrile gas components provided by the invention can complete the analysis of various impurities in the C 4 F 7 N-CO 2 mixed gas through one sample injection, and avoid instrument and human errors introduced by multiple sample injections , which improves the accuracy of the analysis and the analysis time is short, which is beneficial for the relevant electrical equipment users to timely and accurately judge the operation status of the electrical equipment according to the analysis results and take corresponding safety measures in time.
附图说明Description of drawings
通过阅读下文优选实施方式的详细描述,各种其他的优点和益处对于本领域普通技术人员将变得清楚明了。附图仅用于示出优选实施方式的目的,而并不认为是对本发明的限制。而且在整个附图中,用相同的参考符号表示相同的部件。在附图中:Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are for the purpose of illustrating preferred embodiments only and are not to be considered limiting of the invention. Also, the same components are denoted by the same reference numerals throughout the drawings. In the attached image:
图1为本发明实施例提供的用于测定全氟异丁腈气体成分的气相色谱检测系统的连接结构示意图;Fig. 1 is the connection structure schematic diagram of the gas chromatography detection system for measuring perfluoroisobutyronitrile gas composition provided by the embodiment of the present invention;
图2为本发明实施例中第一切换阀取样结束,通过三通和第一放空阀进行分流、通过第二放空阀放空CO2的流程示意图;Fig. 2 is the schematic flow chart of the first switching valve sampling in the embodiment of the present invention, shunting through the three-way and the first vent valve, and venting CO 2 through the second vent valve;
图3为本发明实施例中C3F8等杂质进入第一检测器,同时通过第三切换阀对C4F7N进行放空的流程示意图;FIG. 3 is a schematic flow chart showing that impurities such as C 3 F 8 enter the first detector and simultaneously vent C 4 F 7 N through a third switching valve in an embodiment of the present invention;
图4为本发明实施例中第四载气带着第二定量管中的样品进入第一色谱柱且第一色谱柱中C2F6和出峰在C2F6之前的物质全部进入第二色谱柱进行分离的流程示意图;Fig. 4 shows that the fourth carrier gas carries the sample in the second quantitative tube into the first chromatographic column, and all the C 2 F 6 and the substances with peaks before C 2 F 6 in the first chromatographic column enter the first chromatographic column. Schematic flow chart of separation by two chromatographic columns;
图5为本发明实施例中通过第三放空阀放空反吹出峰在C2F6之后的物质的流程示意图;Fig. 5 is the schematic flow chart of venting and backflushing the substance behind C 2 F 6 through the third vent valve in the embodiment of the present invention;
图6为本发明实施例中第一检测器中各杂质气体成分的色谱分析图;6 is a chromatographic analysis diagram of each impurity gas component in the first detector in the embodiment of the present invention;
图7本发明实施例中第二检测器中各杂质气体成分的色谱分析图。FIG. 7 is a chromatographic analysis diagram of each impurity gas component in the second detector in the embodiment of the present invention.
图中:1-第一切换阀;2-第二切换阀;3-第三切换阀;4-第四切换阀;5-第一色谱柱;6-第二色谱柱;7-第三色谱柱;8-第一载气;9-第二载气;10-第三载气;11-第四载气;12-第五载气;13-第一定量管;14-第二定量管;15-待测气体样品进口;16-待测气体样品出口;17-第一放空阀;18-第二放空阀;19-第三放空阀;20-第四放空阀;21-三通;22-第一检测器;23-第二检测器。In the figure: 1- the first switching valve; 2- the second switching valve; 3- the third switching valve; 4- the fourth switching valve; 5- the first chromatographic column; 6- the second chromatographic column; 7- the third chromatographic column Column; 8-first carrier gas; 9-second carrier gas; 10-third carrier gas; 11-fourth carrier gas; 12-fifth carrier gas; 13-first quantitative tube; 14-second quantitative Tube; 15-Gas sample inlet to be tested; 16-Gas sample outlet to be tested; 17-First vent valve; 18-Second vent valve; 19-Third vent valve; 20-Fourth vent valve; 21-Tee ; 22 - the first detector; 23 - the second detector.
具体实施方式Detailed ways
下面将参照附图更详细地描述本公开的示例性实施例。虽然附图中显示了本公开的示例性实施例,然而应当理解,可以以各种形式实现本公开而不应被这里阐述的实施例所限制。相反,提供这些实施例是为了能够更透彻地理解本公开,并且能够将本公开的范围完整的传达给本领域的技术人员。需要说明的是,在不冲突的情况下,本发明中的实施例及实施例中的特征可以相互组合。下面将参考附图并结合实施例来详细说明本发明。Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited by the embodiments set forth herein. Rather, these embodiments are provided so that the present disclosure will be more thoroughly understood, and will fully convey the scope of the present disclosure to those skilled in the art. It should be noted that the embodiments of the present invention and the features of the embodiments may be combined with each other under the condition of no conflict. The present invention will be described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
参阅图1,本发明实施例的用于测定全氟异丁腈气体成分的气相色谱检测系统包括:第一分析单元和第二分析单元;其中,第一分析单元包括依次连接的第一切换阀1、第三色谱柱7、第三切换阀3和第一检测器22;所述第一切换阀1上的第一接口与待测气体样品源连接;所述第三切换阀3上设有第二放空阀18。Referring to FIG. 1 , a gas chromatography detection system for measuring perfluoroisobutyronitrile gas components according to an embodiment of the present invention includes: a first analysis unit and a second analysis unit; wherein the first analysis unit includes a first switching valve connected in
第二分析单元包括依次连接的第二切换阀2、第一色谱柱5、第二色谱柱6、第四切换阀4和第二检测器23;所述第二切换阀2上的第一接口201与待测气体样品源连接;所述第二切换阀2上设有第三放空阀19;所述第四切换阀4上设有第四放空阀20。The second analysis unit includes a
具体而言,本发明中待测气体为C4F7N-CO2混合气体,本实施例中通过第一分析单元测定C4F7N-CO2混合气体分解产物中的C3F8(八氟丙烷)、C2HF5Cl(R125)、C2H3F3(R143a)、C2H2F4(R134a)、C3F6(六氟丙烯)和C2F5CN的含量;通过第二分析单元测定C4F7N-CO2混合气体中分解产物中的Air、CO、CF4和C2F6的含量。第一切换阀1、第三色谱柱7、第三切换阀3的各个接口以及相应的接口与第一检测器22之间均通过气路管道连接;第二切换阀2、第一色谱柱5、第二色谱柱6、第四切换阀4上各个接口以及相应的接口和第二检测器23之间均通过气路管线连接。第二放空阀18、第三放空阀19和第四放空阀20可以均为针阀。Specifically, the gas to be measured in the present invention is a C 4 F 7 N-CO 2 mixed gas. In this embodiment, the first analysis unit is used to measure the C 3 F 8 in the decomposition product of the C 4 F 7 N-CO 2 mixed gas. (Octafluoropropane), C 2 HF 5 Cl (R125), C 2 H 3 F 3 (R143a), C 2 H 2 F 4 (R134a), C 3 F 6 (hexafluoropropene) and C 2 F 5 CN The content of Air, CO, CF 4 and C 2 F 6 in the decomposition product in the C 4 F 7 N-CO 2 mixed gas was determined by the second analysis unit. The interfaces of the
优选的,所述第一切换阀1、所述第三切换阀3和所述第四切换阀4为六通吹扫气动切换阀,所述第二切换阀2为十通吹扫气动切换阀。通过合理的对各个切换阀进行切换,可以有效的简化色谱分析的流程,缩短色谱分析时间,大大提高了色谱分析的工作效率。Preferably, the
优选的,所述第一色谱柱5为C4F7N专用分析预柱,例如可用极性高的分子柱(强极性和中极性的分子柱),以对可以实现空气、C2F6等和C4F7N的预分离;所述第二色谱柱6为C4F7N专用分析柱,例如可采用分子筛色谱柱,实现空气、CO、CF4、CO2和C2F6的分离,所述第三色谱柱7为氟碳类化合物分析毛细柱,对C4F7N分解产物C3F8(八氟丙烷)、C2HF5Cl(R125)、C2H3F3(R143a)、C2H2F4(R134a)、C3F6(六氟丙烯)和C2F5CN进行分离。选择合适的色谱柱可以针对特定的杂质组分进行分离,避免杂质之间的干扰。Preferably, the
所述第一检测器22和所述第二检测器23可以均为脉冲氦离子化检测器,保证了较高的分析灵敏度,可以使得所有组分检测限达到50ppb。The
为了灵活控制第一分析单元,优选的,第一载气8与所述第一切换阀1的第五接口连接;第一切换阀1的第一接口与待测气体样品进口15连接;所述第一切换阀1的第二接口102和所述第二切换阀2的第一接口201连接,也就是说,所述第二切换阀2通过所述第一切换阀1的第二接口与待测气体样品管路连接。所述第一切换阀1的第三接口103与所述第一切换阀1的第六接口106连接的管路上设有第一定量管13;所述第一切换阀1的第四接口104和所述第三色谱柱7的第一端连接。In order to flexibly control the first analysis unit, preferably, the
优选的,所述第一切换阀1与所述第三色谱柱7之间设置有分流单元。更具体的,分流单元包括:三通21和第一放空阀17;其中,所述三通的一端与所述第三色谱柱的第二端连通,所述三通21的另一端与所述第一放空阀17连通。也就是在第一切换阀1和第三色谱柱7连接的管路上设有三通21,所述三通21的另一端连接有第一放空阀17。需要说明的是,第三色谱柱7的第一端可以为进口端,第二端可以为出口端。Preferably, a flow dividing unit is provided between the
本实施例中,在第一切换阀1上设置第一定量管13,可以精确控制样品的用量,以更好的节约样品使用量。第一放空阀17可以为针阀。In this embodiment, the first
三通21的规格与第三色谱柱7中的毛细柱接口相匹配,专用的毛细柱接口三通21降低了死体积,降低了噪音,有效避免了空气干扰。通过三通21和第一放空阀17进行分流,避免进入第三色谱柱7中的待测气体样品的含量不至于过高,有利于延长第三色谱柱7的毛细柱的寿命,且降低了第三色谱柱7中主峰拖尾的干扰问题。The specification of the
第二载气9与所述第三切换阀3的第三接口33连接,所述第二放空阀18与所述第三切换阀3的第一接口31连接,所述第一检测器22与所述第三切换阀3的第五接口35连接;所述第三色谱柱7的另一端与所述第三切换阀3的第六接口36连接;所述第三切换阀3的第二接口32与所述第三切换阀3的第四接口34连接。此流程设计确保了C4F7N和CO2的放空,可以有效避免主峰进入第一检测器22,影响杂质含量的分析。The
为了灵活控制第二分析单元,优选的,第四载气11与所述第二切换阀2的第四接口204连接,第三载气10与所述第二切换阀2的第七接口207连接;所述第三放空阀19与所述第二切换阀2的第八接口208连接,待测气体样品出口16与所述第二切换阀2的第二接口202连接;所述第二切换阀2的第三接口203与所述第二切换阀2的第十接口210连接的管路上设有第二定量管14;所述第二切换阀2的第五接口205与所述第二切换阀2的第九接口209连接的管路上设有所述第一色谱柱5;所述第二切换阀2的第六接口206与所述第四切换阀4的第六接口46连接的管路上设有所述第二色谱柱6。此反吹流程设计避免了C4F7N进入第二检测器23且缩短了分析时间。其中,在检测过程中,为了实现反吹操作的灵活性,优选以第二切换阀2的第四进口作为反吹气进口。在第二切换阀2上设置第二定量管14,可以精确控制样品的用量,以更好的节约样品使用量。In order to flexibly control the second analysis unit, preferably, the
所述第五载气12与所述第四切换阀4的第三接口43连接,所述第四放空阀20与所述第四切换阀4的第一接口41连接,所述第二检测器23与所述第四切换阀4的第五接口45连接;所述第四切换阀4的第二接口42与所述第四切换阀4的第四接口44连接。此流程设计避免CO2进入第二检测器23。本申请中所用的第一载气8、第二载气9、第三载气10、第四载气11和第五载气12为99.999% 高纯氦气。The
上述显然可以得出,本实施例中提供的用于测定全氟异丁腈气体成分的气相色谱检测系统,只需一台仪器即可实现对C4F7N-CO2混合气体分解产物的全部组分的精确分析,有利于据此准确判断电气设备的运行状况;同时,节省了劳动力和测试时间、也减少了仪器投资费用,使得使用成本大幅度降低,相应的也减少了仪器维护成本;此外,采用一台仪器分析可以减少采样量,减少样品气的使用量和样品使用后的处理量,更加安全环保。It can be clearly drawn from the above that the gas chromatographic detection system provided in this embodiment for measuring the gas composition of perfluoroisobutyronitrile only needs one instrument to realize the detection of C 4 F 7 N-CO 2 mixed gas decomposition products. Accurate analysis of all components is beneficial to accurately determine the operating status of electrical equipment; at the same time, labor and testing time are saved, instrument investment costs are also reduced, the use cost is greatly reduced, and the instrument maintenance cost is correspondingly reduced. ; In addition, the use of one instrument for analysis can reduce the amount of sampling, the amount of sample gas used and the amount of sample processing after use, which is safer and more environmentally friendly.
方法实施例:Method example:
本发明实施例提供的分析全氟异丁腈气体成分方法步骤如下:The steps of the method for analyzing the composition of perfluoroisobutyronitrile gas provided in the embodiment of the present invention are as follows:
步骤S1,第一切换阀采用阀进样的方式进样,经过第一定量管的C4F7N-CO2混合气体中的大部分氟碳类化合物经过第三色谱柱分离后,切换第三切换阀3将分离的所述氟碳化合物切换到第一检测器中响应出峰。这里的大部分氟碳化合物包括C3F8(八氟丙烷)、C2HF5Cl(R125)、C2H3F3(R143a)、C2H2F4(R134a)、C3F6(六氟丙烯)和C2F5CN。In step S1, the first switching valve is injected by means of valve injection, and most of the fluorocarbons in the C 4 F 7 N-CO 2 mixed gas passing through the first quantitative tube are separated by the third chromatographic column, and then switched. The
该步骤中的具体进样过程如下:The specific injection process in this step is as follows:
参阅图2,切换所述第一切换阀1,第一载气8携带所述第一定量管13中的待测气体样品进入所述第三色谱柱7,同时通过三通和第一放空阀进行分流,将所述第三色谱柱中出峰在C3F8之前的物质通过第二放空阀放空。这里的出峰在C3F8之前的物质主要指CO2。切换第一切换阀1时,使得第一载气8与第一切换阀的第五接口105相连、同时,第一切换阀1的第五接口105、第六接口106、第一定量管13、第三接口103、第四接口104、三通21和第三色谱柱7、第三切换阀3的第六接口36及第一接口31依次相连,第三切换阀的第一接口31与第二放空阀18的一端相连,以便于将不需要分析的成分(主要为C4F7N)通过第二放空阀放空。Referring to FIG. 2, the
参阅图3,切换所述第三切换阀3,使得C3F8及出峰在其之后的杂质组分分别进入第一检测器22出峰;待C2F5CN出峰完成后,切换所述第三切换阀3回到初始状态,对C4F7N进行放空,至此第一分析单元的分析工作结束。其中:Referring to FIG. 3 , switch the
切换第三切换阀3时,使得第三色谱柱7、第三切换阀3的第六接口36和第一检测器22的进口依次相连,使得C3F8及出峰在其之后的杂质组分进入第一检测器22中。将第三切换阀3切换回到初始状态,即第三切换阀3的第六接口36与第一接口31相连,第一接口31与第二放空阀18的一端相连,第三接口33与第二接口32连接、第四接口34与第五接口35连接的状态,以将从第三色谱柱7分离出来的C4F7N放空。至此,可以得到如图6所示的分析谱图,6图为50ppm左右的C3F8(八氟丙烷)、C2HF5Cl(R125)、C2H3F3(R143a)、C2H2F4(R134a)、C3F6(六氟丙烯)和C2F5CN的标气谱图。When switching the
步骤S2,第二切换阀2采用反吹进样的方式进行,经过第二定量管的C4F7N-CO2混合气体,先通过第一色谱柱实现待测气体样品的预分离,使得Air、CO、CF4、CO2和C2F6先进入第二色谱柱,然后切换第二切换阀反吹预分离得到的其他杂质组分;切换第四切换阀将所述第二色谱柱分离的杂质组分Air、CO、CF4、CO2和C2F6分别切换到第二检测器中响应出峰。In step S2, the
该步骤中的具体的进样过程如下:The specific injection process in this step is as follows:
阅图4,切换所述第二切换阀2和所述第四切换阀4,第四载气11携带所述第二定量管14中的待测气体样品进入所述第一色谱柱5,参阅图5,当所述第一色谱柱5中C2F6和出峰在C2F6之前的物质进入所述第二色谱柱6后切换所述第二切换阀2,使得出峰在C2F6之后的物质通过第三放空阀19反吹放空;同时第三载气10携带从所述第二色谱柱6中分离的其余杂质进入第二检测器23中完成出峰;参阅图1,当CF4出峰完成后,切换所述第四切换阀4使得CO2通过第四放空阀20放空,参阅图5,当CO2完全放空后,切换所述第四切换阀4,使得C2F6出峰。第二检测器23中分析的杂质气体组分为空气、CO、CF4和C2F6。4, switch the
参阅图4,第一次切换第二切换阀2时,第四载气11与第二切换阀2的第四接口连接,并经第二切换阀2的第三接口203进入第二定量管14中,携带第二定量管14中的C4F7N-CO2混合气体依次通过第十接口210和第九接口209进入第一色谱柱5中进行分离后,使得出峰在C2F6之前的物质经第一色谱柱5的出口、第二切换阀2的第五接口205、第六接口206进入第二色谱柱6中。Referring to FIG. 4 , when the
参阅图5,第二次切换第二切换阀2时,使得第四载气11与第二切换阀2的第四接口204连接后,使得第四载气11携带出峰在C2F6之后的物质依次经第五接口205、第一色谱柱5、第九接口209、第八接口208、与第八接口208连接的第三放空阀19放空。同时,第三载气10与第二切换阀2的第七接口相连,同时,切换第四切换阀4,使得第二色谱柱6的出口、第四切换阀4的第六接口46、第五接口45和第二检测器23依次相连,以将从第一色谱柱5分离的杂质组分携带至第二色谱柱6中进行分离后,最终携带至第二检测器23中。Referring to FIG. 5 , when the
再次参阅图1,待CF4出峰完成后,切换第四切换阀4,使得第四切换阀4的第六接口与第一接口相连,第一接口与第四放空阀20的一端相连,以将CO2通过第四放空阀20放空。参阅图5,待CO2放空后,再次切换第四切换阀4切换至如使得第二色谱柱6、第四切换阀4的第六接口、第五接口与第二检测器23连接,使得C2F6出峰;最后切换第四切换阀4回到如图1所示的状态,分析结束,得到如图7所示的分析谱图,图7为160ppm的空气,50ppm左右的CO、CF4和C2F6的标气谱图。Referring to FIG. 1 again, after the peaking of CF 4 is completed, the
上述步骤S1和步骤S2可以同时进行实现一次进样,通过合理的切换各个分析单元中的切换阀,简化了色谱分析的流程,有效避免其杂质之间的干扰,各杂质组分的检出限可达到50ppb ,实现了C4F7N-CO2混合气体中杂质的全分析。The above steps S1 and S2 can be performed at the same time to realize one sample injection. By reasonably switching the switching valves in each analysis unit, the process of chromatographic analysis is simplified, the interference between impurities is effectively avoided, and the detection limit of each impurity component is It can reach 50ppb, realizing the full analysis of impurities in C 4 F 7 N-CO 2 mixed gas.
可以看出,本发明通过一次进样就可以完成C4F7N-CO2混合气体中各种杂质的分析,避免多次进样引入的仪器和人为误差,提高了分析的准确性且分析时间短,有利于相关电气设备使用人员根据分析结果及时准确的判断出电气设备的运行状况进而及时采取相应的安全措施。It can be seen that the present invention can complete the analysis of various impurities in the C 4 F 7 N-CO 2 mixed gas through one sample injection, avoid instrumental and human errors introduced by multiple sample injections, and improve the accuracy of analysis and analysis. The time is short, which is beneficial for the relevant electrical equipment users to timely and accurately judge the operation status of the electrical equipment according to the analysis results, and then take corresponding safety measures in time.
显然,本领域的技术人员可以对本发明进行各种改动和变型而不脱离本发明的精神和范围。这样,倘若本发明的这些修改和变型属于本发明权利要求及其等同技术的范围之内,则本发明也意图包含这些改动和变型在内。It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention. Thus, provided that these modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include these modifications and variations.
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