CN115639264A - SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof - Google Patents
SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof Download PDFInfo
- Publication number
- CN115639264A CN115639264A CN202211308716.9A CN202211308716A CN115639264A CN 115639264 A CN115639264 A CN 115639264A CN 202211308716 A CN202211308716 A CN 202211308716A CN 115639264 A CN115639264 A CN 115639264A
- Authority
- CN
- China
- Prior art keywords
- sample
- gas
- insulating gas
- atmospheric pressure
- negative ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000001514 detection method Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000005070 sampling Methods 0.000 claims abstract description 47
- 238000010438 heat treatment Methods 0.000 claims abstract description 33
- 238000009413 insulation Methods 0.000 claims abstract description 29
- 238000010926 purge Methods 0.000 claims abstract description 27
- 239000000919 ceramic Substances 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000004458 analytical method Methods 0.000 claims abstract description 15
- 238000000451 chemical ionisation Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 230000005855 radiation Effects 0.000 claims abstract description 4
- 238000002347 injection Methods 0.000 claims description 13
- 239000007924 injection Substances 0.000 claims description 13
- 238000004321 preservation Methods 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 8
- 230000035945 sensitivity Effects 0.000 abstract description 8
- 238000000752 ionisation method Methods 0.000 abstract description 7
- 238000000691 measurement method Methods 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 132
- 150000002500 ions Chemical class 0.000 description 29
- 150000001450 anions Chemical class 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 229910018503 SF6 Inorganic materials 0.000 description 4
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 4
- 229960000909 sulfur hexafluoride Drugs 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000065 atmospheric pressure chemical ionisation Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000001153 fluoro group Chemical group F* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
本发明一种绝缘气体中SO2的大气压负离子检测装置及其使用方法,绝缘气体中SO2的大气压负离子检测装置包括注射泵、开关阀、进样瓶、保温层和飞行时间质谱仪,其中飞行时间质谱仪采用的电离源源为63Ni,电离方式为大气压下化学电离,通过开关阀及进气口连接的样品吹扫气体将绝缘气体样品载带至电离源内,进行高效电离和分析,进样瓶外设置有保温层,保温层内布陶瓷加热层、外部设置加热器连接线连接电源,通电后通过热辐射实现快速升温和降温,用以加热保温,从而干燥水分,水分干燥效果好,能有效防止水分进入至飞行时间质谱仪的电源内部影响检测结果,测定方法简单、样品消耗量低、分析速度快,检测灵敏度能达到ppb量级。
The present invention is a kind of SO2 in the insulating gas Atmospheric pressure negative ion detection device and using method thereof, the SO2 atmospheric pressure negative ion detection device in the insulating gas comprises a syringe pump, a switch valve, a sampling bottle, an insulating layer and a time-of-flight mass spectrometer, wherein the flight The ionization source used by the time mass spectrometer is 63 Ni, and the ionization method is chemical ionization under atmospheric pressure. The sample purge gas connected to the switch valve and the gas inlet carries the insulating gas sample into the ionization source for efficient ionization and analysis. There is an insulation layer on the outside of the bottle, a ceramic heating layer is placed inside the insulation layer, and a heater connection line is installed on the outside to connect to the power supply. After the power is turned on, the rapid heating and cooling can be achieved through thermal radiation, which is used for heating and heat preservation, so as to dry the moisture. The moisture drying effect is good and can Effectively prevent moisture from entering the power supply of the time-of-flight mass spectrometer and affect the detection results. The measurement method is simple, the sample consumption is low, the analysis speed is fast, and the detection sensitivity can reach the ppb level.
Description
技术领域technical field
本发明涉及电气设备中绝缘气体分解产物的检测设备及检测方法技术领域,具体涉及一种绝缘气体中SO2的大气压负离子检测装置及其使用方法。The invention relates to the technical field of detection equipment and a detection method for decomposition products of insulating gas in electrical equipment, in particular to an atmospheric - pressure negative ion detection device for SO2 in insulating gas and a method for using the same.
背景技术Background technique
SF6气体已有百年历史,它是法国两位化学家Moissan和Lebeau于1900年合成的人造惰性气体,1940年前后,美国军方将其用于曼哈顿计划。1947年提供商用。当前SF6气体主要用于电力工业中。SF6气体用于4种类型的电气设备作为绝缘和/或灭弧;SF6断路器及GIS(在这里指六氟化硫封闭式组合电器,国际上称为“气体绝缘开关设备”)、SF6负荷开关设备,SF6绝缘输电管线,SF6变压器及SF6绝缘变电站。SF6气体中,80%用于高中压电力设备。六氟化硫具有良好的电气绝缘性能及优异的灭弧性能。其耐电强度为同一压力下氮气的2.5倍,击穿电压是空气的2.5倍,灭弧能力是空气的100倍,是一种优于空气和油之间的新一代超高压绝缘介质材料。六氟化硫以其良好的绝缘性能和灭弧性能,如:断路器、高压变压器、气封闭组合电容器、高压传输线、互感器等。电子级高纯六氟化硫是一种理想的电子蚀刻剂,被大量应用于微电子技术领域。冷冻工业作为制冷剂,制冷范围可在-45℃~0℃之间。电气工业利用其很高介电强度和良好的灭电弧性能,用作高压开关、大容量变压器、高压电缆和气体的绝缘材料。SF 6 gas has a history of one hundred years. It is an artificial inert gas synthesized by two French chemists, Moissan and Lebeau, in 1900. Around 1940, the US military used it for the Manhattan Project. Commercially available in 1947. Currently SF 6 gas is mainly used in the power industry. SF 6 gas is used in 4 types of electrical equipment as insulation and/or arc extinguishing; SF 6 circuit breakers and GIS (here refers to sulfur hexafluoride closed combination electrical appliances, internationally known as "gas insulated switchgear"), SF 6 load switchgear, SF 6 insulated transmission pipeline, SF 6 transformer and SF 6 insulated substation. Of the SF 6 gas, 80% is used for high and medium voltage power equipment. Sulfur hexafluoride has good electrical insulation performance and excellent arc extinguishing performance. Its electric strength is 2.5 times that of nitrogen under the same pressure, its breakdown voltage is 2.5 times that of air, and its arc extinguishing ability is 100 times that of air. It is a new generation of ultra-high voltage insulating dielectric material superior to that between air and oil. Sulfur hexafluoride is used in circuit breakers, high-voltage transformers, gas-enclosed combined capacitors, high-voltage transmission lines, transformers, etc. due to its good insulation performance and arc-extinguishing performance. Electronic-grade high-purity sulfur hexafluoride is an ideal electronic etchant, which is widely used in the field of microelectronics technology. As a refrigerant in the refrigeration industry, the refrigeration range can be between -45°C and 0°C. The electrical industry uses its high dielectric strength and good arc extinguishing performance as an insulating material for high-voltage switches, large-capacity transformers, high-voltage cables and gases.
大气压化学电离源是一种软电离技术,产生的碎片离子少,质谱图相对简单,而且具有较高的灵敏度,因此可以用作在线监测质谱仪的电离源。飞行时间质谱仪具有分析速度快、灵敏度高以及全谱扫描的优点,联合大气压化学电离源则能够实现多种混合样品的高灵敏在线检测。近年来电网安全事故频发,对国民经济和输电安全产生了较大的影响,因此对绝缘气体的监测有利于供电设备的安全运行。SF6在放电时产生的放电产物中大部分含有F原子,而F原子具有强的吸电子能力,SF6的放电产物大部分具有较高的电负性,这比较有利于用负离子模式检测。因此采用大气压负离子电离源结合飞行时间质谱仪对SF6放电分解产物中的典型分解产物SO2进行检测。通过对SO2的定性定量分析及时发现电气设备内部的故障隐患,对电网设备的正常运作具有指导意义。Atmospheric pressure chemical ionization source is a soft ionization technology that produces few fragment ions, relatively simple mass spectrum and high sensitivity, so it can be used as an ionization source for on-line monitoring mass spectrometers. Time-of-flight mass spectrometer has the advantages of fast analysis speed, high sensitivity and full-spectrum scanning, and the combination of atmospheric pressure chemical ionization source can realize high-sensitivity online detection of various mixed samples. In recent years, power grid safety accidents have occurred frequently, which has had a great impact on the national economy and power transmission safety. Therefore, the monitoring of insulating gas is conducive to the safe operation of power supply equipment. Most of the discharge products produced by SF 6 during discharge contain F atoms, and F atoms have a strong electron-withdrawing ability. Most of the discharge products of SF 6 have high electronegativity, which is more conducive to detection in negative ion mode. Therefore, an atmospheric pressure negative ion ionization source combined with a time-of-flight mass spectrometer was used to detect SO 2 , a typical decomposition product in the decomposition products of SF 6 discharge. Through the qualitative and quantitative analysis of SO 2 , timely discovery of hidden troubles inside electrical equipment has guiding significance for the normal operation of power grid equipment.
本发明专利采用注射泵将少量的气体样品通过吹扫气载带至飞行时间质谱仪电离区进行检测,大气压负离子源可以实现SO2的高效电离和分析。且该装置和方法样品消耗量低,分析速度快。The patent of the present invention uses a syringe pump to carry a small amount of gas samples to the ionization area of the time-of-flight mass spectrometer for detection, and the atmospheric pressure negative ion source can realize efficient ionization and analysis of SO 2 . Moreover, the device and method have low sample consumption and fast analysis speed.
发明内容Contents of the invention
针对现有技术的不足,本发明的目的是提供一种测定方法简单、样品消耗量低、分析速度快的绝缘气体中SO2的大气压负离子检测装置及其使用方法。Aiming at the deficiencies in the prior art, the object of the present invention is to provide a kind of measuring method simple, sample consumption is low, the analysis speed SO in the insulating gas The atmospheric pressure anion detection device and using method thereof.
为了实现上述目的,本发明采用的技术方案如下:一种绝缘气体中SO2的大气压负离子检测装置,所述绝缘气体中SO2的大气压负离子检测装置包括:注射泵、开关阀、进样瓶、保温层、飞行时间质谱仪;所述注射泵的出口直接伸入到所述进样瓶的内部;In order to achieve the above object, the technical scheme that the present invention adopts is as follows: a kind of SO in the insulating gas The atmospheric pressure negative ion detection device of SO in the insulating gas The atmospheric pressure negative ion detection device includes: syringe pump, switch valve, sampling bottle, Insulation layer, time-of-flight mass spectrometer; the outlet of the syringe pump directly extends into the inside of the sampling bottle;
所述进样瓶的左右两侧分别设置有进气口和出气口,所述进气口上设置有启闭所述进气口的所述开关阀,所述出气口的一端直接伸入到所述飞行时间质谱仪的电离区内部;The left and right sides of the sampling bottle are respectively provided with an air inlet and an air outlet, and the air inlet is provided with the switch valve for opening and closing the air inlet, and one end of the air outlet directly extends into the inside the ionization region of the time-of-flight mass spectrometer;
所述进样瓶的外壁设置有保温层,所述保温层内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温;The outer wall of the sample injection bottle is provided with a thermal insulation layer, and the thermal insulation layer is equipped with a ceramic heating layer, and a heater connecting line is arranged on the outside to connect to the power supply. to heat and keep warm;
所述飞行时间质谱仪采用的电离源为63Ni,电离方式为大气压下化学电离。The ionization source adopted by the time-of-flight mass spectrometer is 63 Ni, and the ionization method is chemical ionization under atmospheric pressure.
进一步地,所述的注射泵采用的注射器量程为1-5 ml,线速度为1ml/min,用以将绝缘气体样品匀速注入所述进样瓶中。Further, the volume of the syringe used in the syringe pump is 1-5 ml, and the linear speed is 1 ml/min, so as to inject the insulating gas sample into the sampling bottle at a uniform speed.
进一步地,所述的进气口与样品吹扫气体的出气口相连接;所述出气口的长度控制在45-55㎝。Further, the gas inlet is connected to the gas outlet of the sample purge gas; the length of the gas outlet is controlled at 45-55cm.
进一步地,所述样品吹扫气体选择N2、干净空气、He中的任意一种。Further, the sample purge gas is selected from any one of N 2 , clean air, and He.
进一步地,所述保温层内陶瓷加热层的厚度在10-20㎜。Further, the thickness of the ceramic heating layer in the thermal insulation layer is 10-20 mm.
本发明还提供了一种绝缘气体中SO2的大气压负离子检测装置的使用方法,包括以下步骤:The present invention also provides a method for using an atmospheric pressure anion detection device for SO in an insulating gas, comprising the following steps:
步骤S1,将绝缘气体样品注入注射泵,通过注射泵将绝缘气体样品匀速地注入到进样瓶中;Step S1, inject the insulating gas sample into the syringe pump, and inject the insulating gas sample into the sampling bottle at a uniform speed through the syringe pump;
步骤S2,同时开启所述开关阀打开所述进气口,样品吹扫气体通过所述进气口送入所述进样瓶;Step S2, simultaneously opening the on-off valve to open the air inlet, and the sample purge gas is sent into the sampling bottle through the air inlet;
步骤S3,开启所述进样瓶外部设置的保温层,对所述进样瓶内及出气口内的绝缘气体样品加热保温,起到干燥的作用,防止水分进入所述飞行时间质谱仪的电离源内部;Step S3, opening the insulation layer provided outside the sampling bottle, heating and insulating the insulating gas samples in the sampling bottle and the gas outlet, so as to play a role of drying and prevent moisture from entering the ionization source of the time-of-flight mass spectrometer internal;
步骤S4,样品吹扫气体通过所述出气口将绝缘气体样品载带至所述飞行时间质谱仪的电离区进行电离分析。In step S4, the sample purge gas carries the insulating gas sample to the ionization region of the time-of-flight mass spectrometer through the gas outlet for ionization analysis.
进一步地,所述步骤S2中样品吹扫气体的流速控制在35~40ml/min。Further, the flow rate of the sample purge gas in the step S2 is controlled at 35-40 ml/min.
进一步地,所述步骤S3中所述进样瓶内的温度控制在75~85℃;所述出气口内的温度控制在85~95℃。Further, in the step S3, the temperature inside the sampling bottle is controlled at 75-85°C; the temperature inside the gas outlet is controlled at 85-95°C.
进一步地,所述步骤S3中所述进样瓶与所述出气口的温差控制在8~12℃。Further, in the step S3, the temperature difference between the sampling bottle and the gas outlet is controlled at 8-12°C.
进一步地,所述步骤S4中采集质荷比为83、112的离子峰。Further, in the step S4, ion peaks with mass-to-charge ratios of 83 and 112 are collected.
本发明的有益效果是:本发明一种绝缘气体中SO2的大气压负离子检测装置及其使用方法,绝缘气体中SO2的大气压负离子检测装置包括注射泵、开关阀、进样瓶、保温层和飞行时间质谱仪,其中飞行时间质谱仪采用的电离源源为63Ni,电离方式为大气压下化学电离,通过开关阀及进气口连接的样品吹扫气体将绝缘气体样品载带至电离源内,进行高效电离和分析,进样瓶外设置有保温层,用于对绝缘气体样品加热保温,保温层内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温,从而干燥水分,水分干燥效果好,能有效防止水分进入至飞行时间质谱仪的电源内部影响检测结果,测定方法简单、样品消耗量低、分析速度快,检测灵敏度能达到ppb量级。The beneficial effect of the present invention is: a kind of SO in the insulating gas of the present invention The atmospheric pressure negative ion detection device and its use method, SO in the insulating gas The atmospheric pressure negative ion detection device comprises a syringe pump, a switch valve, a sampling bottle, an insulating layer and Time-of-flight mass spectrometer, wherein the ionization source used by the time-of-flight mass spectrometer is 63 Ni, and the ionization method is chemical ionization under atmospheric pressure. The insulating gas sample is carried into the ionization source through the switch valve and the sample purge gas connected to the gas inlet, and the High-efficiency ionization and analysis. There is an insulation layer outside the sampling bottle, which is used to heat and keep the insulating gas sample. The insulation layer is equipped with a ceramic heating layer, and the external heater is connected to the power supply. After the power is turned on, the surface of the ceramic heating layer is heated. Through Thermal radiation realizes rapid heating and cooling, which is used for heating and heat preservation, thereby drying moisture. The moisture drying effect is good, which can effectively prevent moisture from entering the power supply of the time-of-flight mass spectrometer and affect the detection results. The measurement method is simple, the sample consumption is low, and the analysis speed Fast, the detection sensitivity can reach the ppb level.
本发明一种绝缘气体中SO2的大气压负离子检测装置及其使用方法,控制出气口的长度,同时控制进样瓶以及出气口的温度,相当于在进样瓶对绝缘气体样品进行一次干燥,再在出气口对绝缘气体样品进行二次干燥,绝缘气体样品的干燥效果更好,进一步防止水分进入至飞行时间质谱仪的电源内部,检测精度更高;控制所述进样瓶与所述出气口的温差,绝缘气体样品的干燥效果更好,进一步防止水分进入至飞行时间质谱仪的电源内部,检测精度更高。The present invention is an atmospheric-pressure negative ion detection device for SO2 in insulating gas and its use method. The length of the gas outlet is controlled, and the temperature of the sampling bottle and the gas outlet is controlled at the same time, which is equivalent to drying the insulating gas sample once in the sampling bottle, and then Perform secondary drying on the insulating gas sample at the gas outlet, the drying effect of the insulating gas sample is better, further prevent moisture from entering the power supply of the time-of-flight mass spectrometer, and the detection accuracy is higher; control the sampling bottle and the gas outlet The temperature difference is better, the drying effect of the insulating gas sample is better, and the moisture is further prevented from entering the power supply of the time-of-flight mass spectrometer, and the detection accuracy is higher.
附图说明Description of drawings
图1是本发明装置的结构示意图;Fig. 1 is the structural representation of device of the present invention;
图中:1、注射泵;2、开关阀;3、进样瓶;4、保温层;5、飞行时间质谱仪; 31、进气口;32、出气口。In the figure: 1. Syringe pump; 2. On-off valve; 3. Injection bottle; 4. Insulation layer; 5. Time-of-flight mass spectrometer; 31. Air inlet; 32. Air outlet.
图2是本发明实施例1中的检测结果图。Fig. 2 is a graph of detection results in Example 1 of the present invention.
具体实施方式Detailed ways
下面的实施例可以帮助本领域的技术人员更全面地理解本发明,但不可以以任何方式限制本发明。The following examples can help those skilled in the art to understand the present invention more comprehensively, but the present invention cannot be limited in any way.
本发明一种绝缘气体中SO2的大气压负离子检测装置及其使用方法,所述样品吹扫气体选择N2、干净空气、He中的任意一种;下述实施例中选用的样品吹扫气体为N2。The present invention is a kind of SO2 in insulating gas Atmospheric pressure anion detection device and using method thereof, described sample purge gas selects any one in N 2 , clean air, He; The sample purge gas selected in the following examples is N 2 .
本发明装置的具体实施方式一:The specific embodiment one of device of the present invention:
一种绝缘气体中SO2的大气压负离子检测装置,所述绝缘气体中SO2的大气压负离子检测装置包括:注射泵1、开关阀2、进样瓶3、保温层4、飞行时间质谱仪5;所述注射泵1的出口直接伸入到所述进样瓶3的内部;所述的注射泵1采用的注射器量程为1-5 ml,线速度为1ml/min,用以将绝缘气体样品匀速注入所述进样瓶3中;An atmospheric pressure anion detection device for SO2 in an insulating gas, the atmospheric pressure negative ion detection device for SO2 in an insulating gas comprises: a
所述进样瓶3的左右两侧分别设置有进气口31和出气口32,所述进气口31上设置有启闭所述进气口31的所述开关阀2,所述出气口32的一端直接伸入到所述飞行时间质谱仪5的电离区内部;所述的进气口31与样品吹扫气体的出气口相连接;所述出气口32的长度控制在50㎝;The left and right sides of the
所述进样瓶3的外壁设置有保温层4,所述保温层4内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温;所述保温层4内陶瓷加热层的厚度在15㎜;The outer wall of the
所述飞行时间质谱仪5采用的电离源为63Ni,电离方式为大气压下化学电离。The ionization source adopted by the time-of-
本发明装置的具体实施方式二:The specific embodiment two of device of the present invention:
一种绝缘气体中SO2的大气压负离子检测装置,所述绝缘气体中SO2的大气压负离子检测装置包括:注射泵1、开关阀2、进样瓶3、保温层4、飞行时间质谱仪5;所述注射泵1的出口直接伸入到所述进样瓶3的内部;所述的注射泵1采用的注射器量程为1-5 ml,线速度为1ml/min,用以将绝缘气体样品匀速注入所述进样瓶3中;An atmospheric pressure anion detection device for SO2 in an insulating gas, the atmospheric pressure negative ion detection device for SO2 in an insulating gas comprises: a
所述进样瓶3的左右两侧分别设置有进气口31和出气口32,所述进气口31上设置有启闭所述进气口31的所述开关阀2,所述出气口32的一端直接伸入到所述飞行时间质谱仪5的电离区内部;所述的进气口31与样品吹扫气体的出气口相连接;所述出气口32的长度控制在25㎝;The left and right sides of the
所述进样瓶3的外壁设置有保温层4,所述保温层4内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温;所述保温层4内陶瓷加热层的厚度在15㎜;The outer wall of the
所述飞行时间质谱仪5采用的电离源为63Ni,电离方式为大气压下化学电离。The ionization source adopted by the time-of-
本发明装置的具体实施方式三:The specific embodiment three of the device of the present invention:
一种绝缘气体中SO2的大气压负离子检测装置,所述绝缘气体中SO2的大气压负离子检测装置包括:注射泵1、开关阀2、进样瓶3、保温层4、飞行时间质谱仪5;所述注射泵1的出口直接伸入到所述进样瓶3的内部;所述的注射泵1采用的注射器量程为1-5 ml,线速度为1ml/min,用以将绝缘气体样品匀速注入所述进样瓶3中;An atmospheric pressure anion detection device for SO2 in an insulating gas, the atmospheric pressure negative ion detection device for SO2 in an insulating gas comprises: a
所述进样瓶3的左右两侧分别设置有进气口31和出气口32,所述进气口31上设置有启闭所述进气口31的所述开关阀2,所述出气口32的一端直接伸入到所述飞行时间质谱仪5的电离区内部;所述的进气口31与样品吹扫气体的出气口相连接;所述出气口32的长度控制在75㎝;The left and right sides of the
所述进样瓶3的外壁设置有保温层4,所述保温层4内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温;所述保温层4内陶瓷加热层的厚度在15㎜;The outer wall of the
所述飞行时间质谱仪5采用的电离源为63Ni,电离方式为大气压下化学电离。The ionization source adopted by the time-of-
本发明装置的具体实施方式一~具体实施方式三的区别仅在于出气口32的长度,采用对具体实施方式一~具体实施方式三中的装置进行SF6绝缘气体干燥实验,实验过程中,进样瓶1内的温度控制在75~85℃;所述出气口32内的温度控制在95~105℃,SF6绝缘气体干燥实验表明,出气口的长度控制在45-55㎝,SF6绝缘气体干燥效果最好,能有效防止水分进入至飞行时间质谱仪的电源内部,检测精度更高。The difference between
实施例1:利用具体实施方式一中的发明装置进行SF6绝缘气体中SO2的检测实验Embodiment 1 : Utilize the inventive device in the specific embodiment one to carry out SF 6 in insulating gas SO detection experiment
一种绝缘气体中SO2的大气压负离子检测装置的使用方法,包括以下步骤: A method for using an atmospheric pressure negative ion detection device for SO in an insulating gas, comprising the following steps:
步骤S1,将绝缘气体样品注入注射泵1,通过注射泵1将绝缘气体样品匀速地注入到进样瓶3中;注射泵1采用的注射器量程为1-5ml,线速度为1ml/min;Step S1, inject the insulating gas sample into the
步骤S2,同时开启所述开关阀2打开所述进气口31,样品吹扫气体通过所述进气口31送入所述进样瓶3;样品吹扫气体的流速控制在35ml/min;Step S2, open the on-off valve 2 at the same time to open the
步骤S3,开启所述进样瓶3外部设置的保温层4,对所述进样瓶3内及出气口32内的绝缘气体样品加热保温,起到干燥的作用,防止水分进入所述飞行时间质谱仪5的电离源内部;所述进样瓶3内的温度控制在75℃;所述出气口32内的温度控制在85℃;所述步骤S3中所述进样瓶3与所述出气口32的温差控制在10℃;Step S3, opening the
步骤S4,样品吹扫气体通过所述出气口32将绝缘气体样品载带至所述飞行时间质谱仪5的电离区进行电离分析,SO2会形成质荷比83和112的两个离子峰,且信号强度高,因此采集质荷比为83、112的离子峰;利用大气压负离子检测SF6绝缘气体中的SO2,浓度为100ppm,检测结果如图2所示,能够明显看到负离子检测模式下,SO2会形成质荷比83和112的两个离子峰,且信号强度高,按照S/N=3:1计算,其灵敏度能达到ppb量级。Step S4, the sample purge gas passes through the
实施例2:利用具体实施方式一中的发明装置进行SF6绝缘气体中SO2的检测实验Embodiment 2 : Utilize the inventive device in the specific embodiment one to carry out SF 6 in insulating gas SO detection experiment
一种绝缘气体中SO2的大气压负离子检测装置的使用方法,包括以下步骤: A method for using an atmospheric pressure negative ion detection device for SO in an insulating gas, comprising the following steps:
步骤S1,将绝缘气体样品注入注射泵1,通过注射泵1将绝缘气体样品匀速地注入到进样瓶3中;注射泵1采用的注射器量程为1-5ml,线速度为1ml/min;Step S1, inject the insulating gas sample into the
步骤S2,同时开启所述开关阀2打开所述进气口31,样品吹扫气体通过所述进气口31送入所述进样瓶3;样品吹扫气体的流速控制在40ml/min;Step S2, open the on-off valve 2 at the same time to open the
步骤S3,开启所述进样瓶3外部设置的保温层4,对所述进样瓶3内及出气口32内的绝缘气体样品加热保温,起到干燥的作用,防止水分进入所述飞行时间质谱仪5的电离源内部;所述进样瓶3内的温度控制在85℃;所述出气口32内的温度控制在95℃;所述步骤S3中所述进样瓶3与所述出气口32的温差控制在10℃;Step S3, opening the
步骤S4,样品吹扫气体通过所述出气口32将绝缘气体样品载带至所述飞行时间质谱仪5的电离区进行电离分析,SO2会形成质荷比83和112的两个离子峰,且信号强度高,因此采集质荷比为83、112的离子峰;利用大气压负离子检测SF6绝缘气体中的SO2,按照S/N=3:1计算,其灵敏度能达到ppb量级。Step S4, the sample purge gas passes through the
实施例3:利用具体实施方式一中的发明装置进行SF6绝缘气体中SO2的检测实验Embodiment 3 : Utilize the inventive device in the specific embodiment one to carry out SF 6 in insulating gas SO detection experiment
一种绝缘气体中SO2的大气压负离子检测装置的使用方法,包括以下步骤: A method for using an atmospheric pressure negative ion detection device for SO in an insulating gas, comprising the following steps:
步骤S1,将绝缘气体样品注入注射泵1,通过注射泵1将绝缘气体样品匀速地注入到进样瓶3中;注射泵1采用的注射器量程为1-5ml,线速度为1ml/min;Step S1, inject the insulating gas sample into the
步骤S2,同时开启所述开关阀2打开所述进气口31,样品吹扫气体通过所述进气口31送入所述进样瓶3;样品吹扫气体的流速控制在37ml/min;Step S2, open the on-off valve 2 at the same time to open the
步骤S3,开启所述进样瓶3外部设置的保温层4,对所述进样瓶3内及出气口32内的绝缘气体样品加热保温,起到干燥的作用,防止水分进入所述飞行时间质谱仪5的电离源内部;所述进样瓶3内的温度控制在78℃;所述出气口32内的温度控制在90℃;所述步骤S3中所述进样瓶3与所述出气口32的温差控制在12℃;Step S3, opening the
步骤S4,样品吹扫气体通过所述出气口32将绝缘气体样品载带至所述飞行时间质谱仪5的电离区进行电离分析,SO2会形成质荷比83和112的两个离子峰,且信号强度高,因此采集质荷比为83、112的离子峰;利用大气压负离子检测SF6绝缘气体中的SO2,按照S/N=3:1计算,其灵敏度能达到ppb量级。Step S4, the sample purge gas passes through the
本发明一种绝缘气体中SO2的大气压负离子检测装置及其使用方法,绝缘气体中SO2的大气压负离子检测装置包括注射泵1、开关阀2、进样瓶3、保温层4、飞行时间质谱仪5,其中飞行时间质谱仪5采用的电离源源为63Ni,电离方式为大气压下化学电离,通过开关阀2及进气口31连接的样品吹扫气体将绝缘气体样品载带至电离源内,进行高效电离和分析,进样瓶3外设置有保温层4,用于对绝缘气体样品加热保温,保温层4内布陶瓷加热层、外部设置加热器连接线连接电源,通电后陶瓷加热层板面发热,通过热辐射实现快速升温和降温,用以加热保温,从而干燥水分,水分干燥效果好,能有效防止水分进入至飞行时间质谱仪5的电源内部影响检测结果,测定方法简单、样品消耗量低、分析速度快,检测灵敏度能达到ppb量级;控制出气口32的长度,同时控制进样瓶3以及出气口32的温度,相当于在进样瓶3对绝缘气体样品进行一次干燥,再在出气口32对绝缘气体样品进行二次干燥,绝缘气体样品的干燥效果更好,进一步防止水分进入至飞行时间质谱仪的电源内部,检测精度更高;控制所述进样瓶3与所述出气口32的温差,绝缘气体样品的干燥效果更好,进一步防止水分进入至飞行时间质谱仪的电源内部,检测精度更高。The present invention is an atmospheric pressure anion detection device for SO2 in an insulating gas and a method for using the same. The atmospheric pressure negative ion detection device for SO2 in an insulating gas comprises a
虽然,上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。Although the present invention has been described in detail with general descriptions and specific embodiments above, it is obvious to those skilled in the art that some modifications or improvements can be made on the basis of the present invention. Therefore, the modifications or improvements made on the basis of not departing from the spirit of the present invention all belong to the protection scope of the present invention.
Claims (10)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211308716.9A CN115639264A (en) | 2022-10-25 | 2022-10-25 | SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202211308716.9A CN115639264A (en) | 2022-10-25 | 2022-10-25 | SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof |
Publications (1)
Publication Number | Publication Date |
---|---|
CN115639264A true CN115639264A (en) | 2023-01-24 |
Family
ID=84947606
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202211308716.9A Pending CN115639264A (en) | 2022-10-25 | 2022-10-25 | SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115639264A (en) |
Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04274728A (en) * | 1990-10-31 | 1992-09-30 | Extrel Corp | Preconcentration method and device for trace component analysis in gas |
CN1265230A (en) * | 1997-07-22 | 2000-08-30 | 布莱克光电有限公司 | Inorganic hydrogen compounds, separation methods, and fuel applications |
CN103163007A (en) * | 2011-12-19 | 2013-06-19 | 中国科学院大连化学物理研究所 | Solid phase and liquid phase compound dynamic gas preparation device and gas preparation method |
CN105758969A (en) * | 2016-05-05 | 2016-07-13 | 煤科集团沈阳研究院有限公司 | Gas chromatograph used under mine and use method |
US20190348269A1 (en) * | 2018-05-13 | 2019-11-14 | Aviv Amirav | Mass Spectrometer with Photoionization Ion Source Method and System |
CN112798680A (en) * | 2020-12-01 | 2021-05-14 | 广西电网有限责任公司电力科学研究院 | Be applied to SF6Device and method for detecting decomposition product |
CN112951703A (en) * | 2019-12-10 | 2021-06-11 | 中国科学院大连化学物理研究所 | Heatable VUV photoionization source |
CN113964015A (en) * | 2021-10-27 | 2022-01-21 | 广西电网有限责任公司电力科学研究院 | Device for external standard quantification of time-of-flight mass spectrum |
-
2022
- 2022-10-25 CN CN202211308716.9A patent/CN115639264A/en active Pending
Patent Citations (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH04274728A (en) * | 1990-10-31 | 1992-09-30 | Extrel Corp | Preconcentration method and device for trace component analysis in gas |
CN1265230A (en) * | 1997-07-22 | 2000-08-30 | 布莱克光电有限公司 | Inorganic hydrogen compounds, separation methods, and fuel applications |
CN103163007A (en) * | 2011-12-19 | 2013-06-19 | 中国科学院大连化学物理研究所 | Solid phase and liquid phase compound dynamic gas preparation device and gas preparation method |
CN105758969A (en) * | 2016-05-05 | 2016-07-13 | 煤科集团沈阳研究院有限公司 | Gas chromatograph used under mine and use method |
US20190348269A1 (en) * | 2018-05-13 | 2019-11-14 | Aviv Amirav | Mass Spectrometer with Photoionization Ion Source Method and System |
CN112951703A (en) * | 2019-12-10 | 2021-06-11 | 中国科学院大连化学物理研究所 | Heatable VUV photoionization source |
CN112798680A (en) * | 2020-12-01 | 2021-05-14 | 广西电网有限责任公司电力科学研究院 | Be applied to SF6Device and method for detecting decomposition product |
CN113964015A (en) * | 2021-10-27 | 2022-01-21 | 广西电网有限责任公司电力科学研究院 | Device for external standard quantification of time-of-flight mass spectrum |
Non-Patent Citations (1)
Title |
---|
唐彬: "脉冲进样便携式TOF MS现场检测SF6电气设备中的分解产物", 《质谱学报》, no. 4, 31 July 2018 (2018-07-31) * |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110763968B (en) | Full-angle visual gas breakdown testing system | |
CN105699366A (en) | A kind of SF6 mixed gas plasma spectrum measuring device and method | |
CN105387342B (en) | The micro-water treatment system of GIS air chamber | |
CN109444346A (en) | Gas on-line monitoring system and monitoring method | |
CN103545165A (en) | A mass spectrometry ionization method and ion source device based on cold plasma jet | |
CN109442225A (en) | The insulating gas on-line monitoring system and method for preventing signal piping leakage | |
CN115639264A (en) | SO in insulating gas 2 Atmospheric negative ion detection device and using method thereof | |
KR20150117363A (en) | Circuit breaker of gas insulation switchgear | |
Boggs | Sulphur hexafluoride: introduction to the material and dielectric | |
CN203150462U (en) | Sulfur hexafluoride high-voltage electrical equipment for cold regions | |
CN209311430U (en) | Gas on-line monitoring system | |
CN208314123U (en) | It is a kind of it is extremely cold under the conditions of high-tension insulator edge flashing experimental provision | |
CN204424207U (en) | A kind of plasma electrospray mass spectrometry ionization source | |
CN108896705B (en) | SF (sulfur hexafluoride)6Gas on-line monitoring method and monitoring system thereof | |
Yang et al. | Characterization of pre-flashover behavior based on leakage current along suspension insulator strings covered with ice | |
Rao et al. | Study on the influence rules of trace H2O on SF6 spark discharge decomposition characteristic components | |
Zheng et al. | Temperature effect on the insulation performance of SF 6/N 2 gas mixture at a constant volume | |
Meier et al. | Investigations of nozzle materials in SF6 circuit breakers | |
CN114822916B (en) | Insulation protection device, data center protection method and data center | |
CN209727564U (en) | A kind of SF with gas collector6Chromatographic detection system | |
CN111595991B (en) | A kind of sulfur hexafluoride electrolysis intermediate product extraction device | |
Juhre et al. | Investigations on the long-term performance of Fluoronitrile-containing gas mixtures in gas-insulated systems | |
CN107326331A (en) | A kind of process for improving epoxy resins insulation Work tool surface dielectric performance | |
CN208013353U (en) | A kind of micro water syringe for SF6 electric discharge decomposition experiments | |
JP2003297200A (en) | Gas-blast circuit breaker |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination |