CN102128894A - Online analytical chromatograph and chromatographic detection method for gases in insulating oil - Google Patents

Online analytical chromatograph and chromatographic detection method for gases in insulating oil Download PDF

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Publication number
CN102128894A
CN102128894A CN 201010611860 CN201010611860A CN102128894A CN 102128894 A CN102128894 A CN 102128894A CN 201010611860 CN201010611860 CN 201010611860 CN 201010611860 A CN201010611860 A CN 201010611860A CN 102128894 A CN102128894 A CN 102128894A
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gas
sample
sample gas
testing agency
chromatographic
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CN102128894B (en
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梁轩伟
曹建
范竞敏
安晨光
邢升
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Beijing Huadian Yuntong Power Technology Co Ltd
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Beijing Huadian Yuntong Power Technology Co Ltd
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Abstract

The invention discloses an online analytical chromatograph and a chromatographic detection method for gases in insulating oil, which adopt an instrument system and a detection method with double-column serial connection, one-step automatic sample injection, program control switch and single detector analysis. The technical scheme provided by the invention meets the chromatographic detection standard of a domestic power industry on an oil charge electric equipment insulating oil gas chromatograph, has excellent sensitivity on all component gases, especially C2H2, improves the integral stability of an insulating oil gas chromatographic analysis system and the repeatability and accuracy of detected data, simplifies a hardware structure, improves the automation level, reduces the system cost and is suitable for large-scale popularization and application in an intelligent grid project.

Description

Online insulation dissolved gas analysis chromatograph and chromatographic detection method
 
Technical field
The present invention relates to a kind of gas chromatographic detection equipment and detection technique class, refer to a kind of gas-chromatography detection method and gas analysis chromatograph that is used for the oil-filled insulation of electrical installation dissolved gas analysis of voltage levels especially.
Background technology
At present, domestic electric system detects oil-filled electrical equipment and when safeguarding, need analyze the insulation oil dissolved gas, and most widely used is the stratographic analysis of off-line laboratory, also is simultaneously the arbitration means that detection department adopts.The special-purpose gas chromatograph of domestic electric power oil-filled equipment of present stage generally adopts hand sampling, twin columns and connects once shunting, the analytical technology system that three detecting devices detect simultaneously.Three detecting devices are generally 1 thermal conductance+two hydrogen ion flame detector.
Above-mentioned analytic system has obtained bigger success in off-line is used, but in view of power system development trend be on-line monitoring, repair based on condition of component, intelligent transformer station etc., the chromatographic technique that development is suitable for online application is must tending to of power system development.Yet, if with above-mentioned hand sampling, twin columns and connect, once shunting, the analytical technology that three detecting devices detect simultaneously carries out having problems in linearize, as the sample introduction aspect, because sample introduction adopts manual operations, is difficult in linearize.And because automaticity is not high, complex operation step, the factor of introducing error is many, so operating personnel are had very high requirement.The detection technique aspect, the technology that above-mentioned analytic system adopts three detecting devices (1 thermal conductance+two hydrogen ion flame detector) to detect simultaneously, wherein the hydrogen ion detecting device needs H 2Igniting, H 2Belong to hazardous gas, can not be applied in the transformer station scene.And thermal conductivity detector (TCD) is only to H 2Component has sensitivity preferably, and the sensitivity extreme difference to other component gas (CO, CO2, hydro carbons) does not satisfy the requirement of online application.In addition, because said system three detector technologies of sampling, increase the complexity and the hardware cost of system greatly, be unfavorable for the large-scale promotion in the online application.
In sum, how on the basis of simplied system structure, reduction hardware cost, to propose a kind of repeatability, accuracy and sensitivity and meet CNS and power industry standard, satisfy online application requirements, the gas-chromatography detection method that is suitable for large-scale promotion just becomes electric power research worker's a problem.
Summary of the invention
At the problem that prior art exists, the object of the present invention is to provide the gas-chromatography detection method of finishing the insulation dissolved gas analysis of a kind of single carrier gas, auto injection, single detecting device analysis.
Another object of the present invention is to provide a kind of transformer station scene that operates in that can be safe and reliable,, improve the online insulation dissolved gas analysis chromatograph of analysis result accuracy to improve the efficient of dielectric oil chromatographic analysis.
Online insulation dissolved gas analysis chromatograph of the present invention, comprise casing, sample introduction mechanism, sample gas separating mechanism and sample gas testing agency are set in the casing, link to each other by gas path pipe successively between sample introduction mechanism, sample gas separating mechanism and the sample gas testing agency, sample introduction mechanism charges into gas in the quantitative insulating oil in sample gas separating mechanism, sample gas separating mechanism is with H in the insulating oil 2, O 2, CO, CH 4, C 2H 4, C 2H 6And C 2H 2Separate, and enter sample gas testing agency in order, detect the content of seven kinds of gases by this sample gas testing agency successively.
Further, described sample introduction mechanism's input end and sample gas separating mechanism output terminal also are connected with carrier gas channel, and the carrier gas that feeds by carrier gas channel is sent into gas in the quantitative insulating oil sample gas separating mechanism and seven kinds of gases that sample gas its disengagement goes out are sent into described sample gas testing agency.
Further, described sample introduction mechanism comprises that quantity tube, ten-way valve and gas circuit switch cylinder, and quantity tube is connected ten-way valve two interfaces, imports quantitative sample gas by ten-way valve in quantity tube; Gas circuit switching cylinder is used to drive the ten-way valve rotation makes it be in air inlet position or detection position.
Further, described sample gas separating mechanism comprises two root chromatogram columns and heating aluminium ingot, two root chromatogram column coileds, and dish is on the heating aluminium ingot, and head and the tail are connected in series between two root chromatogram columns, and a root chromatogram column is used for H 2, O 2, CO, CH 4Gas group and C 2H 4, C 2H 6And C 2H 2Separate, another root chromatogram column is used for further with H 2, O 2, CO, CH 4Each gas in the gas group is separated.
Further, described sample gas testing agency comprises zirconium pipe, thermopair, quartz ampoule and resistance wire, and zirconium pipe and thermopair are arranged in the quartz ampoule, and the injection port of sample gas testing agency links to each other with the zirconium pipe, is used for feeding in the zirconium pipe sample gas; Resistance wire is wrapped in the zirconium pipe heating that is used on the quartz ampoule wherein, and thermopair and zirconium pipe bottom are oppositely arranged, and are used to detect the temperature of zirconium pipe, and control the temperature of zirconium pipe all the time in working temperature by resistance wire; Quartz ampoule also is provided with heat-preservation cotton outward.
Above-mentioned chromatographic chromatographic detection method of the present invention, 1) gas in the quantitative insulating oil is once fed chromatographic sample introduction mechanism; 2) by sample gas separating mechanism with sample gas with H 2, O 2, CO, CH 4, C 2H 4, C 2H 6, C 2H 2Order is separated; 3) detect H successively 2, O 2, CO, CH 4, C 2H 4, C 2H 6, C 2H 2Content.
Further, step 1) is specially: the ten-way valve of control sample introduction mechanism charges into gas in the insulating oil in the air inlet position in the quantity tube of sample introduction mechanism, feed carrier gas simultaneously in two root chromatogram columns of sample gas separating mechanism.
Further, step 2) be specially: the ten-way valve of control sample introduction mechanism is in the detection position, and the sample gas in the quantity tube is sent in two root chromatogram columns with carrier gas, at first passes through first chromatographic column with H 2, O 2, CO, CH 4Gas group and C 2H 4, C 2H 6And C 2H 2Separate, through second chromatographic column with H 2, each gas in O2, CO, the CH4 gas group separates, gas is pressed H2, O2, CO, CH4, C2H4, C2H6, the C2H2 order feeds sample gas testing agency with carrier gas.
Further, filler is a 80-100 purpose 5A molecular sieve in described first chromatographic column, and filler is 60-80 order Propak-N in described second chromatographic column.
Further, step 3) is specially: the heating-up temperature of control sample gas testing agency reacts seven kinds of gases that feed successively, to measure the content of seven kinds of gases in the zirconium pipe of sample gas testing agency.
Online insulation dissolved gas analysis chromatograph of the present invention and chromatographic detection method are compared with existing equipment and detection method and are had the following advantages.
One, sampling new fuel cell detector technologies.What application was more during domestic off-line chromatograph detected is the detector combination mode of " 1TCD+2FID ", by the narration of background technology as can be known, based on the gas chromatograph of above-mentioned detector combination technical approach exist hardware configuration complexity, automaticity low, be difficult in shortcomings such as linearizes, especially fid detector is owing to need H 2The characteristic of igniting determined above-mentioned three detector technologies hardly may be in online application large-scale promotion.The present invention adopts special detecting device, and single detecting device can detect H 2, O 2, CO, CH 4, C 2H 4, C 2H 6, C 2H 2Seven component gas in the oil, and each component gas had excellent sensitivity, to key feature gas C 2H 2Sensitivity be 0.1uL/L.With respect to three traditional detecting device analytical approachs, the present invention has simplified hardware configuration greatly, has reduced hardware cost, has improved the reliability of system, helps large-scale promotion in the online application.
Its two, adopt series connection auto injection mode.Dissolved gas analyzing method in traditional off-line insulating oil is owing to adopt three detector arrangement, the gas sampling mode is generally " manually, shunting in parallel " sample introduction, above-mentioned sample injection method step is various, operating personnel there is higher requirement, and because different personnel's operation technique difference, when its when carrying out same instrument experimentized, may cause measurement result there are differences because of " split ratio " is different.The present invention adopts the ten-way valve auto injection, and input mode is the series connection sample introduction, and the sampling action of ten-way valve is controlled by the computer program of embedded system, has improved instrument automation level greatly, has guaranteed the repeatability of sample introduction.
Its three, adopt the chromatographic column switching mode to carry out gas and separate.Because have seven kinds of characteristic components to need to separate, a root chromatogram column can not satisfy separation requirement.The mode that the present invention adopts the series connection of two root chromatogram columns to switch, handoff functionality is realized by ten-way valve.
Description of drawings
Fig. 1 is a chromatographic structural representation of the present invention;
Fig. 2 is the structural representation of sample gas separating mechanism of the present invention;
Fig. 3 is the structural representation of sample gas of the present invention testing agency;
Fig. 4 is a chromatographic gas circuit synoptic diagram of the present invention;
Fig. 5 is the process of gas path figure of ten-way valve air inlet position;
Fig. 6 is the process of gas path figure of ten-way valve detection position.
Embodiment
As Figure 1-3, online insulation dissolved gas analysis chromatograph of the present invention, comprise casing 1, sample introduction mechanism 2, sample gas separating mechanism 3 and sample gas testing agency 4 are set in the casing 1, and sample gas separating mechanism 3 comprises post case 11, and two root chromatogram columns 17 and heating aluminium ingot 18 are set in the post case 11, two root chromatogram columns, 17 head and the tail coiled connected in series, dish is provided with heat-preservation cotton 16 in the post case 11 on heating aluminium ingot 18, chromatographic column 17 keeps certain temperature by heating aluminium ingot 18 under the effect of heat-preservation cotton 16; Sample gas testing agency 4 comprises shell 41, shell 41 is provided with injection port 42, injection port 42 is imported gas in the zirconium pipe 44 by sample introduction pipe 43, zirconium pipe 44 is relatively set with thermopair 46, zirconium pipe 44 and thermopair 46 all are contained in the quartz ampoule 45, be provided with heat-preservation cotton 47 around the quartz ampoule 45, heat-preservation cotton 47 outer periphery are equipped with heating plate 48, heating plate 48 also can substitute with resistance wire, only need resistance wire is wrapped on the quartz ampoule 45, guarantee the temperature of zirconium pipe 44 environment of living in, thermopair 46 detects the temperature of zirconium pipe 44 always, and then 48 intensifications of control heating plate or cooling, guarantee that zirconium pipe 44 is in working temperature all the time.
As shown in Figure 4, sample introduction mechanism 2 comprises ten-way valve and gas circuit switching cylinder, the carrier gas channel input end is provided with the carrier gas solenoid valve and connects a T-valve then carrier gas is divided into two-way, one the tunnel connects solenoid valve for sampling, gas circuit is switched cylinder and ten-way valve, the T-valve of the output terminal of ten-way valve and sample gas separating mechanism 3 is sent into by connect pressure maintaining valve and flow stabilizing valve with T-valve in another road, ten-way valve output is connected the input end of sample gas separating mechanism 3, the output termination T-valve of sample gas separating mechanism 3, last interface of this T-valve links to each other with the injection port 42 of sample gas testing agency 4, and the output of sample gas testing agency 4 connects tail and blows solenoid valve and flowmeter.
As illustrated in Figures 5 and 6, be connected with quantity tube on the ten-way valve, before carrying out the detection of sample gas, at first control ten-way valve in air inlet position (shown in Figure 5), be sent to the mouth 2,3 of gas in the insulating oil by ten-way valve in the quantity tube this moment, and carrier gas is sent into through chromatographic column A and chromatographic column B from the mouth 10 of ten-way valve; Wherein carrier gas is 99.999% high-purity N 2, chromatographic column A filler is 60-80 order Propak-N, 4 meters of length, and chromatographic column B filler is a 80-100 purpose 5A molecular sieve, length is 2 meters.After finishing gas sampling, the control ten-way valve switches to detection position (shown in Figure 6), at this moment, by carrier gas the sample gas in the quantity tube is transported to chromatographic column B, through chromatographic column B sample gas is isolated H2, O2, CO, CH4 gas group and C2H4, C2H6 and C2H2, above-mentioned gas passes through chromatographic column A again with H2, O2, CO, each gas in the CH4 gas group is separated, the final H2 that presses, O2, CO, CH4, C2H4, C2H6, the order of C2H2 is sent in the sample gas testing agency 4 successively, finally detect the content of seven kinds of gases, the gas stream that comes out from detecting device is crossed tail and is blown solenoid valve and flowmeter, emptying then.
This gas-chromatography detection method that is used for the oil-filled insulation of electrical installation dissolved gas analysis of voltage levels according to above technical scheme, meet the chromatogram examination criteria of domestic power industry to oil-filled insulation of electrical installation oil gas chromatography, each component gas especially C2H2 had excellent sensitivity, when improving insulating oil chromatographic analysis systems resistance to overturning, detecting data repeatability and accuracy, simplified hardware configuration, improved automatization level, reduce system cost, be suitable for large-scale promotion and application in the intelligent grid project.This detection method not only provides strong technical support for the detection technique of power industry, and also improving overall economic efficiency owing to have good cost performance for enterprise simultaneously provides technical guarantee.
It is to be noted and any distortion of making according to the specific embodiment of the present invention all do not break away from the scope that spirit of the present invention and claim are put down in writing.

Claims (10)

1. online insulation dissolved gas analysis chromatograph, it is characterized in that, comprise casing, sample introduction mechanism, sample gas separating mechanism and sample gas testing agency are set in the casing, link to each other by gas path pipe successively between sample introduction mechanism, sample gas separating mechanism and the sample gas testing agency, sample introduction mechanism charges into gas in the quantitative insulating oil in sample gas separating mechanism, sample gas separating mechanism is separated H2, O2, CO, CH4, C2H4, C2H6 and C2H2 in the insulating oil, and enter sample gas testing agency in order, detect the content of seven kinds of gases successively by this sample gas testing agency.
2. online insulation dissolved gas analysis chromatograph as claimed in claim 1, it is characterized in that, described sample introduction mechanism's input end and sample gas separating mechanism output terminal also are connected with carrier gas channel, and the carrier gas that feeds by carrier gas channel is sent into gas in the quantitative insulating oil sample gas separating mechanism and seven kinds of gases that sample gas its disengagement goes out are sent into described sample gas testing agency.
3. online insulation dissolved gas analysis chromatograph as claimed in claim 2, it is characterized in that, described sample introduction mechanism comprises that quantity tube, ten-way valve and gas circuit switch cylinder, and quantity tube is connected ten-way valve two interfaces, imports quantitative sample gas by ten-way valve in quantity tube; Gas circuit switching cylinder is used to drive the ten-way valve rotation makes it be in air inlet position or detection position.
4. online insulation dissolved gas analysis chromatograph as claimed in claim 3, it is characterized in that, described sample gas separating mechanism comprises two root chromatogram columns and heating aluminium ingot, two root chromatogram column coileds, dish is on the heating aluminium ingot, head and the tail are connected in series between two root chromatogram columns, and a root chromatogram column is used for H2, O2, CO, CH4 gas group and C2H4, C2H6 and C2H2 are separated, and another root chromatogram column is used for further each gas of H2, O2, CO, CH4 gas group being separated.
5. online insulation dissolved gas analysis chromatograph as claimed in claim 4, it is characterized in that, described sample gas testing agency comprises zirconium pipe, thermopair, quartz ampoule and resistance wire, zirconium pipe and thermopair are arranged in the quartz ampoule, the injection port of sample gas testing agency links to each other with the zirconium pipe, is used for feeding in the zirconium pipe sample gas; Resistance wire is wrapped in the zirconium pipe heating that is used on the quartz ampoule wherein, and thermopair and zirconium pipe bottom are oppositely arranged, and are used to detect the temperature of zirconium pipe, and control the temperature of zirconium pipe all the time in working temperature by resistance wire; Quartz ampoule also is provided with heat-preservation cotton outward.
6. as claim 1-5 chromatographic chromatographic detection method as described in each, 1) gas in the quantitative insulating oil is once fed chromatographic sample introduction mechanism; 2) by sample gas separating mechanism sample gas is separated in proper order with H2, O2, CO, CH4, C2H4, C2H6, C2H2; 3) detect the content of H2, O2, CO, CH4, C2H4, C2H6, C2H2 successively.
7. chromatographic detection method as claimed in claim 6, it is characterized in that, step 1) is specially: the ten-way valve of control sample introduction mechanism charges into gas in the insulating oil in the air inlet position in the quantity tube of sample introduction mechanism, feed carrier gas simultaneously in two root chromatogram columns of sample gas separating mechanism.
8. chromatographic detection method as claimed in claim 7, it is characterized in that, step 2) be specially: the ten-way valve of control sample introduction mechanism is in the detection position, sample gas in the quantity tube is sent in two root chromatogram columns with carrier gas, at first H2, O2, CO, CH4 gas group and C2H4, C2H6 and C2H2 are separated by first chromatographic column, through second chromatographic column each gas in H2, O2, CO, the CH4 gas group is separated, gas is pressed H2, O2, CO, CH4, C2H4, C2H6, C2H2 order with carrier gas feeding sample gas testing agency.
9. chromatographic detection method as claimed in claim 8 is characterized in that, filler is a 80-100 purpose 5A molecular sieve in described first chromatographic column, and filler is 60-80 order Propak-N in described second chromatographic column.
10. chromatographic detection method as claimed in claim 9 is characterized in that step 3) is specially: the heating-up temperature of control sample gas testing agency reacts seven kinds of gases that feed successively, to measure the content of seven kinds of gases in the zirconium pipe of sample gas testing agency.
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CN103105472A (en) * 2012-04-06 2013-05-15 刘忠 Method and system for detecting dissolved hydrogen in water
CN103472162A (en) * 2013-09-11 2013-12-25 农业部沼气科学研究所 Method for simultaneously detecting methane and hydrogen in biogas
CN104076102A (en) * 2014-07-01 2014-10-01 长沙业嘉电子科技有限公司 Analyzer for gas dissolved in mobile type insulating oil and detection method of gas dissolved in mobile type insulating oil
CN104359988A (en) * 2014-11-06 2015-02-18 长沙业嘉电子科技有限公司 Novel gas chromatography detecting method for analyzing gas dissolved into mineral oil
CN104374860A (en) * 2014-11-28 2015-02-25 长沙业嘉电子科技有限公司 Portable analyzer for analyzing trace dissolved gas in mineral oil and detecting method
CN105758958A (en) * 2016-03-01 2016-07-13 湖南大学 Quick detector for hydrogen and methane components in respiratory air
CN106290664A (en) * 2016-08-26 2017-01-04 台州市创导科学仪器有限公司 A kind of gases dissolved in insulation oil separation detecting device
CN106404968A (en) * 2016-08-31 2017-02-15 许继集团有限公司 Gas circuit connecting piece
CN110672748A (en) * 2019-10-24 2020-01-10 福建工程学院 Method and system for identifying oil chromatographic peak
CN113984938A (en) * 2021-12-29 2022-01-28 佛山速敏智能仪器科技有限公司 Remove portable gas analysis chromatograph
CN114200072A (en) * 2022-02-21 2022-03-18 佛山速敏智能仪器科技有限公司 Method and device for calibrating online monitoring system for dissolved gas in transformer oil
CN114509472A (en) * 2022-04-19 2022-05-17 佛山速敏智能仪器科技有限公司 Gas detection system, detection method and gas detection device in transformer oil

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CN103105472A (en) * 2012-04-06 2013-05-15 刘忠 Method and system for detecting dissolved hydrogen in water
CN103105472B (en) * 2012-04-06 2015-05-27 刘忠 Method and system for detecting dissolved hydrogen in water
CN103472162A (en) * 2013-09-11 2013-12-25 农业部沼气科学研究所 Method for simultaneously detecting methane and hydrogen in biogas
CN104076102B (en) * 2014-07-01 2016-08-17 长沙业嘉电子科技有限公司 Mobile insulation dissolved gas analysis instrument and detection method thereof
CN104076102A (en) * 2014-07-01 2014-10-01 长沙业嘉电子科技有限公司 Analyzer for gas dissolved in mobile type insulating oil and detection method of gas dissolved in mobile type insulating oil
CN104359988A (en) * 2014-11-06 2015-02-18 长沙业嘉电子科技有限公司 Novel gas chromatography detecting method for analyzing gas dissolved into mineral oil
CN104359988B (en) * 2014-11-06 2016-05-25 长沙业嘉电子科技有限公司 A kind of gas-chromatography detection method of new mineral dissolved gas analysis
CN104374860A (en) * 2014-11-28 2015-02-25 长沙业嘉电子科技有限公司 Portable analyzer for analyzing trace dissolved gas in mineral oil and detecting method
CN105758958A (en) * 2016-03-01 2016-07-13 湖南大学 Quick detector for hydrogen and methane components in respiratory air
CN106290664A (en) * 2016-08-26 2017-01-04 台州市创导科学仪器有限公司 A kind of gases dissolved in insulation oil separation detecting device
CN106290664B (en) * 2016-08-26 2019-07-02 台州市创导科学仪器有限公司 A kind of gases dissolved in insulation oil separation detecting device
CN106404968A (en) * 2016-08-31 2017-02-15 许继集团有限公司 Gas circuit connecting piece
CN110672748A (en) * 2019-10-24 2020-01-10 福建工程学院 Method and system for identifying oil chromatographic peak
CN113984938A (en) * 2021-12-29 2022-01-28 佛山速敏智能仪器科技有限公司 Remove portable gas analysis chromatograph
CN114200072A (en) * 2022-02-21 2022-03-18 佛山速敏智能仪器科技有限公司 Method and device for calibrating online monitoring system for dissolved gas in transformer oil
CN114509472A (en) * 2022-04-19 2022-05-17 佛山速敏智能仪器科技有限公司 Gas detection system, detection method and gas detection device in transformer oil

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