CN102128894B - 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 PDFInfo
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- CN102128894B CN102128894B CN 201010611860 CN201010611860A CN102128894B CN 102128894 B CN102128894 B CN 102128894B CN 201010611860 CN201010611860 CN 201010611860 CN 201010611860 A CN201010611860 A CN 201010611860A CN 102128894 B CN102128894 B CN 102128894B
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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
Technical field
The present invention relates to a kind of gas chromatographic detection equipment and detection technique class, espespecially a kind of gas-chromatography detection method and analysis chromatograph for gas for the analysis of voltage levels oil-filled electric equipment Dissolved Gases in Insulating Oil.
Background technology
At present, domestic electric system detects oil-filled electric equipment and when safeguarding, need to analyze Dissolved Gases in Insulating Oil, and most widely used is the stratographic analysis of test experiment chamber, also is simultaneously the arbitration means that detection department adopts.Current Domestic oil filled electric power equipment special-purpose gas chromatograph 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 larger success in off-line is used, but in view of the development trend of electric system be on-line monitoring, repair based on condition of component, Intelligent transformer station etc., it is must tending to of power system development that development is suitable for the online chromatographic technique of using.Yet, if with above-mentioned hand sampling, twin columns and connect, once shunting, the analytical technology that three detecting devices detect is simultaneously carried out in linearize, has problems, such 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, therefore 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 substation field.And thermal conductivity detector (TCD) is only to H
2Component has preferably sensitivity, to the sensitivity extreme difference of other component gas (CO, CO2, hydro carbons), does not satisfy online requirement of using.In addition, because said system three detector technologies of sampling, greatly increase complexity and the hardware cost of system, be unfavorable for the large-scale promotion in online the application.
In sum, how to propose a kind of repeatability, accuracy and sensitivity on the basis of simplied system structure, reduction hardware cost 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
For the problem that prior art exists, the object of the present invention is to provide the gas-chromatography detection method of finishing the Dissolved Gases in Insulating Oil 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 can be safe and reliable operate in substation field, to improve the efficient of dielectric oil chromatographic analysis, improve the online Dissolved Gases in Insulating Oil analytical chromatograph of analysis result accuracy.
Online analysis chromatograph for gas in insulating oil 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 is filled with quantitative gases dissolved in insulation 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 in order sample gas testing agency, detected successively the content of seven kinds of gases by this sample gas testing agency.
Further, described sample introduction mechanism input end and sample gas separating mechanism output terminal also are connected with carrier gas channel, and the carrier gas that passes into by carrier gas channel is sent into quantitative gases dissolved in insulation 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 quantity tube, ten-way valve and gas circuit switching cylinder, and quantity tube is connected to ten-way valve two interfaces, inputs quantitative sample gas by ten-way valve in quantity tube; Gas circuit is switched cylinder makes it be in Inlet Position or detection position for driving the ten-way valve rotation.
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 passing into sample gas in the zirconium pipe; Resistance wire is wrapped on the quartz ampoule zirconium pipe heating that is used for wherein, and thermopair is oppositely arranged with zirconium pipe bottom, for detection of the temperature of zirconium pipe, and controls 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) quantitative gases dissolved in insulation oil is once passed into 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 successively H
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 is filled with gases dissolved in insulation oil at Inlet Position in the quantity tube of sample introduction mechanism, pass into 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 the first chromatographic column with H
2, O
2, CO, CH
4Gas group and C
2H
4, C
2H
6And C
2H
2Separate, through the second chromatographic column with H
2, each gas in O2, CO, the CH4 gas group separates, gas passes into sample gas testing agency by H2, O2, CO, CH4, C2H4, C2H6, C2H2 order with carrier gas.
Further, filler is 80-100 purpose 5A molecular sieve in described the first chromatographic column, and filler is 60-80 order Propak-N in described the second chromatographic column.
Further, step 3) is specially: the heating-up temperature of control sample gas testing agency reacts seven kinds of gases that pass into successively, to measure the content of seven kinds of gases in the zirconium pipe of sample gas testing agency.
Online analysis chromatograph for gas in insulating oil 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 needing H
2The characteristic of igniting determined above-mentioned three detector technologies hardly may be in online the 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 the sensitivity that each component gas is had excellence are 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, is conducive to large-scale promotion in online the application.
Its two, adopt series connection auto injection mode.Traditional off-line Dissolved Gases in Insulating Oil analytical approach is owing to adopting 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 is different, when its when carrying out same instrument tested, may cause measurement result there are differences because " 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 greatly improved the automatization level of instrument, 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 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 chromatographic gas circuit schematic diagram of the present invention;
Fig. 5 is the process of gas path figure of ten-way valve Inlet Position;
Fig. 6 is the process of gas path figure of ten-way valve detection position.
Embodiment
As Figure 1-3, online analysis chromatograph for gas in insulating oil of the present invention, comprise casing 1, casing 1 interior sample introduction mechanism 2, sample gas separating mechanism 3 and the sample gas testing agency 4 of arranging, sample gas separating mechanism 3 comprises post case 11, post case 11 interior two root chromatogram columns 17 and the heating aluminium ingots 18 of arranging, 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, be provided with injection port 42 on the shell 41, injection port 42 is inputted gas in the zirconium pipe 44 by sample feeding 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 peripheries are provided 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 then connects a T-valve 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 on another road by connect pressure maintaining valve and flow stabilizing valve with T-valve, ten-way valve output is connected to 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 Inlet Position (shown in Figure 5), be sent to the mouth 2,3 of gases dissolved in insulation 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 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, cross tail from detecting device gas flow out and blow solenoid valve and flowmeter, then emptying.
This gas-chromatography detection method for the analysis of voltage levels oil-filled electric equipment Dissolved Gases in Insulating Oil according to above technical scheme, meet domestic power industry to the chromatogram examination criteria of oil-filled electric equipment insulating oil gas chromatograph, each component gas especially C2H2 had excellent sensitivity, when improving insulating oil chromatographic analysis systems resistance to overturning, the repeatability that detects data 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 having 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 (8)
1. online analysis chromatograph for gas in insulating oil, it is characterized in that, comprise casing, sample introduction mechanism is set in the casing, sample gas separating mechanism and sample gas testing agency, sample introduction mechanism, link to each other by gas path pipe successively between sample gas separating mechanism and the sample gas testing agency, sample introduction mechanism is filled with quantitative gases dissolved in insulation oil in sample gas separating mechanism, 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, one root chromatogram column is used for H2, O2, CO, CH4 gas group and C2H4, C2H6 and C2H2 separate, and another root chromatogram column is used for further with H2, O2, CO, each gas in the CH4 gas group is separated; Sample gas separating mechanism is separated H2, O2, CO, CH4, C2H4, C2H6 and C2H2 in the insulating oil, and enter in order sample gas testing agency, detected successively the content of seven kinds of gases by this sample gas testing agency, 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 passing into sample gas in the zirconium pipe; Resistance wire is wrapped on the quartz ampoule zirconium pipe heating that is used for wherein, and thermopair is oppositely arranged with zirconium pipe bottom, for detection of the temperature of zirconium pipe, and controls the temperature of zirconium pipe all the time in working temperature by resistance wire; Quartz ampoule also is provided with heat-preservation cotton outward.
2. online analysis chromatograph for gas in insulating oil as claimed in claim 1, it is characterized in that, described sample introduction mechanism input end and sample gas separating mechanism output terminal also are connected with carrier gas channel, and the carrier gas that passes into by carrier gas channel is sent into quantitative gases dissolved in insulation 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 analysis chromatograph for gas in insulating oil as claimed in claim 2, it is characterized in that, described sample introduction mechanism comprises quantity tube, ten-way valve and gas circuit switching cylinder, and quantity tube is connected to ten-way valve two interfaces, inputs quantitative sample gas by ten-way valve in quantity tube; Gas circuit is switched cylinder makes it be in Inlet Position or detection position for driving the ten-way valve rotation.
4. adopt the chromatographic chromatographic detection method as described in each such as claim 1-3,1) quantitative gases dissolved in insulation oil is once passed into chromatographic sample introduction mechanism; 2) by sample gas separating mechanism sample gas is sequentially separated with H2, O2, CO, CH4, C2H4, C2H6, C2H2; 3) detect successively the content of H2, O2, CO, CH4, C2H4, C2H6, C2H2.
5. chromatographic detection method as claimed in claim 4, it is characterized in that, step 1) is specially: the ten-way valve of control sample introduction mechanism is filled with gases dissolved in insulation oil at Inlet Position in the quantity tube of sample introduction mechanism, pass into carrier gas simultaneously in two root chromatogram columns of sample gas separating mechanism.
6. chromatographic detection method as claimed in claim 5, 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 by the first chromatographic column H2, O2, CO, CH4 gas group and C2H4, C2H6 and C2H2 are separated, through the second chromatographic column each gas in H2, O2, CO, the CH4 gas group is separated, gas passes into sample gas testing agency by H2, O2, CO, CH4, C2H4, C2H6, C2H2 order with carrier gas.
7. chromatographic detection method as claimed in claim 6 is characterized in that, filler is 80-100 purpose 5A molecular sieve in described the first chromatographic column, and filler is 60-80 order Propak-N in described the second chromatographic column.
8. chromatographic detection method as claimed in claim 7 is characterized in that, step 3) is specially: the heating-up temperature of control sample gas testing agency reacts seven kinds of gases that pass into successively, to measure the content of seven kinds of gases in the zirconium pipe of sample gas testing agency.
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Cited By (1)
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|---|---|---|---|---|
| CN106124676A (en) * | 2016-09-08 | 2016-11-16 | 国网上海市电力公司 | A kind of for measuring the gas chromatograph of solution gas in transformer oil |
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