CN103018378A - Gas chromatograph with oil-gas separation function and gas chromatography process for determination of trace moisture in insulating oil - Google Patents
Gas chromatograph with oil-gas separation function and gas chromatography process for determination of trace moisture in insulating oil Download PDFInfo
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Abstract
The invention relates to a gas chromatograph with an oil-gas separation function and a gas chromatography process for the determination of trace moisture in insulating oil. According to the chromatograph, a determination gas passage and a backblowing gas passage are formed in a manner that a three-way valve, pressure stabilizing valves, an electromagnetic valve, a six-way valve, a sample feeder, chromatographic columns, connecting pipelines, joints and the like are connected according to a certain sequence and the passage switchover of the six-way valve and the on/off of the electromagnetic valve are carried out. The gas chromatograph and the gas chromatography process have the positive and beneficial effects that the situation that a moisture peak form is not affected during analysis can be guaranteed, and a fed oil sample and oil vapor can be back-blown out of a chromatographic system in time, so that the pollution to an analytical column and a detector pool body caused by residual oil is avoided; due to a designed sample inlet structure, the situation that oil samples difficult to be gasified are stopped at a sample inlet during sample inletting can be effectively guaranteed; during backblowing, the residual oil can be smoothly discharged from the chromatographic system conveniently; gas passage structures are simple, the manufacture is easier compared with that of a high-temperature direct oil-gas separation sample feeder, and the effect of oil-gas separation function realizing is obvious; and the overall sealing performance of a system is good.
Description
Technical field
The present invention relates to a kind of gas chromatographic analysis technique field, be specifically related to a kind of based on the blowback principle, with the gas chromatograph of gas-oil separation function and measure the process of gas chromatography of micro-moisture in the insulating oil.
Background technology
Power industry generally adopts insulating oil to guarantee the insulation between associated components in transformer and the sleeve pipe.And along with the operation of these equipment, can sneak into some micro-moistures in the oil, and then greatly reduce the insulating property of insulating oil, shortened the normal service life of transformer and sleeve pipe, also may cause the generation of some accidents, cause huge loss and harm.Therefore, the little water monitoring in the insulating oil becomes an important indicator of oil monitoring, in GB/T 7595-2008(transformer oil quality in service) etc. water content in oil is had clear and definite regulation in the standard, and GB/T 7601 also is the method for wherein recommending.GB/T 7601-2008(transformer oil in service, steam turbine oil determination of moisture vapor-phase chromatography) in recommend injector with the gas-oil separation function as vaporizer.Under normal circumstances, to the requirement of this injector be: 1. can withstand long term exposure 200 ℃ high temperature; 2. used material can allow hydrone freely see through, and oil sample can be by effectively catching in injector; 3. behind each oil-feed sample, Residual oil must in time be discharged injector, interacts in case cause profit, affects little instant water gasification, and can not affect the impermeability of air-channel system in this process; 4. the injector internal volume of water molecule energy contact is as far as possible little, otherwise Wei Shui peak type broadening, can't be quantitative.Because high to the injector performance requirement, also do not have thisly under hot conditions on the market, can effectively realize the microsyringe of oil-water separating function moment.And adopt general gas chromatograph, only sample introduction just makes the chromatographic column severe contamination several times, even pollutes conductance cell, and mensuration can't be carried out, and also can damage valuable chromatograph.
Summary of the invention
The technical problem to be solved in the present invention provide a kind of gas circuit structure simple, be easy to make and the gas-oil separation function effective, based on the gas chromatograph with the gas-oil separation function of blowback principle, and a kind of process of gas chromatography of measuring micro-moisture in the insulating oil is disclosed.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Design a kind of gas chromatograph with the gas-oil separation function, contain thermal conductivity detector (TCD) (TCD) in its gas circuit structure, analyze chromatographic column, the protection chromatographic column, six-way valve, injector, T-valve, pressure maintaining valve A and B, needle valve, solenoid valve A and B, the air intake opening end communication with carrier gas source of described T-valve, its two outlet connects respectively and detects gas circuit and blowback gas circuit, described detection gas circuit connects described pressure maintaining valve A successively via tracheae or the passage of correspondence, needle valve, the reference arm of thermal conductivity detector (TCD), the six-way valve interface 1., the six-way valve interface 2., injector, the protection chromatographic column, the six-way valve interface 5., the six-way valve interface 6., analyze chromatographic column, the gage beam of thermal conductivity detector (TCD) and forming, described blowback gas circuit connects described solenoid valve A successively via tracheae or the passage of correspondence, pressure maintaining valve B, the six-way valve interface 4. with connect open to atmosphere six-way valve interface and 3. form; Described injector comprises by shell body, be positioned at the injection port at top, the cavity that loading plate limits, this cavity is distinguished into sample cavity and exocoel two parts by inner tube wherein, be filled with carrier in the described sample cavity, and its upper open end is corresponding to described injection port, its lower outlet end butts up against the set bleeder vent in described loading plate middle part, described shell body bottom is provided with to the air intake opening of the logical carrier gas of described exocoel, its top is provided with the exhausr port for the outside exhaust of described exocoel, and be connected to solenoid valve B behind this exhausr port, 2. described air intake opening is connected to described six-way valve interface via the pipeline of correspondence, and the lower end of this injector is connected with described protection chromatographic column via the pipeline of correspondence; When carrying out sample determination, described solenoid valve A and B close, and described six-way valve interface 1. and 2., 3. and 4., 5. and 6. be connected respectively; 2. and 3. 1. and 6. when carrying out the gas circuit blowback, described solenoid valve A and B open, and described six-way valve interface,, 4. and 5. are connected.
Utilize the process of gas chromatography of micro-moisture in the above-mentioned gas chromatograph for determination insulating oil, comprising:
(1) the post case temperature that the vaporizer temperature of setting described gas chromatograph sampling device is 200 ℃, include described protection chromatographic column and analyze chromatographic column is 120～150 ℃, the conductance cell temperature of thermal conductivity detector (TCD) is 150～160 ℃, described six-way valve temperature is 100～120 ℃, carrier gas (high pure nitrogen or helium) flow velocity 28～32mL/min;
(2) close described solenoid valve A and the B of closing, 1. and 2. make respectively described six-way valve interface, 3. and 4., 5. and 6. be connected, inject fast testing sample from the injection port of injector, enter the detection gas circuit through the T-valve branch outlet from source of the gas high pure nitrogen out, successively by pressure maintaining valve A, needle valve, the reference arm that thermal conductance detects, 1. and 2. the six-way valve interface enters described injector afterwards, and carry the vaporized composition to be measured described protection chromatographic column of flowing through successively, 5. and 6. the six-way valve interface, analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects, and tail gas is emptying;
(3) when described composition to be measured flow through described six-way valve interface 6. after, described solenoid valve A and B open simultaneously, and switch the six-way valve connecting interface, 1. and 6. make described six-way valve interface, 2. and 3., 4. and 5. be connected respectively, make high-purity carrier gas of flowing out from described T-valve pass through successively solenoid valve A, pressure maintaining valve B, six-way valve interface 4. and 5., enter successively more emptying behind described protection chromatographic column, the injector and form the blowback gas circuit, and then described protection chromatographic column, injector are carried out reverse blow;
(4) flow out the gage beam of TCD fully when composition to be measured, and until baseline steadily after, described six-way valve and solenoid valve A, B all switch to initial position simultaneously, prepare next sample introduction analysis.
The carrier that described sample cavity is filled is the glass microsphere carrier of silanization or the Diatomaceous Earth Support of processing through deactivation.
Described protection chromatographic column or to analyze filler in the chromatographic column be at least a among GDX502, GDX301, the GDX102.
Described protection chromatographic column and analysis chromatographic column all are arranged in the post case, and its internal diameter is 2mm, and described analysis column's length is not less than 1.8m, and described protection column's length is 1/10th of described analysis chromatographic column.
The present invention has actively useful effect:
⑴ when can guarantee to analyze, moisture peak type was unaffected, can make again into oil sample and oil vapour gone out chromatographic system by in time blowback, avoid Residual oil contamination analysis post and detector cell body.
⑵ the injection port structure that designed, the oil sample of difficult gasification is trapped in injection port in the time of effectively guaranteeing sample introduction; And during blowback, be convenient to Residual oil and discharge smoothly chromatographic system.
⑶ gas circuit structure is simple, and the injector that directly carries out gas-oil separation than high temperature is easy to make, and realizes the successful of gas-oil separation function; The good airproof performance of entire system.
Description of drawings
Fig. 1 is the process of gas chromatography figure under the sample introduction state;
Fig. 2 is the injector assembling flow path figure under the analysis state;
Fig. 3 is the structural representation of used injector in the gas circuit of gas chromatograph of the present invention;
Fig. 4 is certain collection of illustrative plates as a result of micro-moisture in the gas chromatograph for determination insulating oil of the present invention.
1 is T-valve among the figure, and 2 is pressure maintaining valve A, and 3 is needle valve, and 4 is the reference arm of thermal conductivity detector (TCD); 5 is six-way valve, and 6 is injector, and 7 are the protection chromatographic column, and 8 for analyzing chromatographic column; 9 is the gage beam of thermal conductivity detector (TCD), and 10 is solenoid valve A, and 11 is pressure maintaining valve B, and 12 is outer steel sheel; 13 is filler, and 14 is sample cavity, and 15 is openend; 16 is exhausr port, and 17 is air intake opening, and 18 is interior steel pipe; 19 is exocoel, and 20 is loading plate, and 21 is bleeder vent.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.Each parametric measurement method or inspection method among the following embodiment if no special instructions, are conventional method.
1 one kinds of gas chromatographs with the gas-oil separation function of embodiment, referring to Fig. 1, Fig. 2, Fig. 3, contain thermal conductivity detector (TCD) in its gas circuit structure, analyze chromatographic column 8(internal diameter 2mm, column length is not less than 1.8m, adopt porous polymer bead class filler, such as GDX502, GDX301 or GDX102), protection chromatographic column 7(internal diameter 2mm, column length is about 1/10th of analytical column, adopt porous polymer bead class filler, such as GDX502, GDX301 or GDX102), six-way valve 5, injector 6, T-valve 1, pressure maintaining valve A 2 and pressure maintaining valve B 11, be with manometric needle valve 3, solenoid valve A 10 and solenoid valve B 22, the air intake opening end communication with carrier gas source of T-valve 1, its two outlet connects respectively and detects gas circuit and blowback gas circuit, described detection gas circuit connects pressure maintaining valve A 2 successively via tracheae or the passage of correspondence, needle valve 3, the reference arm 4 of thermal conductivity detector (TCD), six-way valve 5 interfaces 1., six-way valve 5 interfaces 2., injector 6, protection chromatographic column 7, six-way valve 5 interfaces 5., six-way valve 5 interfaces 6., analyze chromatographic column 8, the gage beam 9 of thermal conductivity detector (TCD) and forming, described blowback gas circuit is via the tracheae of correspondence or passage successively connected electromagnetic valve A 10, pressure maintaining valve B 11, six-way valve 5 interfaces 4. with connect open to atmosphere six-way valve 5 interfaces and 3. form; When carrying out sample determination, solenoid valve A 10 and solenoid valve B 22 close, and six-way valve 5 interfaces 1. and 2., 3. and 4., 5. and 6. be connected respectively; When carrying out the gas circuit blowback, solenoid valve A 10 and solenoid valve B 22 opens, and six-way valve 5 interfaces 1. with interface 6., 2. and 3., 4. and 5. be connected respectively, in this state, injector 6 and protection chromatographic column 7 are in the blowback state.The switching mode of six-way valve can adopt pneumatic or motorized motions, but generally speaking, adopts pneumatic type of drive more convenient.
Described injector 6 comprises by outer steel sheel 12, be positioned at the injection port at top, the cavity that loading plate 20 limits, this cavity is by wherein interior steel pipe 18(internal diameter 4～5mm, the stainless-steel tube of length 30～40mm) is distinguished into sample cavity 14 and exocoel 19 two parts, be filled with carrier (can be glass microsphere carrier or other Diatomaceous Earth Support of processing through deactivation of silanization) in the sample cavity 14, and its upper open end 15 is corresponding to injection port, its lower outlet end butts up against the set bleeder vent 21 in loading plate 20 middle parts, outer steel sheel 12 bottoms are provided with to the air intake opening 17 of exocoel 19 logical carrier gas, its top is provided with the exhausr port 18 for exocoel 19 outside exhausts, and be connected to solenoid valve B 22 behind this exhausr port 18,2. air intake opening 17 is connected to six-way valve 5 interfaces via the pipeline of correspondence, and the lower end of this injector is connected with protection chromatographic column 7 via the pipeline of correspondence; Sample injects with the openend 15 of micro-injection pin from the injection port top, and in the gasification of the upper end of sample cavity 14.
TCD detecting device in the gas circuit is highly sensitive pair of pond four arm detecting devices, does in the carrier gas situation at nitrogen, can be less than 0.5ppm to the sensitivity of little water.
TCD pond body is arranged in the environment that can keep constant high temperature in the described process of gas path; injector 6 temperature can be heated to 200 ℃ at least; six-way valve 5 is in the environment that is not less than 100 ℃, and protection chromatographic column 7 and analysis chromatographic column 8 are arranged in the post case, and post case temperature should be able to free setting.
Utilize the process of gas chromatography of micro-moisture in the above-mentioned gas chromatograph for determination insulating oil, comprising:
(1) the post case temperature that vaporizer (injector) temperature of setting described gas chromatograph sampling device is 180～220 ℃, include described protection chromatographic column and analyze chromatographic column is 120 ℃, the conductance cell temperature of thermal conductivity detector (TCD) is 150 ℃, described six-way valve temperature is 100 ℃, carrier gas (high pure nitrogen) flow velocity 30mL/min;
(2) close described solenoid valve A and the B of closing, 1. and 2. make respectively described six-way valve interface, 3. and 4., 5. and 6. be connected, inject fast testing sample from the injection port of injector, enter the detection gas circuit through the T-valve branch outlet from source of the gas high-purity carrier gas out, successively by pressure maintaining valve A, needle valve, the reference arm that thermal conductance detects, 1. and 2. the six-way valve interface enters described injector afterwards, and carry the vaporized composition to be measured described protection chromatographic column of flowing through successively, 5. and 6. the six-way valve interface, analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects (testing result is referring to Fig. 4), and tail gas is emptying;
(3) when described composition to be measured flow through described six-way valve interface 6. after, described solenoid valve A and B open simultaneously, and switch the six-way valve connecting interface, 1. and 6. make described six-way valve interface, 2. and 3., 4. and 5. be connected respectively, make the high pure nitrogen that flows out from described T-valve pass through successively solenoid valve A, pressure maintaining valve B, six-way valve interface 4. and 5., enter successively more emptying behind described protection chromatographic column, the injector and form the blowback gas circuit, and then described protection chromatographic column, injector are carried out reverse blow;
(4) flow out the gage beam of TCD fully when composition to be measured, and until baseline steadily after, described six-way valve and solenoid valve A, B all switch to initial position simultaneously, prepare next sample introduction analysis.
Above-mentioned testing process meets among the GB GB/T 7601-2008 need have the sample introduction gasification to chromatograph, separates and get rid of the requirement of Residual oil.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (8)
1. gas chromatograph with the gas-oil separation function, contain thermal conductivity detector (TCD) in its gas circuit structure, analyze chromatographic column, the protection chromatographic column, six-way valve, injector, T-valve, pressure maintaining valve A and pressure maintaining valve B, needle valve, solenoid valve A and solenoid valve B, it is characterized in that, the air intake opening end communication with carrier gas source of described T-valve, its two outlet connects respectively and detects gas circuit and blowback gas circuit, described detection gas circuit connects described pressure maintaining valve A successively via tracheae or the passage of correspondence, needle valve, the reference arm of thermal conductivity detector (TCD), the six-way valve interface 1., the six-way valve interface 2., injector, the protection chromatographic column, the six-way valve interface 5., the six-way valve interface 6., analyze chromatographic column, the gage beam of thermal conductivity detector (TCD) and forming, described blowback gas circuit connects described solenoid valve A successively via tracheae or the passage of correspondence, pressure maintaining valve B, the six-way valve interface 4. with connect open to atmosphere six-way valve interface and 3. form; Described injector comprises by shell body, be positioned at the injection port at top, the cavity that loading plate limits, this cavity is distinguished into sample cavity and exocoel two parts by inner tube wherein, be filled with carrier in the described sample cavity, and its upper open end is corresponding to described injection port, its lower outlet end butts up against the set bleeder vent in described loading plate middle part, described shell body bottom is provided with to the air intake opening of the logical carrier gas of described exocoel, its top is provided with for described exocoel to the exhausr port that effluxes Residual oil, and be connected to solenoid valve B behind this exhausr port, 2. described air intake opening is connected to described six-way valve interface via the pipeline of correspondence, and the lower end of this injector is connected with described protection chromatographic column via the pipeline of correspondence; When carrying out sample determination, described solenoid valve A and solenoid valve B close, and described six-way valve interface 1. with interface 2., interface 3. with interface 4., 6. 5. interface be connected respectively with interface; When carrying out the gas circuit blowback, described solenoid valve A and solenoid valve B open, and described six-way valve interface 1. with interface 6., interface 2. with interface 3., 5. 4. interface be connected respectively with interface.
2. the gas chromatograph with the gas-oil separation function according to claim 1 is characterized in that, the carrier that described sample cavity is filled is the glass microsphere carrier of silanization or the Diatomaceous Earth Support of processing through deactivation.
3. the gas chromatograph with the gas-oil separation function according to claim 1 is characterized in that, described protection chromatographic column or to analyze filler in the chromatographic column be at least a among GDX502, GDX301, the GDX102.
4. the gas chromatograph with the gas-oil separation function according to claim 1; it is characterized in that; described protection chromatographic column and analysis chromatographic column all are arranged in the post case; its internal diameter is 1.5～2.5mm; described analysis column's length is not less than 1.8m, and described protection column's length is 0.1～0.2 times of described analysis chromatographic column.
5. utilize the process of gas chromatography of micro-moisture in the described gas chromatograph for determination insulating oil of claim 1, comprising:
(1) the post case temperature that the vaporizer temperature of setting the described gas chromatograph sampling device of claim 1 is 180～220 ℃, include described protection chromatographic column and analyze chromatographic column is 120～150 ℃, the conductance cell temperature of thermal conductivity detector (TCD) is 150～160 ℃, described six-way valve temperature is 100～120 ℃, and carrier gas high pure nitrogen flow velocity is 28～32ml/min;
(2) close described solenoid valve A and the B of closing, 1. and 2. make respectively described six-way valve interface, 3. and 4. interface, 5. and 6. interface is connected, inject fast testing sample from the injection port of injector, enter the detection gas circuit through the T-valve branch outlet from source of the gas high pure nitrogen out, successively by pressure maintaining valve A, needle valve, the reference arm that thermal conductance detects, 1. and 2. the six-way valve interface enters described injector afterwards, and carry the vaporized composition to be measured described protection chromatographic column of flowing through successively, 5. and 6. the six-way valve interface, analyze chromatographic column, the gage beam that enters thermal conductivity detector (TCD) detects, and tail gas is emptying;
(3) when described composition to be measured flow through described six-way valve interface 6. after, described solenoid valve A and B open simultaneously, and switch the six-way valve connecting interface, make described six-way valve interface 1. and 6., interface 2. and 3., 4. and 5. interface be connected respectively, make the high pure nitrogen that flows out from described T-valve pass through successively solenoid valve A, pressure maintaining valve B, six-way valve interface 4. and 5., enter successively more emptying behind described protection chromatographic column, the injector and form the blowback gas circuit, and then described protection chromatographic column, injector are carried out reverse blow;
(4) divide the gage beam that flows out thermal conductivity detector (TCD) fully when composition to be measured, and until baseline steadily after, described six-way valve and solenoid valve A, B all switch to initial position simultaneously, prepare next sample introduction analysis.
6. the process of gas chromatography of micro-moisture in the mensuration insulating oil according to claim 5 is characterized in that, the carrier that described sample cavity is filled is the glass microsphere carrier of silanization or the Diatomaceous Earth Support of processing through deactivation.
7. the process of gas chromatography of micro-moisture in the mensuration insulating oil according to claim 5 is characterized in that, described protection chromatographic column or to analyze filler in the chromatographic column be at least a among GDX502, GDX301, the GDX102.
8. the process of gas chromatography of micro-moisture in the mensuration insulating oil according to claim 5; it is characterized in that; described protection chromatographic column and analysis chromatographic column all are arranged in the post case; its internal diameter is 1.5～2.5mm; described analysis column's length is not less than 1.8m, and described protection column's length is 0.1～0.2 times of described analysis chromatographic column.
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| CN104297390A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Chromatographic analysis method |
| CN104297388A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Sampling device |
| CN104297389A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Chromatographic analysis system |
| CN110146607A (en) * | 2019-05-06 | 2019-08-20 | 北京水木滨华科技有限公司 | The quantitative detecting method of micro-moisture in a kind of organic system |
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| CN112268975A (en) * | 2020-09-21 | 2021-01-26 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Device and method for expanding multichannel automatic sample introduction of insulating oil-gas chromatograph |
| CN112798723A (en) * | 2021-03-09 | 2021-05-14 | 郑州大学 | Quantitative analysis device for detecting gas chromatograph blowback gas |
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| 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 |
| 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 |
| CN104297389A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Chromatographic analysis system |
| CN104297388A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Sampling device |
| CN104297389B (en) * | 2014-10-23 | 2016-07-06 | 佛山市南海区环境保护监测站 | A kind of chromatographic analysis system |
| CN104297390B (en) * | 2014-10-23 | 2016-07-06 | 佛山市南海区环境保护监测站 | A kind of chromatogram analysis method |
| CN104297390A (en) * | 2014-10-23 | 2015-01-21 | 佛山市南海区环境保护监测站 | Chromatographic analysis method |
| CN104297388B (en) * | 2014-10-23 | 2016-08-24 | 佛山市南海区环境保护监测站 | Sampling device |
| CN110146607A (en) * | 2019-05-06 | 2019-08-20 | 北京水木滨华科技有限公司 | The quantitative detecting method of micro-moisture in a kind of organic system |
| CN110146607B (en) * | 2019-05-06 | 2020-05-15 | 北京水木滨华科技有限公司 | Quantitative detection method for trace moisture in organic system |
| CN111707773A (en) * | 2020-06-19 | 2020-09-25 | 国电南京自动化股份有限公司 | Online gas chromatography column efficiency judging and self-repairing device system |
| CN112268975A (en) * | 2020-09-21 | 2021-01-26 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Device and method for expanding multichannel automatic sample introduction of insulating oil-gas chromatograph |
| CN112881557A (en) * | 2021-01-19 | 2021-06-01 | 华中科技大学 | Gas introduction method and device of gas chromatograph |
| CN112798723A (en) * | 2021-03-09 | 2021-05-14 | 郑州大学 | Quantitative analysis device for detecting gas chromatograph blowback gas |
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